Quality Assurance Guidance Document

Quality Assurance Project Plan:

PM2.5 Chemical Speciation Sampling at Trends, 

NCore, Supplemental and Tribal Sites

(An Update to the PM2.5 Speciation Trends

Network Field Sampling QAPP, December 2000)

EPA-454/B-12-003 

June 2012 

Quality Assurance Guidance Document

Quality Assurance Project Plan:

PM2.5 Chemical Speciation Sampling at

Trends, NCore, Supplemental and Tribal Sites

(An Update to the PM2.5 Speciation Trends

Network Field Sampling QAPP, 

December 2000)

By: 

Ambient Air Monitoring Group, 

Air Quality Assessment Division

US EPA, Office of Air Quality Planning and Standards 

Research Triangle Park, North Carolina
 
 

i

Note: At various points in this QAPP, the reader is referred to the EPA’s AMTIC website for further 

information and updated information.

Foreword

This document is the Quality Assurance Project Plan (QAPP) for all operations involved in the 

PM2.5 Chemical Speciation Network (CSN). The original QAPP was issue in 2000 as the CSN 

was being deployed. The CSN has evolved over time due to the advent of the NCore monitoring 

network prescribed by rulemaking in October 2006 and the most dramatic changes in 2008-2010, 

when the national network of samplers were consolidated to Metone SASS or SuperSASS and 

URG 3000N. This version of the QAPP reflects that transition and a few new quality control 

checks that are recommended to provide a better tracking process for deleterious changes in 

sampler flow rates. The approach to utilizing collocated samplers for network precision has also 

been expanded to a redeploy the collocated samplers at half of the historic, fixed collocation sites 

to annual assignments that rotate among the other NCore sites. 

 This QAPP was generated using the U.S. Environmental Protection Agency (EPA) Quality 

Assurance (QA) regulations and guidance described in EPA QA/R-5, EPA Requirements for 

Quality Assurance Project Plans and the accompanying document EPA QA/G-5, Guidance for 

Quality Assurance Project Plans. All pertinent elements of the requirements and guidance are 

addressed in this QAPP. This QAPP incorporates by reference, the current QAPPs utilized by

analytical and technical support contractors. These are available at the EPA’s Ambient 

Monitoring Technical Information Center (AMTIC) website, 

http://www.epa.gov/ttn/amtic/speciepg.html. The SOPs associated with operating the samplers are 

located at http://www.epa.gov/ttn/amtic/spectraining.html. The SOPs associated with operations 

performed by the contract service lab are located at: http://www.epa.gov/ttn/amtic/specsop.html. 

The date in each section header indicates the last time the particular section was reviewed and/or 

revised by EPA.

This 2012 version is the first revision since the publication of the 2000 document for which EPA 

is requesting that State, Local and Tribal QAPP review and either (1) adopt this QAPP or (2) 

revise their own QAPP. This document should be reviewed by EPA Regional Offices and the 

Regional Speciation Coordinators responsible for implementing the CSN in their respective 

Regions, the EPA Technical Monitors for the network, and the QA Manager of the contracted 

support laboratory for the CSN. The EPA Quality Assurance Policies in EPA Order 5360.1 A2 

require agencies that accept federal grant funding for their air monitoring programs to have a QA 

program with certain elements including quality management plans (QMPs), QAPPs, and the 

identification of a QA management function. It is acceptable for the state, local and/or Tribal 

(SLT) air pollution agencies to use this document in lieu of writing their own field QAPP; 

however, certain sections may have to be revised to make the information specific to the 

monitoring program adopting it. In such case, this document should be modified by the 

submitting SLT monitoring organization, and the EPA Regional Offices shall review and 

approve the SLT’s QAPP, and sign the approval page (see approval page Section 1.2), or if the 

SLT has delegated approval authority through a Regionally approved Quality Management Plan, 

the Region’s signature represents acknowledgement that the QAPP has been “approved.” 
 

ii

Mention of corporation names, trade names, or commercial products does not constitute 

endorsement or recommendation for use. 

The following EPA Office of Air Quality Planning and Standards (OAQPS) personnel may be 

contacted concerning the contents of this document: 

Dennis Crumpler, OAQPS-AAMG C304-06, Research Triangle Park, NC 27711 

crumpler.dennis@epa.gov

David Shelow, OAQPS-AAMG C304-06, Research Triangle Park, NC 27711 

Solomon Ricks, OAQPS-AAMG C304-06, Research Triangle Park, NC 27711 

shelow.david@epa.gov

 

ricks.solomon@epa.gov
 

iii

Acronyms and Abbreviations

AAMG Ambient Air Monitoring Group 

AMTIC Ambient Monitoring Technical Information Center 

ANSI American National Standards Institute

APTI (EPA) Air Pollution Training Institute

ASQC American Society for Quality (Control)

AQS Air Quality System

AQAD Air Quality Analysis Division

CAA Clean Air Act

CASAC (EPA) Clean Air Scientific Advisory Committee

CFR Code of Federal Regulations 

CMD (EPA) Contract Management Division

COC chain of custody 

CSN (PM2.5) Chemical Speciation Network

CV coefficient of variation

DOPO (EPA) delivery order project officer

DQA data quality assessment

DQO data quality objective 

EC/OC elemental carbon/organic carbon

EDXRF energy-dispersive X-ray fluorescence

EPA Environmental Protection Agency 

FR Federal Register

FRM Federal Reference Method (for PM2.5 sampling) 

IC ion chromatography 

IMPROVE Interagency Monitoring of Protected Visual Environments (network or sampler) 

ISO International Organization for Standardization 

IUPAC International Union of Pure and Applied Chemistry 

L/min liters per minute

LCD liquid crystal display

M2.5 mass of PM2.5

m3 cubic meter 

MASS Mass Aerosol Speciation Sampler (URG Corp.) 

max./min. maximum/minimum (thermometer)

mL milliliter

mmHg millimeters of mercury (pressure)

MQO measurement quality objective

MSA metropolitan statistical area

MSR management systems review

NAAQS national ambient air quality standard 

NAMS national air monitoring station

NAREL National Air and Radiation Environmental Laboratory 

NCORE National Core (monitoring network) 

NERL (EPA) National Exposure Research Laboratory 

NIST National Institute of Standards and Technology 

OAQPS (EPA) Office of Air Quality Planning and Standards 
 

iv

OAR (EPA) Office of Air and Radiation

ORD (EPA) Office of Research and Development

ORIA (EPA) Office of Radiation and Indoor Air 

PAMS photochemical air monitoring station

PM2.5 particulate matter, 2.5 micrometer diameter

PO project officer

PQAO primary QA organization 

QA quality assurance

QAL quality assurance lead or leader

QAM quality assurance manager

QAPP Quality Assurance Project Plan

Qavg average flow rate

QC quality control 

QMP quality management plan 

RAAS Reference Ambient Air Sampler (Thermo-Andersen Instruments, Inc.)

R&IE Radiation and Indoor Air 

R&P Rupprecht and Patashnick Co. (No longer in existence) 

RSC regional speciation coordinator 

RTP Research Triangle Park (North Carolina)

SASS Speciation Air Sampling System (Met One Instruments, Inc.)

SHAL sample handling and archival laboratory 

SLAMS state and local air monitoring station

SOP standard operating procedure 

SPM (laboratory) services program manager

SLT state, local and/or Tribal agency or monitoring organization 

STAG state and tribal assistance grants

SVOC semi-volatile organic compound 

TSA technical systems audit

VOC volatile organic compound 

XRF X-ray fluorescence °

C degree Celsius

μg/m3 micrograms (of PM) per cubic meter (of air sampled)
 

v

Tables

Number Section Page

6-1 Critical Measurements in the PM2.5 CSN 6 3

6-2 Checklist of PM2.5 CSN Site Operator

Field Activities

6 4

6-3 Sequence of Activities for Bringing a 

PM2.5 CSN Field Site On-Line

6 9

6-4 Critical Filter and Denuder Holding and 

Use Times

6 11

7-1 MQOs for Total Measurement Error 7 4

7-1.a MQOs for Total Measurement Error (2007 

– 2010 Data From Collocated Samplers 

Upper Bound 90th Percentile CV From 

Values > MDL

7 4

9-1 CSN Reporting Package Information 9 2

10-1 Sequence of Activities for CSN Contracted 

Support Laboratory 

10 1

10-2 Design Criteria for Collection Site 

Surroundings 

10 2

11-1 Summary of Information Provided by 

Speciation Sampler

11 2

11-2 CSN Field Operations Corrective 

Procedures

11 6

12-1 Explanation of CSN Custody and Field 

Data Form

12 6

14-1 MQOs and Associated QC Activities for 

the PM2.5 CSN 

14 3

15-1 Testing and Acceptance Criteria Checklist 

for PM2.5 Speciation Samplers

15 2

15-2 Preventive Maintenance and 

Recertification of CSN Field Equipment 

15 3

16-1 Acceptance Criteria and Calibration and 

Maintenance Frequencies for PM2.5 

Chemical Speciation Samplers

16 4

16-2 Calibration Standards for PM2.5 Chemical 

Speciation Samplers

16 7
 

vi

17-1 Inventory List for CSN Field Equipment 

and Supplies 

17 2

19-1 Suggested Support Laboratory Data 

Record Archival Summary

19 10

19-2 Validation Check Summaries 19 11

19-3 Data Transfer Operations 19 11

19-4 Summary of AQS Data Flags for PM2.5 19 13

19-5 Raw Data Calculations 19 16

20-1 Assessment Summary 20 2

21-1 Summary of Reports to Management for 

CSN

21 2

22-1 Data Verification Activities and 

Responsibilities for the CSN 

22 2

22-2 Quality Control Data for CSN Data 

Verification and Validation

22 7

22-3 Statistical Validation Limits for Blanks 22 13

22-4 Statistical Validation Limits for Routine 

Data 

22 14

22-5 Mapping of Outlier Flags onto AQS Codes 22 14

22-6 Automated Range Checks 22 14

22-7 Data Verification and Validation Summary 22 16
 

vii

Figures 

Number Section Page

4-1 Chemical Speciation Network Coordination Activities 4 2

4-2 Laboratory Technical Management and Staff Organization for 

CSN Filter Analysis and Data Reporting

4 11

5-1 Interrelationships Between chemical Speciation Networks as of 

2011 

5 2

6-1 Summary of the CSN Project Operations 6 2

6-2 Sample Analysis Delivery Order Process 6 7

6-3 Diagram of Laboratory Filter Processing and Analysis 

Activities, by Filter Type

6 8

11-1 Quality Bulletin 11 5

12-1 CSN Custody and Field Data Form for MetOne SASS Sampler 12 5

12-2 CSN Custody and Field Data Form for URG 3000N Sampler 12 6

14-1 Monthly Flow Check Decision Tree for Corrective Actions 14 8

14-2 CSN QA/QC Report Form 14 10

19-1 CSN Data Flow Overview 19 2

20-1 Surveillance Report Form 20 8

20-2 Assessment Finding Response Form 20 8

 
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 1 of 7

1.0 QA Project Plan Identification and Approval

Title: Quality Assurance Project Plan: PM2.5 Chemical Speciation Sampling at NCore

Sites, and State, local and Tribal Supplemental Sites

1.1 The EPA-Approved PM2.5 Chemical Speciation Network (CSN) QAPP 

Category: Category 1

By signing below, the Environmental Protection Agency’s (EPA’s) Office of Air Quality Planning and 

Standards’ (OAQPS) Ambient Monitoring Program and Quality Assurance Leads and Managers have 

found the underlying Quality Assurance Project Plan (QAPP) to provide sufficient detail in quality 

assurance (QA) and quality control (QC) procedures, sampling and analytical procedures, and data 

management as to be directly adoptable by reference by any state, local or Tribal (SLT) monitoring 

agency for the purpose of conducting monitoring of chemically speciated particulate matter with a 

aerodynamic diameter of 2.5 microns (PM2.5) and reporting same in units micrograms per cubic meter 

of air sampled. Signature by a Regional representative, such as a QA manager or monitoring program 

manager or their delegated designee, signifies concurrence with all aspects of this QAPP. 

An example submittal form for adopting the “EPA-Approved QAPP version 1.2.0,” or revising it and 

acquiring EPA Regional approval or acknowledgement is provided in Section 1.2. Each monitoring 

agency may choose to adopt this QAPP in its entirety, revise it as necessary for its specific needs, or 

develop a completely new QAPP to better fit with the implementation of their quality system. In some 

Regions, states have been delegated full signature authority for QAPP approvals through a priori 

approval of their Quality Management Plans (QMPs). In this case, the SLT would have to sign the 

signature page and the Region would retain a copy in their files. 

In those Regions where final approval authority has not been delegated, the Regional Monitoring 

Program and QA managers should approve any SLT adoption or revisions to the QAPP on the 

signature page that is provided. In the latter case, the monitoring agency should submit the revised 

QAPP or a list of modifications to the “EPA Approved” QAPP, to their respective EPA Regional 

Monitoring Program Office with supporting documentation that the revisions fully meet the quality 

system objectives set out in this network QAPP. When signed, these forms are to be kept in the 

permanent records of the EPA Regional Office. 
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 2 of 7

CSN QAPP Version 1.2.0 Approvals 

OAQPS

_______________________ Date ________ 

David Shelow, CSN Program Lead 

_____________________ Date _____________ 

Dennis Crumpler, CSN QA Lead 

_______________________ Date ________ 

Lewis Weinstock, Group Leader, AAMG 

 

Regional Concurrence/Approvals (See Attached pages)

Region 1 

____________________________ Date _______ 

Region 2 

____________________________ Date _______ 

Print name/title below Print name/title below

Region 3 

____________________________ Date _______ 

Region 4 

____________________________ Date _______ 

Print name/title below Print name/title below

Region 5 

____________________________ Date _______

Region 6 

____________________________ Date _______ Print name/title below Print name/title below

Region 7 

____________________________ Date _______

Region 8 

____________________________ Date _______

Print name/title below Print name/title below

Region 9 

____________________________ Date _______

Region 10 

____________________________ Date _______

Print name/title below Print name/title below
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 1 of 7
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 2 of 7
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 3 of 7
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 4 of 7
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 5 of 7
PM2.5 CSN QAPP

Section No. 1

Revision No.: 1.2.0

Date: 05/12

Page 1 of 7

1.2 Adoption of the EPA-Approved CSN QAPP Revision 1.2.0 or Adoption of a 

Revision of the CSN QAPP by a Monitoring Agency (This page is retained by the 

EPA Regional Office)

By signing below, the Monitoring Agency commits to implement either: (check one)

The CSN Quality Assurance Project Plan Revision 1.2.0, dated ________ approved by EPA; or

The CSN Quality Assurance Project Plan submitted herein, with all 

 Agency Name

deviations from the “EPA-Approved CSN QAPP Revision 1.2.0” approved by EPA clearly 

identified, and documentation supporting the proposition that all revisions provide equivalent or 

better quality monitoring data. 

Delegated QAPP Approval Authority 

The has been delegated full QAPP Approval and signature authority 

 Agency Name

by EPA Region ________. 

State/Local/Tribal Agency

Print Name:________________________ Signature:_________________________ 

Date: _________ PM2.5 Speciation Monitoring Coordinator 

Print Name:________________________ Signature:_________________________ 

Date: _________ Quality Assurance Officer 

Print Name:________________________ Signature:_________________________ 

Date: _________ Air Program Director 

EPA Regional Office Acknowledgement or Approval

Print Name:________________________ Signature:_________________________ 

Date: _________ PM2.5 Speciation Monitoring Coordinator 

Print Name:________________________ Signature:_________________________ 

Date: _________ Quality Assurance Manager

Print Name:________________________ Signature:_________________________ 

Date: _________ Grants, Audits & Procurement Program Director 
PM2.5 CSN QAPP

Section No. 2

Revision No.: 1.2.0

Date: 05/12

Page 1 of 7

2.0 Table of Contents

Section Page Revision Date

Foreword i 1.2.0 10/11

Acknowledgments ii 1.2.0 10/11

Acronyms and Abbreviations iii 1.2.0 10/11

Tables vi 1.2.0 10/11

Figures viii 1.2.0 10/11

1.0 QA Project Plan Identification and Approval 1/1 1.2.0 10/11

2.0 Table of Contents 1/7 1.2.0 10/11

3.0 Distribution 1/4 1.2.0 10/11

4.0 Project/Task Organization 1/10 1.2.0 10/11

4.1 Chemical Speciation Network Coordination 

Activities

2/10

4.2 Chemical Speciation Network -- State, Local, and 

Tribal Organizations 

7/10

4.3 CSN Network Laboratory Activities Organization 8/10

5.0 Background and Problem Definition 1/3 1.2.0 10/11

5.1 Background 1/3

5.2 Problem Definition 1/3

5.3 PM2.5 Speciation Sampling Techniques and Ongoing 

Research

2/3

5.4 Monitoring Network Design Considerations 3/3

6.0 Project/Task Description 1/11 1.2.0 10/11

6.1 Description of Work to be Performed 1/11

6.2 Field Activities 3/11
PM2.5 CSN QAPP

Section No. 2

Revision No.: 1.2.0

Date: 05/12

Page 2 of 7

Section Page Revision Date

6.3 Laboratory Activities 4/11

6.4 Schedule of Activities 8/11

6.5 Project Assessment Techniques 11/11

6.6 Project Records 11/11

6.7 References 11/11

7.0 Quality Objectives and Criteria For Measurement Data 1/4 1.2.0 10/11

7.1 Data Quality Objectives Process 1/4

7.2 Development of DQOs for the PM2.5 Chemical 

Speciation Network

1/4

7.3 Measurement Quality Objectives 2/4

7.4 References 4/4

8.0 Special Training Requirements/Certification 1/3 1.2.0 10/11

8.1 Training 1/3

8.2 Certification 3/3

9.0 Documentation and Records 1/6 1.2.0 10/11

9.1 Information in the Management and Organization 

Reporting Package

1/6

9.2 Information in the Field Operations Reporting 

Package

2/6

9.3 Information in the Laboratory Operations Reporting 

Package

4/6

9.4 Information in the QA Reporting Package 4/6

9.5 Reports to Management 5/6

9.6 Archival and Retrieval of Data Reporting Packages 6/6

10.0 Sampling Process Design 1/4 1.2.0 10/11

10.1 Scheduled Project Activities, Including Management 

Activities

1/4

10.2 Rationale for the Design 2/4

10.3 References 4/4
PM2.5 CSN QAPP

Section No. 2

Revision No.: 1.2.0

Date: 05/12

Page 3 of 7

Section Page Revision Date

11.0 Sampling Methods Requirements 1/8 1.2.0 10/11

11.1 Sample Collection and Preparation 1/8

11.2 Sampling/Measurement System Corrective Action 

Process

3/8

11.3 Avoiding Sample Contamination; Temperature and 

Holding Time Requirements 

4/8

12.0 Sample Handling and Custody Requirements 1/6 1.2.0 10/11

12.1 Introduction 1/6

12.2 Filter Handling and Custody Procedures Prior to 

Sampling Event 

1/6

12.3 Sample Handling and Custody Procedures 3/6

12.4 Filter and Sample Archival in the CSN Laboratory 5/6

13.0 Analytical Methods Requirements 1/1 1.2.0 10/11

14.0 Quality Control Requirements 1/11 1.2.0 10/11

14.1 Quality Control Checks 3/11

14.2 QC Samples 3/11

14.3 Collocated Samplers 5/11

14.4 Calculations of Accuracy, Bias, Precision, and 

Completeness

5/11

14.5 References 11/11

15.0 Sampler/Equipment Testing, Inspection, and Maintenance 

Requirements

1/4 1.2.0 10/11

15.1 Testing and Acceptance Criteria 1/4 

15.2 Maintenance 1/4

15.3 Critical Spare Parts 3/4

16.0 Instrument Calibration and Frequency 1/6 1.2.0 10/11

16.1 Overview 1/6
PM2.5 CSN QAPP

Section No. 2

Revision No.: 1.2.0

Date: 05/12

Page 4 of 7

Section Page Revision Date

16.2 Calibration and Verification of Field Instrumentation 1/6

16.3 Calibration and Verification of Laboratory 

Instrumentation

3/6

17.0 Inspection/Acceptance for Supplies and Consumables 1/2 1.2.0 10/11

17.1 Purpose 1/2

17.2 Critical Supplies and Consumables for Field Site 

Operations 

1/2

17.3 Acceptance Criteria 2/2

18.0 Data Acquisition Requirements (Nondirect Measurements) 1/2 1.2.0 10/11

18.1 Acquisition of Nondirect Measurement Data 1/2

19.0 Data Management 1/16 1.2.0 10/11

19.1 Overview 1/16

19.2 Data Management Activities at the CSN Contracted 

Support Laboratory

3/16

19.3 Data Management Activities at the RO 3/16

19.4 Recommended Data Management Practices 6/16

19.5 Data Validation 8/16

19.6 Data Transformations 14/16

19.7 Data Transmittal 14/16

19.8 Data Reduction 14/16

19.9 Data Analysis 15/16

19.10 Data Storage and Retrieval 15/16

20.0 Assessment and Response Actions 1/9 1.2.0 10/11

20.1 Types of Assessments 1/9

20.2 Assessment Frequency 1/9

20.3 Acceptance Criteria 2/9

20.4 Assessment Schedules 3/9

20.5 Assessment Personnel 3/9
PM2.5 CSN QAPP

Section No. 2

Revision No.: 1.2.0

Date: 05/12

Page 5 of 7

Section Page Revision Date

20.6 Assessment Reports 5/9

20.7 Implementation of Response Actions 6/9

20.8 References 9/9

21.0 Reports to Management 1/5 1.2.0 10/11

21.1 Annual QC Summary Report (Laboratory) 3/5

21.2 Annual QA Report to Management (Network 

Review) 

3/5

21.3 Precision, Bias, and Accuracy Quarterly Reports 3/5

21.4 Laboratory Performance Evaluation and Technical 

Systems Audit Results

4/5 

21.5 Site TSAs (External) 4/5

21.6 Routine Quality Control Records 4/5

21.7 Data Validation Summaries 4/5

21.8 Corrective Action Reports and Performance-Related 

Records

5/5

22.0 Data Review, Validation, and Verification Requirements 1/16 1.2.0 10/11

22.1 Data Verification and Validation Responsibilities 1/16

22.2 Corrective Action Reporting Process 6/16

22.3 Use of QC Information for Verification and 

Validation

6/16

22.4 Use of Calibration Information for Verification and 

Validation

6/16

22.5 Level 0 Verification and Validation 9/16

22.6 Level 1 Data Validation 10/16

22.7 Data Screening Techniques used by the Contracted 

Support Laboratory

11/16

22.8 Treatment of Deviations from Requirements 14/16

22.9 Verification and Validation Criteria: Field 

Component 

14/16

23.0 Validation and Verification Methods 1/5 1.2.0 10/11
PM2.5 CSN QAPP

Section No. 2

Revision No.: 1.2.0

Date: 05/12

Page 6 of 7

Section Page Revision Date

23.1 Inter-organizational Responsibilities for Data 

Validation

1/5

23.2 Personnel Responsibilities Within the Reporting 

Organization 

2/5

23.3 Completion of Level 0 Data Verification and 

Validation

2/5

23.4 Identification of Outliers and Data Flagging 

Techniques

3/5

24.0 Reconciliation with Data Quality Objectives 1/7 1.2.0 10/11

24.1 DQO for Chemical Speciation Trends 1/7

24.2 Interim Evaluations of Data Quality 2/7

24.3 Assessing and Reporting Chemical Speciation 

Trends

6/7

24.4 Reconciling Other CSN Research Objectives 7/7

24.5 References 7/7
PM2.5 CSN QAPP

Section No. 2

Revision No.: 1.2.0

Date: 05/12

Page 7 of 7

Appendix A

Section Page Revision Date

A-1 SOP: CSN Standard Operating Procedure for Field 

Installation of PM2.5 Speciation Samplers

1.2.0 10/11

A-2 SOP: CSN Condensed Standard Operating Procedure for 

the MetOne SASS

1.2.0 10/11

A-3 SOP: CSN Standard Operating Procedure for the URG 

3000N Carbon Speciation Sampler

1.2.0 10/11

A-4 SOP: CSN Packing Instructions for the Speciation Sampler 

Modules

1.2.0 10/11

A-5 XL Worksheets and Instructions for Recording and 

Reporting CSN Sampler Performance Verifications

1.2.0 10/11

A-6 XL Worksheets and Instructions for Recording and 

Reporting TSA’s of CSN Monitoring Sites Including 

Sampler Performance Audits

1.2.0 10/11

Note: Standard Operating Procedures (SOPs) for the Andersen RAAS and the URG MASS 400 

and MASS 450 speciation samplers (used in the CSN until 2009) are not included as appendices.

None of these samplers remain in the CSN network and vendor support has been suspended. 

SOPs for these samplers are available on the AMTIC website in the December 2000 QA 

Guidance Document, EPA 454/D01-001.
PM2.5 CSN QAPP

Section No. 3

Revision No.: 1.2.0

Date: 11/11

Page 1 of 1

3.0 Distribution 

An electronic version of this Quality Assurance Project Plan (QAPP) will be available on the 

Ambient Monitoring Technical Information Center (AMTIC) Speciation web page at

http://www.epa.gov/ttn/amtic/specguid.html. Availability of the QAPP will be announced on the 

Monitoring List Serve maintained by the Ambient Monitoring Program within the 

Environmental Protection Agency’s (EPA) Office of Air Quality Planning and Standards 

(OAQPS) at Research Triangle Park, North Carolina. The OAQPS will email a copy to the 

Regional Speciation Coordinators (RSCs) at the National Contract Laboratory, and the EPA’s 

Office of Radiation and Indoor Air (ORIA) National Air and Radiation Environmental 

Laboratory (NAREL), Montgomery, Alabama. The RSCs will be responsible for ensuring that 

the QAPP is distributed through state, local, and/or Tribal (SLT) agency Monitoring Program 

Manager or Director of each field site and analytical laboratory (if different than the national 

contract laboratory) in the environmental data operations of the Chemical Speciation Network 

(CSN). The RSCs should also provide a copy of this QAPP to their Regional Quality Assurance 

(QA) Managers. 

Required Distribution

• Regional RSCs

o SLT Agency Monitoring Program Manager or Director 

 Every monitoring site and site supervisor 

o Analytical support laboratories for specific SLTs who have opted to analyze their 

own filters or who have contracted a laboratory who is not the national contract 

laboratory 

• Delivery Order Project Officers

• Regional QA Managers

• National Contract Laboratory 
PM2.5 CSN QAPP

Section No. 4

Revision No.:1.2.0

Date: 01/12

Page 1 of 10

4.0 Project/Task Organization

This section is intended to provide all parties involved in the Chemical Speciation Network 

(CSN) with a clear understanding of their roles and the lines of authority, communication, and 

reporting for the project.

The organization of the CSN involves multiple interacting entities: 

(1) The EPA’s Office of Air Quality Planning and Standards (OAQPS), Office of Radiation and 

Indoor Air (ORIA), Office of Research and Development (ORD), and Regional Offices; (2)

state, local and/or Tribal (SLT) air monitoring and reporting organizations; and (3) one or more 

contracting laboratories to service monitoring sites with supplies, sample analysis, and data 

reporting. To make the best use of available resources and to meet demanding timelines for 

collection and analysis of samples, the flow of information and samples must be optimally 

organized. The deployment and operation of the network are responsibilities shared among all 

the involved parties. This section describes the roles of all parties and establishes the lines of 

communication and reporting, with the goal of facilitating a smoothly operating network. 

Figure 4-1 provides a unified view of all agencies and contractors involved in the network’s 

operating structure as well as lines of communication and reporting. Block A of Figure 4-1 

points out the CSN’s coordination activities, led by EPA’s OAQPS. The Program Quality 

Assurance (QA) Manager, the network’s Project Officer (PO), the EPA-Regional Speciation 

Coordinators (RSCs), and Delivery Order Project Officers (DOPOs), are also included in the 

network’s planning and coordination activities component. Block B of Figure 4-1 shows the field 

activities, the SLT agency, CSN sampling, and QA/Quality Control (QC) personnel will perform 

and their lines of communication to the DOPOs, the CSN PO, and the contracted support 

laboratory. Block C of Figure 4-1 shows the contracted support laboratories. The EPA ORIA 

technical assistance and QA assessment laboratories are included in Blocks B and C.

The Speciation Contacts Table found on the Ambient Monitoring Technical Information Center 

(AMTIC) website provides the current names and contact information for the persons in each of 

these positions. Sections 4.1 through 4.3 discuss details of the roles and interactions between and 

among the many participants in this maze of activity.
PM2.5 CSN QAPP

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PM2.5 CSN Coordination Activities

EPA PM2.5 Chemical Speciation 

Workgroup

OAQPS Group Leader

Program Manager

PM2.5 Laboratory Services 

Contracts Project Officer (PO)

Program QA Manager or Lead Regional Office

- Regional Speciation 

Coordinators (RSCs)

- Delivery Order Project Officers 

(DOPOs)

Advisors

- CASAC

- ORD/Panel NERL

Block A

CSN Field Activities

State. Local, Tribal Agencies

Field QA Assessments 

ORIA, Las Vegas, NV

CSN Laboratory Support Activities

Chemical Speciation Contracted 

Support Laboratories (CSLs)

Lab QA Auditing and 

Technical Assistance 

ORIA, Montgomery, AL

Block B Block C

Figure 4-1. Chemical Speciation Network Coordination Activities. 

4.1 Chemical Speciation Network Coordination Activities 

The coordination of CSN network activities is accomplished by several groups, as illustrated in 

Figure 4-1. Block A of this figure includes the PM2.5 Chemical Speciation Workgroup, the 

OAQPS Program Manager for the CSN advisory groups (Clean Air Scientific Advisory 

Committee (CASAC) and ORD), the Program QA Manager, and the Laboratory Services 

Contracts PO, the RSCs, and the DOPOs. These groups assist in coordinating, advising, 

planning, and managing the activities of the CSN field and laboratory activities. Roles of the 
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workgroup, advisory panels and committees, and the QA lead person are described below. Not 

all committees and personnel are shown in Figure 4-1. 

4.1.1 PM2.5

The PM

 Chemical Speciation Workgroup 

2.5

4.1.2 Office of Air Quality Planning and Standards Ambient Monitoring Program 

 Chemical Speciation Workgroup was formed at the inception of the CSN in 1998 to 

provide input and the review of all aspects of the chemical speciation program, which

encompasses sampler design, network design and QA procedures. Members of the workgroup 

included personnel from EPA OAQPS, EPA Regional Offices, the EPA ORD’s National 

Exposure Research Laboratory (NERL), and SLT air monitoring organizations. This workgroup 

is currently inactive but may be reconvened if critical issues needing broad technical and policy 

input arise. 

The OAQPS Ambient Monitoring Program has oversight concerning design of the nation’s 

ambient monitoring networks and the quality of the nation’s ambient air data these networks 

generate. The OAQPS has published specific regulations for the development of a quality system 

which are found in 40 Code of Federal Regulations (CFR) Part 58, Appendix A. One specific 

element of this quality system is the development and coordination of the PM2.5 ambient

 Coordinating and overseeing the Chemical Speciation Trends Sampling at NCore

sites which are part of the CSN.

monitoring networks, one of which is the CSN. The OAQPS will ensure the orderly operation of 

the CSN through the following activities: 

 Working with the EPA Regional Offices and SLT organizations to determine the best 

sampling locations. 

 

 Providing a contract vehicle for one (or more) laboratories to support the field sites 

and provide filter analysis and associated functions. 

 Developing documents for the chemical speciation monitoring network, CSN, 

including the strategic plan for the quality system, standard operating procedures 

(SOPs) for field sites and laboratory operations, and the QAPP for the NCore 

chemical speciation sites. 

 Providing, through this document, a model QAPP for state and local air monitoring 

station (SLAMS) and Tribal Networks to adapt and adopt. 

 Developing guidance for field and laboratory personnel requirements as well as

training activities. 

 Securing national experts and advisors to answer specific technical questions and 

review the network; responding to recommendations provided by national experts and 

advisory committees. 

 Assessing the species concentration information entered into the Air Quality System 

(AQS) database. 
PM2.5 CSN QAPP

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 Developing an information management system and other means to archive data, 

assess data sets, and release trends information to stakeholders, data users, and the 

general public by use of the EPA’s AMTIC QA website. 

 Interacting with Regional, SLT agency personnel and the contracted support 

laboratory concerning the setup and operation of the chemical speciation networks 

and their data results. 

 Ensuring the success of the network by coordinating quality assurance oversight 

activities such as management systems reviews (MSRs) and technical systems audits 

(TSAs).

Most budgetary and technical planning activities will be coordinated through the OAQPS. The 

Ambient Air Monitoring Group (AAMG) within the Air Quality Analysis Division (AQAD) is 

ultimately responsible for facilitating the implementation of the CSN. These responsibilities

include most of the technical components (with support from ORD, Regional Offices and 

laboratories, and SLT agencies) and the resource estimates underlying program implementation. 

The CSN Program Lead and QA Lead provide guidance and oversight for the development of 

the CSN quality system. They also oversee the periodic review and revision of this QAPP. 

Resource guidance necessary for the State and Tribal Assistance Grants (STAG) distribution is 

coordinated through core staff within OAQPS. In addition, the EPA Stationary Source 

Compliance Division (SSCD) is responsible for the AQS data management system.

4.1.2.1 The PM2.5

The CSN-QAL, at OAQPS, is responsible for reviewing and assessing the quality system of the 

CSN. The QAL will:

Chemical Speciation Network Quality Assurance Lead (QAL)

 Review the national network’s QAPP and other quality-related documents and 

coordinate their approval. 

 Ensure that contracted support laboratory’s SOPs are reviewed and updated as 

required. 

 Coordinate with the QA Workgroup, the Regional QA laboratories, ORIA, and others 

to ensure that periodic systems reviews and performance reviews of the field and 

laboratory activities are conducted and completed. 

4.1.2.2 The PM 2.5

The OAQPS Program Lead for the CSN is responsible for the activities that are implemented as 

part of normal data collection activities. His/Her responsibilities include:

Chemical Speciation Network Program Lead

 Communication with EPA POs and EPA QA personnel on issues related to routine 

sampling and QA activities;

 Understanding EPA monitoring and QA regulations and guidance, and ensuring all 

key personnel understand and follow these regulations and guidance; 
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 Viewing acquisition packages (contracts, grants, cooperative agreements, interagency agreements) to determine the necessary QA requirements; 

 Developing budgets and providing program costs necessary for EPA allocation 

activities; 

 Ensuring that all personnel involved in environmental data collection have access to 

any training or QA information needed to be knowledgeable of QA requirements, 

protocols, and technology; 

 Recommending management-level corrective actions.

4.1.3 Advisory Panels

Three advisory panels will consult with OAQPS on technical matters related to the CSN in its 

initial development and deployment. These panels were the CASAC, the Expert Panel on 

speciation, and a panel of ORD/NERL technical experts. 

CASAC—This committee is a subcommittee of EPA’s Science Advisory Board (SAB) and 

reports directly to the SAB administrator. It serves as the principal review body for the PM2.5

Expert Panel on Speciation—The Expert Panel on Speciation was formed during the initial years 

of deployment to advise OAQPS on structural and technical matters related to the PM

monitoring program and continues to review technical issues associated with operation of the 

chemical speciation network. A third level subcommittee, the Air Monitoring subcommittee, 

interacts with the OAQPS and, in particular, with the AAMG on all technical and policy issues 

associated with ambient monitoring.

2.5

speciation network. It was composed of recognized technical experts in the fields of network 

monitoring strategy, sampling and monitoring methods for PM2.5

Office of Research and Development—The NERL provided expertise for helping to review the 

original requirements for the speciation samplers and the analytical methodologies selected for 

quantifying species. This office continues to provide advice on sampling technology, and Federal 

Reference and “Equivalent” methods. 

, physical and chemical 

characterization of fine particles, and data analysis and interpretation. External technical review 

and input will continue to be provided through the CASAC. 

4.1.4 Chemical Speciation Network Contracts Project Officer

The CSN Laboratory Services Contracts PO is on the Central Operations and Resources (CORE) 

staff of EPA/OAQPS. He/She is the liaison between the EPA Contracts Management Division, 

the various contractors and vendors, other program staff in OAQPS related to PM 2.5 Chemical 

Activities, the DOPOs, and the contract laboratory’s Services Program Manager. The primary

role of the PO is to approve and forward delivery orders prepared by the DOPOs to the lab 

services contractor and ensure contract details are followed, including the submittal and review 

of required draft and final annual data summary reports from the contracted laboratory. 
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4.1.5 Regional Speciation Contacts

The PM2.5

4.1.6 Delivery Order Project Officer

RSC in each Region interacts with the SLT agencies and provides assistance on fieldrelated network design and QA issues. The Regional contacts also assist SLTs with procuring 

special equipment or non-routine analyses. The names of the RSCs are listed in a table of CSN 

contacts on the AMTIC website at <http://www.epa.gov/ttn/amtic/specgen.html.> 

The DOPO receives PM2.5

4.1.7 EPA Contracts Management Division 

speciation analytical orders directly from SLT agencies and will 

consolidate the requests for sampling media and sample analysis received from the RSCs. A 

DOPO is assigned to the East (Regions 1-4 and Puerto Rico), Midwest (Regions 5-7), and West 

(Regions 8-10) sections of the United States. The DOPO will communicate with the CSN

Contracts PO and with the contracted support laboratory for analysis of filters and other 

sampling media. The DOPO will also review the monthly analytical data packages from the 

contracted support laboratory, ensure they are complete and, after approval, make arrangements 

for payment of the invoice for the various delivery orders. The names of the DOPOs are listed in 

a table of CSN contacts on the AMTIC website at <http://www.epa.gov/ttn/amtic/specgen.html.> 

The Contracts Management Division (CMD) is located within the Office of Acquisition 

Management (OAM). The CMD is responsible for all communications with vendors and 

extramural contract organizations. For the CSN, the CMD will: 

 Provide a Contracts PO to represent the government; 

 Award national contracts for filter purchases, sample shipping, and laboratory support 

and analyses of speciation sampler filters; 

 Approve work assignments, delivery orders and task orders written by OAQPS or, in 

some cases, EPA Regional Offices, for activities supporting the operation and QA 

programs for the CSN; 

 Communicate with OAQPS to provide the above services. 

4.2 Chemical Speciation Network—State, Local and Tribal Organizations 

Personnel from SLT agencies (Block B of Figure 4-1) install speciation samplers at NCore sites

as well as at other SLAMS sites, operate the speciation samplers at the sites, and recover and 

ship samples to the contracted support laboratory by predetermined schedules. It is the 

responsibility of the SLT personnel to implement quality control (QC) procedures as given in the 

SOPs for sampler operation and sample shipping. The SLT personnel will consult with the 

DOPO and the RSC regarding issues concerning sampling equipment and laboratory supply or 

sample analysis. Interested SLT personnel may also participate in Chemical Speciation 

Workgroup discussions. 

The SLT site operators and supervisors should communicate directly with the contracted support 

laboratory only when there are concerns about timely shipment and receipt of supplies, sampling 
PM2.5 CSN QAPP

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media, and data packages. Field sites will also communicate with OAQPS and with the EPA 

Regional QA laboratories for technical assistance on QA issues. The SLT site operations and 

records will be subject to systems and performance reviews. The EPA Regional CSN contacts 

are expected to conduct full program and technical systems audits of every SLT monitoring 

program at least once every 3 years.

4.2.1 Organization for Routine Field Sampling Operations

The SLT agencies are responsible for day-to-day operation of CSN sites. The management and 

technical organizations already in place at these agencies will be used to implement operations. 

Personnel will need to be assigned and organized to accomplish the following tasks, among 

others: 

 Site selection and platform and utility installations and maintenance. 

 Ensure these data are posted in proper fields of AQS for QA reports. 

 Purchase, receipt, acceptance testing, and installation of sampler, calibration 

equipment, and meteorological equipment and maintenance/replacement of the above. 

 Operator hiring and training. 

 Communication with the RSC and DOPO regarding sample analysis task orders. 

 Scheduled operation of the sampling site, including internal QA/QC activities. 

 Monthly validation of draft data sets received from the contract laboratory within 

specified time constraints. 

 Interactions with CSN network management personnel. 

 Participation in external QA activities such as TSAs and site audits. 

4.2.2 QA/QC Organization for State, Local and Tribal Agency Field Site Operations

Quality assurance activities supporting the CSN sites will be arranged through the QA Manager 

at each SLT agency. The QA personnel will be identified prior to

 Implementation of the quality system for the CSN. 

field data collection and will 

be assigned and organized to accomplish the following tasks, among others: 

 Review and approval of the network’s field QAPP or acceptance of this QAPP as 

the field QAPP. 

 Site inspections (and/or audits) and review of procedures to ensure specified 

QA/QC checks are being made and measurements systems are in control. 

 Email prescribed audit reports to the support contractor for posting flow audit data 

on AQS and other audit results in the speciation audit data-base.

 Issuance of corrective action memoranda and monitoring of follow-up actions. 

 Participation in monthly validation of draft data sets received from the contracted 

support laboratory within specified time constraints. 
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 Arrangement for and participation in QA activities called for by EPA Regional 

Offices.

4.3 CSN Network Laboratory Activities Organization 

Block C of Figure 4-1 illustrates the organization of the CSN laboratory activities. Laboratory 

activities include QA-related work by the EPA ORIA and the contracted support laboratory 

which provides field site filter supply and filter analysis services for the NCore (previously the 

Speciation Trends Network) sites. There are other service laboratories contracted by individual 

SLT agencies that are part of the chemical speciation program; these are also audited by the 

EPA. 

4.3.1 EPA QA Laboratories 

Two of the EPA’s ORIA laboratories work with OAQPS to provide QA oversight of CSN field 

and laboratory activities. These two laboratories are the National Air and Radiation 

Environmental Laboratory (NAREL) in Montgomery, Alabama, and the Radiation and Indoor 

Air (R&IE) laboratory in Las Vegas, Nevada. These laboratories will: 

 Provide speciation laboratory QA support to the state and local agencies and to the 

contracted support laboratories. 

 Provide QA auditing and technical assistance to the field sites and to the contracted

support laboratory. 

 Assist OAQPS in development of training materials and staffing training activities. 

 Communicate with OAQPS regarding QA issues in performance of the Contract 

Laboratory and field operations of the CSN (and supplemental networks). The 

OAQPS will in turn communicate ORIA’s findings on the performance of the 

network to the PO and the RSCs.

4.3.2 Contracted Support Laboratory Organization 

Figure 4-2 illustrates the typical organization of management, QA, and technical staff for the 

PM2.5

Management Organization—The PM

 contracted support laboratory. 

2.5

 Receives and acts on site servicing delivery orders from the EPA DOPOs. 

 contracted support laboratory is headed by a Laboratory 

Services Program Manager and a Deputy Manager. The Laboratory Services Program Manager: 

 Is responsible for returning analyzed filters to SLT agencies that request them. 

 Oversees activities of the technical laboratories and the data management office. 

 Receives and responds to quality systems findings provided by the contracted support 

laboratory QA Manager and staff as well as to findings in external audit reports. 

Quality Assurance Organization—The contracted support laboratory’s QA Office is staffed by a 

QA Manager, a Deputy QA Manager, and support staff. The QA Manager interacts with each of 
PM2.5 CSN QAPP

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the technical area laboratories or offices to conduct scheduled and follow-up systems and 

performance evaluations (PEs). Findings from internal QA activities are reported to the 

laboratory services program manager for review and action. This office summarizes QA 

activities for inclusion in monthly and annual reports to EPA. The QA Office also assists in the 

preparation and update of the laboratory QAPP and associated SOPs. 

Technical Organization—The present contracted support laboratory is composed of seven 

technical components that provide the following analytical services and data report packages to 

CSN sites:

 Sample Handling and Archival Laboratory (SHAL). Supplies each CSN site with 

all necessary sampling supplies to include coated denuders, sampling filter media, 

assembled sampling modules, shipping containers, and documentation paperwork. 

(The hardware is purchased by the state or local organization; the contractor will 

supply only the filters.) 

 Gravimetric and Microscopy Laboratories. PM2.5

 Elemental Analysis Laboratory. Elements and metals by energy-dispersive X-ray 

fluorescence (EDXRF) determination and other methods such as ICP-AES.

mass by microbalance 

determination. 

 Cations/Anions Laboratory. Cations and anions by ion chromatography (IC) 

analysis.

 Carbon Species and Semi-volatile Organic Carbon Compounds Laboratory. 

Carbon species by elemental carbon/organic carbon (EC/OC) analysis. 

Determination of semi-volatile organic compounds (SVOC’s) as requested. 

 Denuder Refurbishment Laboratory. Denuder refurbishment with magnesium 

oxide or other prescribed coating material. 

 Data Management Office. Track sampling media components and manage all data. 

This includes issuance of monthly and quarterly data sets to SLT agencies and to the 

EPA DOPOs and entry of validated data to the AQS database system.

Details on these CSL activities can be found in the laboratory QAPP and associated SOPs for 

this program, which are available on the AMTIC website. 
PM2.5 CSN QAPP

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EPA Project Officer

and

Delivery Order Project Officers 

Quality Assurance Manager

Deputy Quality Assurance 

Manager

QA Support Staff

CSL Services Program 

Manager

CSL Deputy Services 

Program manager

Subcontractors

Technical Advisors

Consultants

Sample 

Handling and 

Archiving Lab 

(SHAL)

Manager

Support Staff

Gravimetric and 

Microscopy 

Labs

Technical 

Supervisor

Support Staff

Elemental 

Analysis Lab

Technical 

Supervisor

Support Staff 

and 

Subcontractors

Cations/Anions 

Lab

Technical 

Supervisor

Support Staff

Carbon 

Species and 

SVOC Lab

Technical 

Supervisors

Support Staff 

and 

Subcontractors

Denuder 

Refurbishment 

Lab

Technical 

supervisor

Support Staff

Data 

Management 

Office

Technical 

Supervisor

Support Staff

Services 

Program 

Manager

Data Set 

Releases

§ State/Local

§ EPA DOPO

§ AQS

Services 

Program 

Manager

Send/Receive 

Sampling 

Media

§ State

§ Local

§ Tribal

§ EPA Regions

Figure 4-2. Laboratory Technical Management and Staff Organization for CSN Filter 

Analysis and Data Reporting. 
PM2.5 CSN QAPP

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5.0 Background and Problem Definition

For environmental pollutants, the term particulate matter (PM) is used to describe a broad class 

of chemically and physically diverse substances that are either natural in origin, emitted directly 

from stationary and mobile sources, or formed in the atmosphere by reactions of gaseous 

emissions such as nitrogen oxides, sulfur dioxide, and volatile organic compounds (VOCs). 

5.1 Background 

The Clean Air Act (CAA) requires EPA to revise or update the air quality standards based on 

review of the latest scientific information on known and potential human health effects 

associated with PM levels typically found in the ambient air. In fulfilling these obligations, the 

EPA in the mid-1990’s, reviewed the air quality criteria and National Ambient Air Quality 

Standards (NAAQS) for PM. The epidemiological evidence revealed an association between 

ambient concentrations of PM and a range of serious health effects. Based on the results of its 

review, the EPA revised and promulgated two new primary standards for the fine fraction of PM 

(i.e., particles with aerodynamic diameters less than or equal to 2.5 μm, referred to as PM2.5) and 

issued regulatory requirements for monitoring the chemical composition of these particles. The 

EPA, with state, local, and Tribal (SLT) agencies and EPA Regions, designed a chemical 

speciation network projected to consist of approximately 300 monitoring sites, to monitor and 

gather data on the chemical makeup of PM2.5. The EPA designated 54 of the sites for tracking

temporal trends in concentration levels of selected ions, metals, carbon species, and organic 

compounds in PM2.5. The implementing regulation further required that approximately 25 of the 

trends samplers be placed at existing Photochemical Assessment Monitoring Stations (PAMS). 

The locations for the remaining chemical speciation trends sites were primarily in or near larger 

Metropolitan Statistical Areas (MSAs); data from these sites were to enhance the required trends 

network and to provide information for developing effective State Implementation Plans (SIPs). 

The balance of the 300 chemical speciation sites, dubbed “supplemental,” were to be deployed at 

either PM2.5 State and Local Air Monitoring Sites (SLAMS) for better spatial representation of 

community scale or rural background air sheds, or for specially selected source attribution sites. 

Selection of the SLAMS and other locations for supplemental chemical speciation was left up to 

the particular monitoring organization. Approximately 50 of the supplemental speciation sites 

selected for rural background were permitted to utilize Interagency Monitoring of Protected 

Visual Environments (IMPROVE) samplers as described below. These are called IMPROVE 

protocol sites. The combined Speciation Trends Network (STN) and supplemental network, 

including IMPROVE protocol sites, reached its zenith in 2004 at around 325 sites.

The IMPROVE samplers were originally designed to help quantify visibility impairment in our 

nation’s Class 1 areas. When the Regional Haze rules were promulgated in 1999, the IMPROVE 

and IMPROVE protocol network were adopted as the network to measure the baseline year 

concentrations and subsequent trends of haze-forming aerosols in Class 1 areas. The IMPROVE 

sampler measures essentially the same attributes of fine particulate as the Chemical Speciation 

Network (CSN) samplers. However, it uses a flow rate of 22.7 liters per minute and it employs a 

smaller filter (25 mm). A typical IMPROVE station also incorporates a PM10 collection channel. 
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The primary analytical protocols for total mass, trace metals and anions are very similar, but 

carbon quantification in the CSN (a Thermal Optical Transmittance (TOT) method) until 2007 

was procedurally different, and the data reflected a small but noticeable bias. The URG 3000N 

replaced all the legacy carbon samplers of the STN and supplemental CSN in 2007-2009. It was 

deployed to make carbon measurement in the CSN the same as the IMPROVE network. It uses 

the sample filter media, sampler module and flow rate as the IMPROVE sampler. The only 

significant difference is that the URG uses a mass flow controller to assure the flow remains 

constant over the 24-hour sampling period. The same analytical procedure used by IMPROVE 

(Thermal Optical Reflectance (TOR) “Method A”) is now used by the CSN to quantify the 

carbon constituents on the URG 3000N quartz filter. In a rulemaking by EPA (71 FR 61236, 

October 17, 2006), a new designation of monitoring sites was adopted as part of a revised 

national monitoring strategy. The NCore strategy called for PM2.5 chemical speciation trends 

sites to be incorporated into NCore sites; however, a few adjustments were anticipated. NCore

sites will employ filter-based PM speciation sampling and analyses along with a myriad of other 

monitoring protocols including new generation trace gas measurements for ozone (O3), carbon 

monoxide (CO), sulfur dioxide (SO2), and nitrogen oxide (NOY) (all reactive oxygenated 

nitrogen gases). NCore sites will continue to emphasize ambient concentration trends. The total 

size of the filter-based PM2.5 CSN has shrunk from its initial 300 plus sites to between 150 and 

200 sites which includes approximately 80 NCore sites and still more than 40 IMPROVE 

protocol sites. The overall numbers will change further in the future, but the NCore sites should 

operate indefinitely. Figure 5-1 illustrates the interrelationships of the CSN and the 

IMPROVE/IMPROVE protocol networks. 
PM2.5 CSN QAPP

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Note that this Quality Assurance Project Plan (QAPP) still pertains to the filter-based 

collection and measurement of speciated PM2.5. IMPROVE protocol sites that are part of 

the CSN network are subject to siting criteria of the CSN and IMPROVE, but their 

operating procedures and data management are subject to the IMPROVE QAPP and 

standard operating procedures (SOPs). The IMPROVE network operates under its own 

QAPP for the purposes of supporting the assessment of visibility impairment and regional 

haze. Those documents may be found on the IMPROVE website 

http://vista.cira.colostate.edu/improve/Publications/publications.htm; or through a link on 

AMTIC at http://www.epa.gov/ttn/amtic/qapollutant.html. 

5.2 Problem Definition 

The CSN is a complementary network to the National PM2.5 Mass Monitoring Network (whose 

goal is to measure ambient concentrations to be compared against the PM2.5 NAAQS). The CSN 

data have not been used for attainment or nonattainment decisions related to PM2.5

 Annual and seasonal spatial characterization of aerosols; 

mass but its 

use for other regulatory purposes, such as visibility and SIP development, are possible in the 

future. The programmatic objectives of the CSN network are to provide: 

 Air quality trends information for analysis and tracking the progress of SIP control 

programs; 

 Data to assist in development of emission control strategies; and

 A chemical speciation data set for comparison to the data collected from the

IMPROVE network. 

Primary stakeholders in the CSN are decision-makers of SLT agencies, who will use the data as 

input to models and for development of emission control strategies and determination of their 

long-term effectiveness. Secondary stakeholders will include EPA analysts who will use CSN

data to determine trends of PM2.5 chemical species over a period of 3 or more years, to relate the 

data to health effects, and to develop and evaluate air quality models. Other users will be public 

health officials and epidemiological researchers. However, expectations for data sets from the 

CSN must be put in context. A number of limitations are recognized, one being the 24-hour 

integrated sample approach with samples taken every 3rd

The measurement quality objectives stated in the IMPROVE QAPP are more stringent than those 

of the CSN. To the extent that the IMPROVE data quality is found comparable to or better than 

the CSN data, IMPROVE’s data may also be combined with CSN data in the analyses conducted 

for the trends and other monitoring objectives stated in Chapter 7. 

day, which cannot allow determination 

of diurnal patterns and may have limited use for those who study acute health effects. The EPA 

recognizes these data use limitations as well as limitations of the sampling and analysis 

methodologies. Thus, the EPA does not rule out the possibility that objectives, requirements, and 

methods for speciation sampling may need to be adjusted in the future. 
PM2.5 CSN QAPP

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5.3 PM2.5

PM

Speciation Sampling Techniques and Ongoing Research

2.5 speciation samplers are designed to collect 24-hour integrated samples on three different 

filter media (polytetrafluoroethylene [PTFE], nylon, quartz). The CSN network samplers covered

by this QAPP are the MetOne SASSTM (spiral ambient air sampler) and Super SASS, and the 

URG 3000N carbon sampler.1

The MetOne SASS and SuperSASS samplers use PTFE, nylon, and quartz filter media for the 

collection of target analytes. The PTFE filter is used to collect particles for the analysis of mass 

and metals composition; samples for ion analysis are collected on nylon. A few MetOne 

samplers still collect carbon components on quartz, but the URG 3000N is the primary carbon 

sampler. It is limited to only carbon. Each sampler’s operating manual and the corresponding 

field operations SOP (refer to Appendix A) should be consulted for further details. New 

prototype semi-continuous samplers have been developed for sulfates, carbon containing species 

and trace elements. Their comparability to the filter-based sampling techniques have not been 

established to date; consequently this QAPP will not apply to their utilization.

The design and operation of the 3000N sampler is modeled after 

IMPROVE network samplers. Appendix A to this QAPP provides SOPs for the SASSTM and a 

detailed SOP for setup and operation of the URG 3000N sampler. 

5.4 Monitoring Network Design Considerations

The initial design of the old Trends network was influenced by the need to place sites primarily 

in populated areas of the country and to link PM2.5 speciation data sets to data collected at 

collocated PAMS and PM2.5 mass sampling sites. Appendix D of the Part 58 PM2.5 regulations 

(62 FR38763) provides the general criteria to apply in choosing new monitoring stations for 

PM2.5

The initial selection of the remaining (trends) sites was based on EPA recommendations, with 

review and advice from state and local agencies. Most of the remaining sites were located in 

MSAs. Their specific locations were based on factors such as:

. General requirements for the Trends network specified that approximately 25 sites must 

be located at existing “type 2 PAMS sites.” (PAMS network design and monitoring objectives 

are explained in Code of Federal Regulations (CFR), Part 58 Appendix D.) 

 Location of existing PAMS. 

 Geographic locations of MSAs using the latest available population statistics. 

 Ozone nonattainment areas. 

 PM10 nonattainment areas. 

 

1 Historical speciation samplers included the R&P Model 2300, the URG MASS (mass aerosol speciation sampler) 

400 and 450, and the Andersen RASSTM (reference ambient air sampler) 401and 410. These are no longer supported 

by their manufacturers and have been replaced by the SuperSASS and URG 3000N. SOPs for the MASS and 

RASSTM samplers are found in the December 2000 version of the QA Project Plan for PM2.5 Speciation Field 

Sampling which is available from the EPA Ambient Monitoring Technical Information Center (AMTIC) website.
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CSN supplemental sites were initially placed at the one MSA community-oriented PM2.5

Sites placed at population centers in the central, midwest, and southeast portions of the country, 

brought the total number of PM

federal 

reference method (FRM) mass site that has exhibited the maximum concentration in the area. 

2.5

The strategy for the NCore network was to incorporate as many existing PM

 speciation trends sites to a maximum of 54. This number 

decreased to 52 in 2009 and may change further as the national monitoring strategy evolves. 

2.5 speciation trends 

sites as feasible. Locating speciation trends sites at NCore provides PM2.5

For further information on the existing locations of PM

particulate matter 

speciation data to complement and supplement NCore gaseous pollutant and meteorological 

measurements. By mid-2009, about 2/3 (38) of the original 52 trends sites were included in the 

NCore network design. It is likely that a few of the original trends sites may change location. 

The remaining 14 STN sites will continue with their designation monitoring objective, but they 

will be considered part of the CSN. The national air monitoring station (NAMS) designation was 

eliminated by the October 2006 rulemaking. 

2.5

Refer to Section 10.0 for further information on the sampling process design for the PM

 speciation sites in the CSN, including 

trends sites that are to be located at the NCore sites, refer to the EPA AMTIC website. 

2.5

5.4 Monitoring Site-Specific Design Considerations

CSN. 

The CSN sampler siting criteria is based on that established for the PM2.5 FRM network. Key 

requirements are set out in 40 CFR part 58 as follows 

APPENDIX A Section 3.2.5.6 states

“The two collocated monitors must

be within 4 meters of each other and at least

2 meters apart for flow rates greater than 200

liters/minute or at least 1 meter apart for samplers

having flow rates less than 200 liters/

minute to preclude airflow interference.”

APPENDIX E: PROBE AND MONITORING PATH SITING CRITERIA FOR 

AMBIENT AIR QUALITY MONITORING, in addition to the Appendix A requirements, 

are summarized below. 

1. Inlets should be >20 meters from the drip line of tree(s) and must be 10 meters from the 

drip line when the tree(s) act as an obstruction.

2. Distance from sampler, probe, or 90 percent of monitoring path to obstacle, such as a 

building, must be at least twice the height the obstacle protrudes above the sampler, 

probe, or monitoring path. 

3. Inlet must have unrestricted airflow 270 degrees around the probe or sampler; 180 

degrees if the probe is on the side of a building. 
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4. The probe, sampler, or monitoring path should be away from minor sources, such as 

furnace or incineration flues. The separation distance is dependent on the height of the 

minor source’s emission point (such as a flue), the type of fuel or waste burned, and the 

quality of the fuel (sulfur, ash, or lead content). This criterion is designed to avoid undue 

influences from minor sources. 

5. Distance from roadways may be an important decision based on the monitoring 

objectives for the particular site. Appendix E Section 6.3 covers these criteria. 

All siting criteria should be discussed in the Monitoring Agency’s monitoring plan and approved 

by the EPA Regional Monitoring Program. The Region may also grant exemptions from some 

siting criteria. 
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6.0 Project/Task Description

This section provides PM2.5

6.1 Description of the Work to be Performed

Chemical Speciation Network (CSN) participants with a background 

understanding of the CSN program and the types of activities to be conducted which include: 

acquiring the samples; performing chemical analysis; carrying out quality assurance/quality 

control (QA/QC) procedures to achieve data quality goals; and meeting the schedules for 

continued network implementation, operation, and data reporting. 

6.1.1 Overview of CSN Operations

The operation of the CSN is a series of interrelated field and laboratory activities. Figure 6-1 

depicts ten steps involved in implementing and operating a site in the network and the 

delineation of responsibilities for required tasks. Each step or set of activities is briefly described 

below: 

1. The PM2.5

2. The site contact conveys the site’s needs with respect to the requirements for number 

and type of sample filters, denuders, and sample analyses to the Delivery Order 

Project Officer (DOPO). The DOPO consolidates several requests and informs the 

contract laboratory’s Services Program Manager (SPM) of each site’s address, point 

of contact, sampling schedule, needed sampling equipment and filter media, and suite 

of analytes. The lab support contract project officer at the Office of Air Quality 

Planning and Standards (OAQPS) authorizes the contract laboratory to begin 

supplying the site, analyzing samples received, and sending analytical results. 

CSN site contact person makes arrangements for purchase and delivery of 

sampling equipment to the site. Information about field site contact names, mailing 

and shipping addresses, telephone numbers, supplies, and the sampling schedule is 

sent to the Regional Speciation Coordinator (RSC) by the site contact person or other 

state, local and/or Tribal (SLT) coordinator. The requirements for number and type of 

sample filters, denuders, and sample analyses are sent to the RSC as information only. 

3. The analytical support laboratory ships sampling supplies to the site contact address. 

4. Site personnel conduct sampler quality control checks (e.g., time and date, leakage, 

temperature, barometric pressure, flow rates, and cleanliness), conduct QC checks on 

the meteorological sensors, if present (e.g., examine anemometer and wind vane for 

damage; check real-time data display for wind speed, wind direction, temperature, 

and relative humidity against independent observations), collect the PM2.5

5. Site personnel ship routine samples and field data to the contracted support 

laboratory. (Sometimes non-routine and quality assurance samples are sent to the 

designated EPA QA laboratory. The RSC informs the site when there are non-routine 

or QA samples and how and where to send them.) 

samples, 

deploy and retrieve field or trip blanks, pack all samples, complete the custody and 

field data forms, and download data stored in the sampler’s memory to an electronic 

storage device. 
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6. The contracted support laboratory analyzes filter samples and conducts level 0 and 

level 1 data validation. The data are sent to the state and locals who review and accept 

the levels 0 and 1 validated data or provide edits. The information is sent back to the 

contracted support laboratory which corrects data. The contracted support laboratory 

makes final Air Quality System (AQS) database entry.

7. The contracted support laboratory archives filter extracts for 6 months. The 

contracted support laboratory archives the polytetrafluoroethylene (PTFE) and carbon 

filters and will dispose as directed by EPA at the end of their contract. Upon request, 

the laboratory sends filters back to the reporting organizations that wish to store 

filters for a longer period of time. 

8. The contracted support laboratory prepares monthly analysis and QA/QC activity 

reports. 

9. The contracted support laboratory submits the monthly analysis report to CSN site 

personnel for review, further validation, and verification. This report is also submitted 

to the DOPO.

10. The SLT personnel conduct levels 2 and 3 data validations; questions about results 

are directed to the laboratory through the DOPO. Data users and stakeholders 

interpret and summarize the validated data sets to detect trends according to their own 

established protocols. 

Figure 6-1. CSN Activities and Responsibilities
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Table 6-1 lists critical field and laboratory measurements for the PM2.5

Table 6-1. Critical Measurements in the PM

CSN and gives the 

methods to be used to acquire the data. Consult the EPA Ambient Monitoring Technical 

Information Center (AMTIC) website for updates.

2.5 CSN 

Parameter and/or Analyte Methodology

Field Site

Site name, sample date, and sample ID

Temperature, ambient (Celsius) Commercial speciation sampler’s sensor

Temperature, ambient (Celsius)** Meteorological package

Relative humidity (percentage)** Meteorological package

Pressure, atmospheric (mmHg) Commercial speciation sampler’s sensor

Date and elapsed sample time (h) Commercial speciation sampler’s clock and timer

Flow rate, sampler (L/min)*** Commercial speciation sampler’s flow rate sensor

Total volume sampled (m3) Commercial speciation sampler’s display

Wind speed (m per s)** Anemometer of meteorological package

Wind direction (degrees of compass)** Wind vane of meteorological package

Free-form notes on sampling difficulties and unusual 

conditions at the site

Analytical Support Laboratory

Temperature, shipment container (Celsius) Digital thermometer

Mass, PM2.5 (PTFE filter) (μg/filter and μg/m3 of air) Balance, microgram

Elements (PTFE filter) (μg/m3 Energy-dispersive X-ray fluorescence (EDXRF) (Na 

through Pb)

)

Cations (various filters) (μg/m3) Ion chromatography (IC) (NH4

+

, Na+, K+)

Anions (various filters) (μg/m3) IC (nitrate, sulfate)

Carbon species (quartz filter) (μg/m3 Thermal/optical analysis (total, organic, elemental, and 

carbonate carbon)

)

** Meteorological measurements required at NCore sites; optional elsewhere.

*** Flow rates are measured by samplers over 15 minute periods and is averaged for 24-hour events

6.2 Field Activities 

6.2.1 Checklist of Field Activities

From the perspective of field QA there are two key areas of concern. Making sure the sampler 

operates at the design flow rate with little variability and minimizing sample contamination. 

Strict attention to procedures and constant awareness of the possibility for sample contamination 

are keys to obtaining a valid sample. Table 6-2 lists the activities the field site operator is 

expected to accomplish for the CSN. The table also gives the frequency at which the activity 

should be performed. 
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Table 6-2. Checklist of PM2.5 CSN Site Operator Field Activities

Activity Frequency Comment or Reference

Attend hands-on training sessions. Update training via 

website or other means.

Once, prior to site operation. 

Updated training as required.

See Section 8.0, this 

document

Assist with equipment selection, contact with RSC, 

and ordering of laboratory analytical services. 

Once, prior to beginning site 

operation or after request of 

new equipment.

Equipment (sampler, calibration or verification 

devices, and so on) receipt, inspection, inventory, and 

operability checkout. Maintain spare parts inventory.

Once, initially, and whenever 

new or replacement parts 

arrive.

Quality Assurance

Guidance Document 

2.12, Section 4

Install sampler(s) at site. De-installation of sampler(s) 

at site.

Once, at beginning of CSN

participation. Again if site is 

moved or closed.

Refer to Appendix A-1 of 

this QAPP

Sampler calibrations. Prior to first sampling event; 

annually thereafter or whenever 

out-of-tolerance checks occur 

that cannot be corrected; 

following repairs affecting flow 

rate.

Refer to Appendices A-2, 

A-3, and A-4 of this 

QAPP

QC checks of sampler operation (checks of time and 

date display, leaks, ambient and interior temperature 

sensors, pressure sensor, and flow rate).

Check dependent; see Table

14-1

Refer to Table 14-1

Appendices A-2, A-3, and 

A-4

Sampler operation. Includes preventive maintenance, 

maintaining sampler cleanliness, installing denuders 

and sampling media, programming sampler start/end 

times, and keeping field activities notes in site logbook 

and/or on field data forms. 

NCore and Trends sites every 

3rd day with dates and start/end 

times specified by EPA. Some 

non-trends sites sample every 

3rd

Cleaning process must be 

thorough and avoid 

contamination of sample 

pathways

day and others every 6th 

day.

Retrieval and packaging of samples, field blanks, and 

denuders into shipment container. Completion of 

custody and field data forms, and shipment of samples 

to laboratory via overnight express service. 

Per frequency of sampler 

operation or as specified in 

Section 6.4 to coincide with 

laboratory supplied filters and 

deunders.

Refer to 

Appendix A-1, & A-2 

Data download and retrieve data memory card from 

sampler. Store download data from MetOne samplers 

to the compact flash card of the URG 3000N.

At time of each filter retrieval 

or as soon thereafter as 

practicable

Pay close attention to card

insertion and removal 

procedures in the URG 

3000N SOP, Appendix A2 and Operator’s Manual.

For the MetOne 

SASS/SuperSASS refer to 

Appendix A-1 and 

MetOne SASS COM AQ 

instructions

Participate in data validation as needed. Review initial 

data from laboratory; conduct levels 2 and 3 data 

validation†

Initial training. Follow-up 

sessions. Monthly review of 

. Inform DOPO and the lab SPM of data data sets.

acceptability.

Communicate with state or local management, CSN

management, and contract laboratory (through 

DOPO).

As required and appropriate.
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Activity Frequency Comment or Reference

Participate in scheduled CSN QA activities (for 

example, on-site and field office inspections, handling 

of special QA samples, installation and periodic 

operation of a collocated sampler).

As scheduled by Monitoring 

Agencies QA program or EPA 

Office of Air Quality Planning 

and Standards (OAQPS) or 

EPA Regional QA Officers.

See Section 14, Table 14-1 of 

this QAPP for specific

frequency

† The contract support lab will conduct a level 0 and level 1 validation but the field operators must 

participate by accurately entering data on the COC and field data form (CAFDS), and then they must 

review the data that have been recorded to accompany the results to make sure there are no 

transcription errors. They would participate in levels 2 and 3 validations when the SLT data analyst 

inquires about specific sampling results and associated meta data.

6.3 Laboratory Activities

The CSN requires extensive laboratory activities. A single contracted network support laboratory 

(with subcontractors) is employed for analysis of routine samples from the network. The 

following subsections and figures summarize the laboratory activities that support the CSN. 

6.3.1 Pre-sampling Activities

1. PTFE, nylon, and quartz filters are received from various vendors and examined for 

integrity and background analyte concentrations.

2. Filters (or their containers) are numbered or otherwise identified to allow tracking and 

accurate data entry.

3. Filters are conditioned, tested, equilibrated, and weighed as required and stored 

awaiting use.

4. Filters are packaged in various filter holders or sampling modules that are specific to 

the type of sampler to be used at the field site. 

5. The laboratory maintains shipping/receiving supplies to include shipment containers, 

ice substitute packs, and custody and field data forms.

6. Assembled sampling modules including denuders are shipped to sampling sites on a 

pre-determined schedule.

6.3.2 Post-sampling Activities

1. Shipments of sampling modules containing filters bearing PM2.5

2. Filters are placed in labeled containers which are stored (refrigerated or frozen) until 

ready for analysis.

 deposits are received 

in the laboratory, checked for integrity (damage, shipment temperature, and so on), 

and logged in. Information on the custody and field data form is reviewed.
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3. Filters and denuders intended for analysis of acidic or basic gases are promptly 

distributed to individual laboratories for weight determination and other analyses so 

that strict time frames for completion of activities are met.

4. Results of analyses are entered into the laboratory database.

5. Sampled volume data are entered into the data entry system in order to calculate 

concentrations of species in terms of a mass per unit volume of air sampled (μg/m3

6. Filters and filter extracts are archived (frozen or refrigerated) for 6 months or longer 

if requested.

).

7. Data are electronically posted for examination by the DOPO and the designated SLT

contact for each CSN site. After edits and approval, the service laboratory uploads 

data to the national AQS database. The reporting schedule is set-up with the 

laboratory through the contract, but it is consistent with the reporting schedule for the 

PM2.5 

8. All paperwork, including custody and field data forms, chromatograms, thermograms, 

analyzer data reports, results of QA/QC studies, and free-form notes, are filed for 

ready retrieval and inspection as required for at least a 3-year period. 

FRM network reporting requirements at 40 CFR Part 58.16. 
PM2.5 CSN QAPP

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The details for these activities are included in the laboratory SOPs, which are part of the 

contracted support laboratory’s QAPP available on the EPA AMTIC website. Figure 6-2 is a 

simplified flow diagram of the sample analysis delivery order process. Figure 6-3 is a flow 

diagram of handling and analysis steps for the filters. 
PM2.5 CSN QAPP

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Mass and Elements 

Sodium-Lead

PTFE Teflon

Acceptance Testing

Pre-sampling 

Gravimetry

PTFE Teflon

Equilibration

Acceptance Testing

Prefiring

Quartz

Carbon: Total, Organic, 

Elemental and Carbonate

X-Ray Fluorescence 

Elements SodiumLead

Post-sampling 

Gravimetry Mass

Field Sampling

Transfer to the Field

Transfer to the 

Laboratory

Quartz

Filter and extract 

handling

Thermal Optical Analysis 

Total, Organic, and 

Elemental, Carbonate 

Carbon

Database: AIRS-AQS 

Input

Refrigerated

Storage

Cations: Ammonia Sodium, 

Potassium

Anions: Nitrate, Sulfate

Refrigerated Storage 

and Archive for possible 

Re-analysis

Nylon

Washing

Acceptance Testing

Nylon 

(Teflon in case of 

URG samples)

Ion Chromatography 

Ammonium, Sodium, 

Potassium, Nitrate, and 

Sulfate

Filter Extraction

Figure 6-3. Diagram of laboratory filter processing and analysis activities, by filter type. 
PM2.5 CSN QAPP

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6.3.3 Critical Laboratory Processes and Measurements

In order to generate a mass concentration, the most critical measurements of the laboratory are 

the unexposed filter preweights and the exposed filter postweights or concentrations in terms of 

μg/filter. The difference between these two measurements provides the net weight of particles (or 

particle components) in micrograms (μg) that, when divided by the field sampler air volume in 

cubic meters (m3), provides a final concentration in micrograms per cubic meter (μg/m3

6.4 Schedule of Activities

). Table 

6-1 lists all the analytes to be quantified for the CSN samples. 

Whenever a new or relocated CSN or other type PM2.5

6.4.1 Planning Time Lines

speciation sampling site comes on-line, 

many aspects of the program must be completed in a timely, efficient fashion in order to meet 

goals for data quality and timelines for data review and reporting.

Table 6-3 outlines the sequence of activities for bringing a PM2.5

Table 6-3. Sequence of Activities for Bringing a PM

CSN field site on-line. 

2.5 CSN Field Site On-Line

Activity Notes

Select sites. Arrange for space, electrical power, 

personnel.

Ensure siting criteria are met.

Order speciation sampler(s) and accessories. Confer with EPA Regional Office and OAQPS prior to 

ordering to confirm sampler selection 

Acquire 10-m meteorological tower and sensor 

package, if appropriate.

Confer with EPA prior to ordering.

Order only if needed at site(s).

Review conditionally approve CSN quality assurance 

project plan (QAPP) and pertinent standard operating 

procedures (SOPs).

Receive and inventory sampler(s) and spare parts. Contingent on vendor schedule.

Confer with Regional Speciation Coordinator (RSC) 

and others.

Finalize mechanism and schedule for delivery order 

process for routine, non-routine, and QA samples.

Attend training sessions and/or review training video. Consult EPA’s OAQPS and EPA Regional Offices for 

plans.

Complete site preparation and sampler installation. 

Conduct safety and security checks.

Conduct acceptance tests per Table 15-1. Obtain site 

documentation and photographs/slides for site file.

Establish communications with contracted support 

laboratory to set date for first series of sample 

collections.

Request filters, data sheets, etc., from contracted support 

laboratory.

As needed, conduct hands-on training at site. Collect 

one or more 24-hour test samples and complete data 

transcription and documentation.

Involve field staff, RSC, support laboratory, and OAQPS 

as required.

Begin routine, every 3rd-day speciation sampling at Refer to every 3

CSN trend sites and frequencies for other SLAMS 

CSN sites as adopted by the monitoring agencies.

rd, 6th,12th -day sampling schedules on 

AMTIC website.

Conduct routine field QA activities and participate in 

independent audits and program assessments. 

As scheduled or requested, interact with RSC.
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Activity Notes

Review data and conduct level 2 and level 3 

validations of monthly data reports received from 

laboratory.

Each month. Complete review within 30 days. Interact with 

RSC and OAQPS to resolve problems.

Report problems and suggestions for improvement to 

SLT management.

As required, interact with RSC and OAQPS.

6.4.2 Implementation Time Lines

Other important dates must be met during implementation activities at a new site. They involve 

both laboratory and field activities. One aspect of the field site implementation process that is

critical is the time-efficient use and return of denuders and filter media to the support laboratory. 

As shown in Table 6-4 and stipulated in the Code of Federal Regulations (CFR), PTFE filters 

must be used at the field site within 30 calendar days of presampling weighing or they must be 

reconditioned and reweighed. Furthermore, the contracted support laboratory must submit 

validated speciation concentration data to the EPA within 20 business days following receipt of 

any sample from the field. Therefore, it is critical that the laboratory and the field sites develop, 

agree on, and consistently follow a schedule that will satisfy the requirement that the mass of 

PM2.5

6.4.3 Field Time Lines

 on PTFE filters be determined within 10 days after the sampling period ends and that 

determination of all analytes be completed, validated, and submitted to the DOPO and site 

contact person for review and acceptance within 20 business days. 

Table 6-4 indicates that sample filters collected by a single event sampler or a sampler run in a 

single event mode should be collected and be prepared and ready for shipment to the laboratory 

within 48 hours of the end of the sample period in order to prepare for the next 1-in-3 day

sampling period. In some circumstances, this may not be practical or possible. If the agency 

cannot collect the samples on a weekend, then an alternate schedule must be adopted. This 

should be noted on the chain of custody form. Any other instance where a sample is not shipped 

within 48 hours should also be noted. Refer to the AMTIC website for information on alternate 

schedules. The EPA is also allowing a 110-hour retrieval and shipping schedule for filters used 

in a sampler that is operated in a sequential mode typically due to an inability to perform weekend or holiday retrievals. This applies to the first sampling event filter generated in the sequential 

two event series. The second event filter is still subject to the normal 48-hour retrieval and 

shipping requirement. If the monitoring agency has concerns over loss of semi-volatile mass, the 

operator may retrieve the first set of MetOne PTFE and nylon filters on the first work day 

following the first sequential sampling event. This can be done while the sampler is engaged in 

the second of the sequential events. Data should be downloaded or removed via memory card or 

other storage device from the speciation samplers on the day of filter sample retrieval. Data 

should be stored on two media, one serving as the backup. In addition, the most critical data 

values must also be hand-recorded from each sampler’s display screens onto the sample custody 

and field data form (supplied by the contracted support laboratory) and sent back to the 

laboratory with the samples. The CAFDS is the form to be completed for the CSN; examples of 

this form for the MetOne SASS and SuperSASS and the URG 3000N are found in Section 12. 
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Table 6-4. Critical Filter and Denuder Holding and Use Times 

(*) Special deadlines for use and shipment may apply to field blank and collocated sampler filters.

(**) MetOne SASS sampler denuder is integral to the ion sampling module and are serviced by the contracted 

support laboratory.

6.4.4 Data Assessment Time Line

Data Availability—In order to compare the PM2.5 speciation and PM2.5 routine FRM or FEM 

samplers’ mass data, data from the routine FRM or FEM sampler must also be available in AQS. 

“Routine sampler” refers to the gravimetric only network sampler which is always present at a 

NCore or CSN Trends site. State/local requirement for data upload to AQS is 90 days after the 

quarter in which the data were collected. However, the time frame for pre- and post-sampling 

weighing is now more rigid than the PM2.5 total mass network, as indicated in Table 6-4. The 

reason for this is to minimize any losses of semivolatiles or formation of secondary PM that was 

not on the filter at the time it is retrieved. This requirement is written into the support 

laboratory’s contract with OAQPS. The ability to include a comparison of data acquired with 

speciation monitors with that of FRM or FEM samplers at the same monitoring site in a level 

1validation is contingent on the availability of the FRM or FEM routine sampler data within the 

20 business day window. The SLT may have a better opportunity to make this comparative 

assessments during levels 2 and 3 validations. Assessments—after both routine (gravimetric mass 

only) data and speciation data for a site are in the AQS database, OAQPS, Regions, and SLT

agencies can use the AQS data evaluation programs, based on data quality assessment (DQA) 

techniques, to assess this information. This assessment is part of the level 2 and level 3 data 

validation process. Consult the AMTIC website for information on use of the Special Data 

Validation Tool (SDVAT) program for statistical assessment of data sets.

Filter or Denuder Type Field Deadlines Laboratory Deadlines

PTFE (*) Use within 30 days of preweighing; 

retrieve and ship within 48 hours of 

sample completion or 110 hours 

following first event of sequential 

sampling. 

Condition and reweigh within 10 

business days of receipt from field 

site.

Quartz (*) Retrieve and ship within 48 hours of 

sample completion or 110 hours 

following first event of sequential 

sampling.

Analyze filter deposit within 20 

business days of receipt of sample.

Nylon (*) Retrieve and ship within 48 hours of 

sample completion or 110 hours 

following first event of sequential 

sampling.

Analyze filter deposit within 20 

business days of receipt of sample.

Nitric acid denuder (magnesium 

oxide) MetOne SASS sampler .(**)

Replace each denuder after 3 months 

use.

Refurbish or replace as required.
PM2.5 CSN QAPP

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6.4.5 OAQPS Reporting Time Lines

QA Reports—The OAQPS prepares a yearly QA Final Report and an interpretive QA report 

every 5 years to coincide with the data quality objectives. The yearly report beginning in 2012 

will be based on the past calendar year but will include a 2-year look back on key QA and QC 

elements. It is completed 6 months after the last valid entry of routine data in the preceding 

calendar year’s data base. The 5-year QA report is generated within 12 months after the last valid 

entry of routine data in the fifth year by the state and local agencies. 

6.5 Project Assessment Techniques

An assessment is an evaluation process used to measure the performance or effectiveness of a 

system and its elements. As used here, assessment is an all-inclusive term used to denote any of 

the following: management systems reviews, network reviews, technical system audits, 

performance evaluations, and audits of data quality. Table 20-1 specifies the regions, 

laboratories, and agencies responsible for these assessments.

6.6 Project Records

The field and contract laboratory programs will establish and maintain procedures for the timely 

preparation, review, approval, issuance, use, control, revision, and maintenance of documents 

and records. Refer to Table 9-1, CSN reporting Package Information, for the categories and types 

of records and documents applicable to document control for PM2.5

6.7 References

 sampling and analysis. 

Information on key documents in each category is explained in more detail in Section 9.0 of this 

QAPP. 

1. Quality Assurance Guidance Document 2.12. Monitoring PM2.5 in Ambient Air Using

Designated Reference or Class I Equivalent Methods. US EPA, November 1998, Available at 

http://www.epa.gov/ttn/amtic/files/ambient/pm25/qa/m212covd.pdf. 

2. SDVAT Speciation Data Validation Tool. Information and program available at: 

http://www.epa.gov/ttn/amtic/sdvat.html. 
PM2.5 CSN QAPP

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7.0 Quality Objectives and Criteria for Measurement Data

7.1 Data Quality Objectives Process

The data quality objectives (DQO) process is a strategic planning approach used to prepare for a data 

collection activity in order to achieve data of adequate quality to support decision-making. The DQO 

process helps to ensure that the type, quantity, and quality of environmental monitoring data will be 

sufficient for the data’s intended use, while simultaneously ensuring that resources are not wasted 

collecting unnecessary, redundant, or overly precise data. The formal DQO process consists of the 

following seven steps that allow an experimental design to be developed to meet specific decision 

criteria specified by stakeholders in the decision, as described in EPA QA/G-4, Guidance on Systematic 

Planning Using the Data Quality Objectives Process (U.S. Environmental Protection Agency, 2006):

 State the problem.

 Identify the decision. 

 Identify the inputs to the decision. 

 Define the boundaries of the study. 

 Develop a decision rule.

 Specify tolerable limits on decision errors.

 Optimize the design.

A Chemical Speciation DQO Workgroup was established to develop and document DQOs for the PM2.5 

Chemical Speciation Trends Network (STN). The STN was subsumed into the, now called the 

Chemical Speciation Network (CSN). The DQO process that the workgroup employed is fully 

documented in its report (U.S. EPA, 1998), which is available online at the Ambient Monitoring 

Technical Information Center (AMTIC) Web page for speciation: 

http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/dqo3.pdf. 

7.2 Development of DQOs for the PM2.5 Chemical Speciation Network

The primary DQO, detection of trends in the chemical speciation data, was defined as follows by the 

EPA workgroup, whose members acted as stakeholders for the program:

“... to be able to detect a ±3 to 5 percent annual trend [i.e., ± 3 to 5 percent change in one 

year] in the concentrations of selected chemical species with 3 to 5 years of data on a 

site-by-site basis after adjusting for seasonality, with power of 0.80.” (U.S. EPA, 1999a) 

It should be noted that the DQO statement says "±3 to 5 percent" with "3 to 5 years" of data. The 

default assumptions in this Quality Assurance Project Plan (QAPP) will be detection of an average ± 5 

percent trend after 5 years at 80 percent probability. This presumes that 5 at least years of data are 

collected at any given site with no fundamental change or changes in the way data are collected. A 

fundamental change would reset the baseline year of the data collection period. However, a change in 

the trend may or may not be noticeable depending on whether the change or changes affect the 

uncertainty of data (hopefully improves it) or they create a systematic bias in the results, which would 

be noticed as a discreet change in the values of the data.
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Statistical power is defined as the likelihood that a particular statistical test will correctly reject the null 

hypothesis when it is false. Because the null hypothesis is that a trend does not exist, the DQO 

statement means that there must be an 80 percent probability of detecting a trend of 

5 percent after 5 years at any particular site, for any single analyte although only sulfate, calcium, total 

carbon, and nitrate were shown to have met these criteria (EPA 1999a). 

Several secondary objectives for data collected at the STN sites (and now the additional NCore sites) 

and other chemical speciation sites were identified, but these were not evaluated quantitatively by the 

workgroup. Five important secondary data uses are as follows: 

 Model evaluation, verification, and/or validation; 

 Emission inventory; 

 Source attribution; 

 Spatial and seasonal characterization of aerosol distributions; 

 State Implementation Plan attainment strategy development.

The desirable data quality characteristics for these secondary uses are probably significantly different 

from those applicable to trend assessment. This QAPP section only considers the needs of the primary 

objective for trend detection. 

The DQO study also concluded that by sampling every 3rd

± 5 percent per year can be detected for sulfate, calcium, and total carbon, on a single-site basis. For 

nitrate, however, the annual trend must exceed ± 6.3 percent to be detected with a power of 80 percent. 

The decision-makers concluded that this was not sufficiently different from the 5 percent goal to require 

adjustment to the sampling design. Sampling daily instead of every 3

 day for 5 years, trends greater than 

rd day provides little improvement 

in the ability to detect trends; however, the model showed that cutting the sampling rate to every 6th

Significant changes at several sites have occurred in the network’s history. Andersen samplers were 

left unsupported by their manufacturer and were pulled from the network. The URG 400 & 450 MASS 

samplers were replaced in 2007-2009 due to a decision to outfit all CSN sites—most especially trends 

and NCore with the same samplers—the Metone SASS or SuperSASS for mass, trace elements, and 

ions; and the URG 3000N for carbon and carbon compounds. 

 day

begins to impair the ability to detect concentrations trends within 5 years. 

7.3 Measurement Quality Objectives

Once a DQO is established, the quality of the data must be evaluated and controlled to ensure that it is 

maintained within the established acceptance criteria. Measurement Quality Objectives (MQOs) are 

designed to evaluate and control various phases (sampling, preparation, analysis) of the measurement 

process to ensure that total measurement uncertainty is within the range necessary to achieve the DQOs. 

The MQOs can be defined in terms of the following data quality indicators described below. However,

these MQOs can evolve into DQOs by aggregating over longer time periods, e.g., 5 years vs. a single 

event or a month; and over a broader population of data sources, e.g., a geographic region vs. one or 

two sites. 

Precision - A measure of mutual agreement among individual measurements of the same property, 

usually under prescribed similar conditions, and expressed generally in terms of the percent deviation 
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from an average of all the measured values, which is accepted as the best representation of the real 

measured value. This is the random component of error. 

Bias - The systematic or persistent distortion of a measurement process which causes error in one 

direction (i.e., the expected sample measurement is different from the sample’s true value in one 

direction). Bias will be determined by estimating the positive and negative deviation from the true or 

accepted value as a percentage of the true or accepted value and then summing the deviations. 

Representativeness - A measure of the degree which data accurately and precisely represent a 

characteristic of a population, parameter variations at a sampling point, a process condition, or an 

environmental condition. 

Detectability - The determination of the low range critical value of a characteristic that a methodspecific procedure can reliably discern.

Detection Limits Exist in the Field Measurements and the Laboratory - A measure of the capability 

of an analytical method to distinguish samples that do not contain a specific analyte from samples that 

contain low concentrations of the analyte; the lowest concentration or amount of the target analyte that 

can be determined to be different from zero by a single measurement at a stated level of probability. 

Detection limits are analyte and matrix specific and may be laboratory dependent. This characteristic is 

determined by the supporting contract laboratory and it should be explained fully in the laboratory’s 

QAPP. 

In the field, it is described as the value at which imprecision becomes unacceptably high. This value is 

typically identified by the manufacturer as the recommended range of measured parameter to which the 

measurement device may be utilized. The device should also be certified as yielding comparable values 

to a device that has been recently certified as traceable to the National Institute of Standards and 

Technology (NIST) standard reference devices and procedures for making the same measurement.

Completeness - A measure of the amount of valid data obtained from a measurement system compared 

to the amount that was expected to be obtained under correct, normal conditions. Data completeness 

requirements are included in the reference methods (40 CFR Part 50). 

Comparability - A measure of confidence with which one data set can be compared to another. 

Agreement among methods measuring the same or similar parameter; that is, converging on the same 

answer, provides a measure by which to judge bias of methods deployed in the network.

For PM2.5 speciation field activities, Section 14.0 of this QAPP presents the MQOs and the calculations 

for accuracy, precision, bias, and completeness. Representativeness is determined through the original 

Chemical Speciation Network (CSN) DQO and sampling design process and detectability, as discussed 

in the Quality Assurance Project Plan: Chemical Speciation of PM2.5 Filter Samples prepared by the 

contracted support laboratory and available from the AMTIC website. Comparability is achieved in the 

CSN by use of appropriate (performance-based) sampling instruments, adherence to standard operating 

procedures and QAPPs, and the use of a single laboratory for analysis and data reporting.

The strategic plan for chemical speciation monitoring trends sites (U.S. EPA, 1999b) quotes MQOs for 

the overall measurement process that must be achieved in order to meet the DQO for trend detection. 

These MQOs, which should be interpreted as the total coefficient of variation (CV) attributable to 

sampling and analysis, are summarized in Tables 7-1 and 7.1a. 
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Table 7-1. MQOs for Total Measurement Error

Analysis MQO for Total Measurement Error (Expressed as % CV)

Ions (anions and cations) by IC 10

Total Carbon by TOA 15

Elements by EDXRF 20

Source: U.S. EPA, 1999b.

To calculate the total measurement error corresponding to the values given in Table 7-1, it is necessary 

to quantify the individual components of random error using quality control data collected by the 

monitoring program. This process is described in Section 24.0. The limits on total error given in Table 

7-1 apply only to major ions and elements. Elements present at significantly lower concentrations will 

have much larger CVs, both from natural variability and from measurement uncertainty. These values 

were reevaluated in 2011 using the collocated sampler results from 6 sites in the CSN. The results of 

the analysis are summarized in Table 7.1a below. 

Table 7.1a MQOs for Total Measurement Error 

(2007-2010 Data From Collocated Samplers 

Upper Bound 90th Percentile CV From Values> MDL) 

It should be noted that the data for ions are less precise on the whole than what was projected in 1999. 

This may or may not be a real random variability, because the results from two sites were significantly 

different than the others and skewed the average. These results have led EPA to consider moving the 

samplers from three of the collocation sites and rotating them for 1-year deployments over the entire 

NCore network. On the other hand, the energy-dispersive X-ray fluorescence results were not quite as 

bimodal so it is not as easy to draw the conclusion that it was site-specific issues. 
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7.4 References

U.S. EPA (Environmental Protection Agency). 2006. Guidance on Systematic Planning Using the 

Data Quality Objectives Process: EPA QA/G-4, Report No. EPA/240/B-06/001, U.S. EPA, 

Washington, DC. 

U.S. EPA (Environmental Protection Agency). 1999. Particulate Matter (PM2.5 ) Speciation Guidance 

Document (Third Draft), U.S. EPA, Research Triangle Park, NC, January 5, 1999. 

U.S. EPA (Environmental Protection Agency). 1999a. Data Quality Objectives for the Trends 

Component of the PM2.5 Speciation Network, U.S. EPA, Research Triangle Park, NC, 1999. Available 

online on AMTIC at http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/dqo3.pdf.

U.S. EPA (Environmental Protection Agency). 1999b. Strategic Plan: Development of the Particulate 

Matter (PM2.5) Quality System for the Chemical Speciation Monitoring Trend Sites, U.S. EPA, 

Research Triangle Park, NC, April 16, 1999. 
PM2.5 CSN QAPP

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8.0 Special Training Requirements/Certification

8.1 Training

Personnel assigned to perform PM2.5 chemical speciation monitoring activities should meet the 

educational, work experience, responsibilities, personal attributes, and training requirements for 

their positions. Each state, local, and/or Tribal (SLT) monitoring agency is ultimately responsible 

for adequately training the personnel performing supervisory, quality assurance/quality control 

(QA/QC), data handling, and other duties related to the PM2.5

Section 8.1.1 lists the minimum requirements and some additional suggestions and ideas for 

training personnel who may be unfamiliar with the operation of PM

 Chemical Speciation Network

(CSN). Monitoring Agency management must ensure that these personnel have access to the 

relevant guidance documents, standard operating procedures, Quality Assurance Project Plans 

(QAPPs), and sampler operations manuals. Each monitoring agency is also responsible for 

assessing the adequacy of their personnel's training and performance and for ensuring training 

information is documented. 

2.5 speciation samplers and 

sample handling requirements. Section 8.1.2 describes sources of targeted training and internet 

addresses that are specifically applicable to operating the CSN. The Ambient Monitoring 

Technical Information Center (AMTIC) PM2.5

8.1.1 State, Local, and/or Tribal Agency PM

Chemical Speciation website should be consulted 

for the most recent training materials and workshop presentations. 

2.5

Minimum requirements for training personnel in field and/or laboratory operations for the CSN

are as follows:

Training

 Review of most recent QAPPs for field operations and/or laboratory operations, as 

applicable; 

 Site operators are to review the pertinent speciation sampler manual(s) for their 

site(s); 

 Review of two EPA documents, Particulate Matter Speciation Guidance Document

(January 1999) and Strategic Plan: Development of the PM2.5

Suggestions for SLT management personnel for training operators in CSN site operations are as 

follows: 

 Quality System for the 

Chemical Speciation Monitoring Trend Sites (April 1999). 

 Supply an overview of PM2.5 sampling and analysis through a video presentation. 

Videos are available on AMTIC at http://www.epa.gov/ttn/amtic/spectraining.html. 

 Schedule meetings and/or teleconferences with personnel from the SLT agencies, the 

Office of Air Quality Planning and Standards (OAQPS), the Regional Speciation 

Coordinator, the contracted support laboratory, and the Delivery Order Project 

Officer prior to beginning sampling operations. 
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 Offer operator training classes at a centralized location. For operators who cannot 

attend, a video of the procedures for operating the sampler and submitting the 

samples and data reports could be supplied for training. 

 Field personnel who are unfamiliar with operating and quality assuring data from 

meteorological monitoring systems should review the system’s operating manual and 

consult the EPA’s Quality Assurance Handbook for Air Pollution Measurement 

Systems, Volume IV: Meteorological Measurements (EPA/600/R-94/038d). 

 Continue training through update memoranda, personal instruction during on-site 

systems and performance reviews, and information distributed by the 

OAQPS/AMTIC Technology Transfer Network and Public Forum under the 

speciation topic area. This website is available at 

http://www.epa.gov/ttn/amtic/specgen.html. 

Internet Resources—The following Internet resources are specifically applicable to the PM2.5

Ambient Monitoring Technical Information Center 

speciation monitoring program: 

http://www.epa.gov/ttn/amtic/specgen.html―PM2.5

EPA/OAQPS

 monitoring information: Contains links to 

other areas including chemical speciation documents. 

http://www.epa.gov/ttn/amtic/pmspec.html—Current chemical speciation audit and assessment 

documents. 

http://www.epa.gov/oar/oaqps/pm25/—PM2.5 data analysis: Contains ongoing activities of the 

data analysis virtual workgroup, including background information, the data analysis workbook, 

analysis tools (software), data sets, contacts, and links to documents and to other PM2.5

National Park Service

sites.

http://vista.cira.colostate.edu/IMPROVE/—National Park Service's visibility monitoring 

information, including the Interagency Monitoring of Protected Visual Environments 

(IMPROVE) network.

http://vista.cira.colostate.edu/IMPROVE/publications/IMPROVE_SOPs.htm—IMPROVE 

standard operation procedures (SOPs). 

http://vista.cira.colostate.edu/IMPROVE/publications/news_letters.htm—IMPROVE 

newsletters.
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PM2.5 Speciation Sampler Manufacturers' Information and Contacts 

www.urgcorp.com—URG Corp., manufacturer of the 3000N OC/EC quartz filter-based 

sampler. 

www.metone.com—MetOne Inc., manufacturer of the SASS sampler.

8.2 Certification

There are no special certification requirements applicable to operation of the chemical speciation 

trends samplers. 
PM2.5 CSN QAPP

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9.0 Documentation and Records

This section defines the records critical to the Chemical Speciation Network (CSN), the 

information to be included in reports or to be available for inspection, the data reporting format, 

and the document control 

procedures to be used. 

Each monitoring agency 

participating in the CSN should 

structure its records management 

system in a manner that facilitates 

easy retrieval of information 

during internal and external 

systems audits and reviews. Table 

9-1 identifies the documents and 

records of the CSN that will be 

filed and retained according to the 

requirements discussed in Section 9.6. The field and laboratory standard operating procedures 

(SOPs) will provide instructions on the proper distribution and filing of data collected during 

specific procedures.

The following subsections describe the documents and records to be included in the quality 

assurance (QA) reporting packages for management, site field information operations, laboratory 

operations, data reporting and management, and quality assurance functions of the CSN. The 

term “reporting package” is defined as all the information required to support the chemical 

speciation concentration data (and ancillary data) reported to the EPA, which includes all data 

required to be collected as well as other data deemed to be important to the CSN. 

Implementation of new or modified field or laboratory procedures may require concurrent 

comparison against the old method. The document control feature (generally the date of 

issuance) of the new version will be clearly marked, and the field or laboratory user will be asked 

to discard the old version. 

9.1 Information in the Management and Organization Reporting Package

There are three distinct management organizations associated with the CSN: (1) the EPA Office 

of Air Quality Planning and Standards and Regional EPA offices; (2) the state, local, and/or 

Tribal (SLT) monitoring offices; and (3) the contracted support laboratory. The management 

reporting package for these organizations will vary but would normally consist of an 

organizational structure diagram; records of personnel qualifications and training (e.g., resumes); 

a quality management plan; and files containing records of grants, contracts, and official 

correspondence regarding the CSN. 

A fundamental requirement for the operation of any data 

gathering project is that the sponsoring organizations should 

prepare a Quality Assurance Project Plan (QAPP) and have it 

approved prior to the commencement of data gathering 

operations. In the case of the Chemical Speciation Network, 

the approvals would occur at the state, local, and/or Tribal 

(SLT) agency level and at the EPA Regional Office level. The 

EPA signatories would be the Regional Speciation 

Coordinator and the Regional QA Officer. However, there are 

some states, who have acquired full approval and signature 

authority through Regional approval of their Monitoring 

Program’s Quality Management Plan. 
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Table 9-1. CSN Reporting Package Information

Categories Record/Document Types

Management and 

Organization

Organizational structure

Personnel qualifications and training

Training Certification

Quality Management Plan 

EPA directives

Support contracts

Site Information Site characterization file

Site maps

Site photographs 

Field and 

Laboratory 

Environmental Data 

Operations

QA Project Plans 

Standard operating procedures (SOPs)

Field and laboratory notebooks and communications

Sample handling/custody records

Inspection/Maintenance records

Raw Data Any original data (routine and quality control (QC)

data) including data entry forms

Data Reporting Data/summary/progress reports

Journal articles/papers/presentations

Data Management Data algorithms

Data management plans/flowcharts

PM2.5

Data Management Systems

 data

Quality Assurance Good Laboratory Practice guidelines/requirements

Control charts or tables

Data quality assessments

QA reports 

System audit reports 

Response/Corrective Action reports

Site and laboratory audit reports

9.2 Information in the Field Operations Reporting Package

9.2.1 Site Information 

A file containing site documentation will be maintained in the SLT agency’s central or field 

office for each CSN monitoring site. At a minimum, the site information file must contain the 

following: site characterization information that documents how and why the site was selected, 

including identification of the scale of the site and the locations of nearby sources of particulate 

matter; site maps and sketches; and slides, prints, or digitized images of the site taken soon after 

installation of the PM2.5 speciation sampler(s). The CSN coordination office or the Regional 

Speciation Coordinator may ask for copies of this material for a central file.
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9.2.2 Field Operations

Operators of individual field sites must maintain records as well. The documents and records to 

be maintained at the field office are listed under “Field Operations” in Table 9-1. The following 

types of notebooks or binders are to be used by field personnel to keep documents in order and 

readily accessible during a site systems review.

Field Notebooks—Each field site operator will obtain hard-bound notebooks. The notebooks will 

be uniquely numbered and associated with the individual and the CSN program. Generally, all 

data from all routine field operations will be entered on field data forms or downloaded 

electronically from the sampler’s memory. The field notebook is used to record additional 

information about these operations, such as information regarding weather conditions and 

activities in the area that may influence the PM2.5

Some organizations may have the capability of substituting the field notebook for electronic 

communications (i.e., electronic site notebooks). This is appropriate as long as it is used 

consistently. 

sample content and concentration (wind or 

electrical damage to equipment, construction or mowing activities in the area, welding, traffic). 

Such information should also be included in the comments section of the field data form so the 

laboratory is made aware a sample may be compromised. Maintenance needs for the sampler and 

the platform on which it is positioned (appearance, upkeep, and safety concerns) should be 

relayed to the site operator’s supervisor for consideration and action. In addition, the field 

operator may use this notebook to record important communications. 

Field Binders—A three-ring binder is a convenient repository for the appropriate data forms for 

routine operations, inspection and maintenance forms, systems audit and corrective action forms, 

the field QAPP, SOPs, and updates or advisories received from EPA or from other management 

sectors.

Sample Shipping/Receipt

9.2.3 Electronic Data Collection at Field Sites

—One uniquely numbered notebook to record information about sample 

receipt and shipment will be used by the field site operator. These notebooks are to be dedicated 

to CSN work. It will include examples of standard shipping/receiving forms and areas for freeform notes about shipment difficulties or concerns, such as equipment that arrives damaged or 

has missing parts. 

All electronic data stored in the PM2.5 speciation sampler will be downloaded to a laptop 

computer or other electronic transfer device at each field site. A diskette or other removable 

memory device containing information from each of the sampling events will be created. A copy 

of the electronic download should be retained by the field operator for sampler troubleshooting 

and for later use in data validation. It is recommended that data be downloaded after each run; 

however, data from a number of runs may be accumulated in the sampler’s memory, if bad 

weather or scheduling difficulties prevent prompt downloads. NOTE: The sampler’s memory is 

finite. Do not accumulate more than two runs before downloading. Refer to the sampler 

operating manual for details.
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9.2.4 Hand-Entered Data at Field Sites

A number of forms will require hand entry of data. These forms are primarily associated with the 

field operations. An example of the combined custody and field data form and explanations of its 

content and use can be found in the SOPs of Appendix A to this QAPP and in Section 12.0. The 

forms should be in three-part carbonless paper format. A quality assurance/quality control report 

form, shown in Section 14.0, also requires hand-entry of data from checks of the flow, 

temperature, and pressure sensors of a sampler. Information should be entered clearly with a 

black or blue indelible ballpoint pen. Any entry errors should be marked out with a single line 

and the correct information entered above this line. The operator must sign or initial the form to 

verify the accuracy and completeness of the entries.

Information recorded on these field forms is very important because it serves as a backup in case 

the data downloaded from the sampler become corrupted or lost. Difficulties with, or suggestions 

for improved operation of the samplers should be recorded here and in the field notebook. 

Information about significant events near the site that may affect the representativeness of the 

sample should also be entered into this form so the laboratory will be on alert for an unusually 

high concentration sample. 

A form for audit findings from the internal (or external) systems audits of the field site or the 

contract laboratory is another example of a hand-entered data form. The response to the audit 

finding, a Corrective Action Response (CAR) form, may also be hand-entered. Copies of all field 

site reviews conducted by internal or external agencies and the site’s responses to them should be 

retained at the field site office.

9.3 Information in the Laboratory Operations Reporting Package

9.3.1 General Laboratory Information 

A file or files of general laboratory information should be available for inspection. It will include 

schematics of the laboratories showing locations of analytical stations, a record of equipment 

purchases or leases, warranty information, and maintenance and service agreements with 

instrument vendors and suppliers. The laboratory’s safety manual should be a part of this 

information. 

9.3.2 Laboratory Operations 

Information related to the laboratory operations and data management reporting packages is 

given in the QAPP for the CSN contracted support laboratory. 

9.4 Information in the QA Reporting Package

Four distinct QA organizations are associated with the PM2.5

9.4.1 Network QA Manager

CSN. 

The Office of Air Quality Planning and Standards (OAQPS) management organization has a QA 

Manager. This Manager and staff members will produce and update the quality system and will 
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review QA documents from the CSN’s field and laboratory functions. QA document updates and 

directives will be issued from this office. The QA Manager for OAQPS has overall approval 

authority for the CSN QAPP and any subsequent changes made to it.

9.4.2 State and Local Field Site QA Offices

The various SLT agencies whose personnel operate the CSN sites will keep a file of documents 

and procedures that are part of their customary QA plan for site and sampling, equipment receipt 

and acceptance testing, equipment maintenance, sampler operational checks, and operator 

training. Documented results of and CAR responses to internal site inspections and external 

reviews will also be kept on file for reference and inspection. Each SLT is expected to provide 

independent assessments of their monitoring sites and samplers according to the schedule given 

in Table 14-1 QA/QC activities. 

9.4.3 Contracted Support Laboratory QA Manager’s Office 

The contracted support laboratory’s QA Manager and staff will develop and periodically update 

the laboratory QAPP and SOPs for routine servicing of the sites and analysis of filter samples. 

Results of internal systems and performance reviews of laboratory operations will be kept on file 

and available for inspection by the EPA.

9.4.4 EPA QA Laboratory and Regional Offices support

The EPA’s Office of Radiation and Indoor Ai/National Air and Radiation Environmental 

Laboratory in Montgomery, Alabama, will provide QA services for CSN laboratory activities. 

The EPA OAQPS and Regional laboratories will provide some QA services to the field and 

laboratory components of the CSN such as management system reviews every 3 years and an 

occasional independent audit of one or more monitoring sites. Their procedures will be 

documented and kept on file and updated as necessary using document control methods. 

9.5 Reports to Management

The SLT field site operators will follow their customary procedures for reporting information to 

their management. It is suggested that any verbal communications be documented in the field 

notebook or that a copy of the notebook entry be sent to the manager and to the Regional 

speciation coordinator as appropriate. Field site operators will also report information on PM2.5

They may also report on their review and levels 2 and 3 validation of the draft data sets supplied 

by the contract laboratory, if they perform these validation activities.

sample and meteorological data capture rates and problems with sampling equipment and check 

devices for the speciation samplers. The EPA has constructed electronic reporting forms for all 

performance verifications, technical systems audits, and sampler audits. These are to be uploaded 

to a web-based receptacle from which a non-public data base will be populated. Report functions 

are under development for use by the monitoring agencies and the EPA.
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The contracted support laboratory is responsible for forwarding completed level 0 and level 1 

data validation checklists (Section 22) and the results of filter analyses to the EPA delivery order 

project officer (DOPO) and to the SLT agency contact, who submitted the delivery order, within 

20 business days from receipt of the sample. Levels 0 and 1 data validation is described in the 

laboratory QAPP. Upon approval, the final data set will be released from the laboratory in 

hardcopy and electronic format to the EPA DOPO, the state or local agency contact, and the Air 

Quality System (AQS) electronic data base. Draft and final composite semiannual data summary 

reports will be issued from the laboratory to the SLT agency contact, the DOPO, and the EPA 

Project Officer. Results of resolution of problems with data sets will also be prepared, sent to the 

concerned parties, and filed for the record. 

9.6 Archival and Retrieval of Data Reporting Packages

Each organization participating in the CSN is expected to keep updated versions of the 

documents and data sets listed in Table 9-1 on file and accessible for the duration of the trends 

network’s operation or a specified lesser time. The files of the sites, the contracted support 

laboratory, Regional and EPA QA offices, and validated electronic AQS data sets must be 

retrievable for inspection and review during regular business hours by the OAQPS management 

or other U.S. Government authorities. 

Limits on the time of data (and sample filter) retention are decided by OAQPS program 

management. Storage and archival of all field and laboratory data associated with each analysis 

in electronic format for up to 3 years following sample analysis is required, with the exception of 

particle photomicrographs and associated spectral data in electronic format which may be 

discarded 12 months after receipt of the sample for examination. Data archivists should contact 

OAQPS a month before the data discard date to ask for a decision on further archival or disposal.
PM2.5 CSN QAPP

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10.0 Sampling Process Design

This section describes all components associated with on-site field operations of the nationwide 

PM2.5 Chemical Speciation Network (CSN). The network will be operated by state, local and/or 

Tribal (SLT) agencies. This section describes the field activities and the key parameters to be 

estimated, the networks where primary speciation samplers and collocated quality assurance

(QA) speciation samplers are located, and the frequency of sampling using the primary and QA 

samplers. The EPA Ambient Monitoring Technical Information Center (AMTIC) website

[http://www.epa.gov/ttn/amtic/specgen.html] contains a listing of all current CSN sites. The

network design components comply with the regulations specified in 40 Code of Federal 

Regulations (CFR) Part 58, Section 58.13, Appendices A, D and E, which are further described 

in the document Guidance for Network Design and Optimum Site Exposure for PM2.5 and PM10

10.1 Scheduled Project Activities, Including Management Activities

(U.S. EPA 1997). The NCore and other network components of the CSN have, for the most part, 

already been designed based on collaborative input from SLT agencies and other federal 

agencies (for example, the National Park Service and the National Forest Service). The final 

NCore design has been solidified and the network began operation January 1, 2011. More 

information is available at http://www.epa.gov/ttn/amtic/ncore/index.html. 

The CSN collects filter-based at all NCore locations and at selected state and local air monitoring 

station (SLAMS) sites. Chemical components of PM2.5 are determined by a contracted support 

laboratory. The site locations are determined by the CFR Part 58, Section 58.13, Appendices A 

and D, and by the current National Monitoring Strategy implemented by EPA and SLT agencies. 

All NCore sites will have a collocated PM2.5

Attaining a complete understanding of the interactions and scheduling of field site and support 

laboratory activities is a very important consideration of the sampling process design. The 

sequence of activities for the contracted support laboratory for the NCore trends network 

component of the CSN is presented in Table 10-1. The site supply and analytical aspects of the 

NCore network component of the CSN will remain essentially the same as in prior years. 

Federal Reference Method (FRM) sampler present 

to collect samples for determination of particle mass concentration. 
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Table 10-1. Sequence of Activities for CSN Contracted Support Laboratory 

Activity Notes

Prepare and obtain approval of Quality Assurance Project 

Plan (QAPP) and standard operating procedures (SOPs) for 

laboratory activities and field site support.

Includes laboratory SOPs, tested and approved for 

use.

Meet with OAQPS project scientists, regional speciation 

coordinators, and delivery order project officers (DOPOs).

Receive details on CSN site contacts and sampler 

requirements. Finalize mechanism and schedule for 

delivery order process for routine samples.

Receive and analyze routine speciation samples. Continuing process.

Assemble, validate, and report data. Review field and 

laboratory interactions; review and resolve problems.

Continuing process.

Complete analyses within 20 business days of sample receipt. 

Prepare and submit monthly draft summary data reports to 

DOPO and agencies for review and validation.

Conduct level 0 and level 1 validation of data. 

Submit final data packages following SLT and DOPO 

approval of draft data.

Enter data into Air Quality System.

QA auditing and inspections. QA Manager for contracted support laboratory 

conducted audits.

Systems audit and review of data archives. Coordinated by EPA.

10.2 Rationale for the Design

10.2.1 Network Design

The rationale for the design of the CSN originated in the monitoring regulations, promulgated at

Federal Register (62 FR 38763), as part of the PM2.5 National Ambient Air Quality Standards 

review completed in 1997. The background to the planning and design of the initial CSN is 

covered in Section 5 of this document. The overall network design strategy was to locate 25 

trends-assessing PM2.5 samplers at photochemical air monitoring stations (PAMS) sites and the 

remaining approximately 25 trends sites at “core” SLAMS. The SLT agencies were given the 

responsibility to site supplemental speciation samplers for background, transport, and local 

program needs. Essentially 54 trends sites were established and a supplemental network of up to 

225 sites was deployed at the network’s highest site-count in 2004. Revised monitoring 

regulations in October 2006 called for an updated national strategy that would establish an 

NCore network of up to 75 sites which would incorporate most of the original 54 trends sites.

Approximately 240 of the original 300 plus CSN sites have been retained to monitor for 

speciated PM2.5

Network design requirements stated in 40 CFR Part 58, Appendix D, Sections 4.7.4 and 4.7.5, 

provide guidance on locating monitoring sites for PM

. There are still approximately 60 Interagency Monitoring of Protected Visual 

Environments (IMPROVE) protocol sites and about 180 CSN sites, which include 80 

MetOne/URG speciation sampling combos at NCore sites.

2.5 with respect to scale and monitoring 

objectives. Site requirements with respect to roadways, sampler probe heights, and juxtaposition 

with other samplers are specified at 40 CFR 58, Appendix E, and are summarized below in Table 

10.2. 
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Table 10-2. Design Criteria for Collection Site Surroundings

1. The height of the inlet to the sampler should be between 2 and 15 meters above ground surface.

2. For samplers located on roofs or other structures, the minimum separation distance between the inlet 

and any structure should be greater than 2 meters.

3. The sampler should be located away from obstacles so that the sampler is at a distance at least twice 

the height of the obstacle. For example, a tree is 10 meters tall and is east of the sampler. The 

sampler would need to be placed at least 20 meters (preferably further) away from the drip line of a 

tree.

4. An unrestricted air flow of 270° must exist around the sampler inlet.

5. If the sampler is located on the side of a building, a 180° air flow clearance is required.

6. Sampler inlet should be located at least 10 meters from the drip line of any tree.

7. Minimum distance to any roadway is 10 meters, but this value is determined by the average daily 

number of vehicles (refer to table in 40 CFR Part 58 Appendix E for exact information).

8. The inlet height for collocated samplers should agree vertically within 1 meter.

9. The closest horizontal distance for placement of a collocated sampler to a Lo-Vol sampler is 1 

meter; to a Hi-Vol sampler is 2 meters. The maximum horizontal distance a collocated sampler may

be from any sampler is 4 meters.

10.2.2 Speciation Sampler Design and Deployed Models

Sampler design requirements stated in 40 CFR Part 58, Appendix D, Sections 4.7.4 and 4.7.5, 

require that speciation samplers incorporate particle inlets and size fractionators having particle 

size discrimination curves comparable to the FRM for PM2.5, employ denuder technology to 

remove acidic gases, have face velocities and sample volume capture similar to the FRM, and be 

reliable and rugged in field use. However, speciation samplers are not required to attain reference 

or equivalent method designation and should be selected based on performance in order to meet 

the CSN data quality objectives. Desirable features of speciation samplers are discussed in the 

PM2.5 speciation guidance document (U.S. EPA 1999). Operating information for speciation 

sampler models—MetOne and URG—currently used in the CSN network is given in Appendix 

A-1 and A-2. of this QAPP. 

10.2.3 Sampling Frequency

The NCore sites of the CSN will sample consistently every 3rd day. Routine samples will be 

collected for a 24-hour period beginning and ending at midnight on the assigned day. Other sites 

in the CSN network (such as SLAMS sites) will sample on either an every 3rd day or an 

abbreviated version of the 1in 3 day frequency called the “alternate 1in 3”1; or every 6th

 

1 The national monitoring schedule to which all monitoring programs and networks adhere causes Friday and 

Monday sampling events every third weekend. The Alternate 1 in 3 schedule was established due to the inability of 

SLT’s to authorize overtime work on weekends and holidays to recover samples and set-up the next sampling event. 

It essentially requires the agency to sample on Friday and collect filters on Monday on one week-end; and on the 

day 
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schedule. The sampling schedules are available on the AMTIC website. This schedule should be 

printed and be distributed to all site supervisors and operators. 

Field blanks shall be generated at a frequency of approximately 3 percent of the normal routine 

sampling frequency of MetOne PTFE filters and 10 percent of URG 3000N quartz filters. The 

procedure for MetOne field blanks will change in January 2012 to better simulate the field blank 

procedure of the URG 3000N. That is, the field blank module will be attached to a channel for 

which the air flow tube has been detached from the pump and capped. A very sharp cut cyclone 

will be retained in its operating position. The module will remain on the non-sampling channel 

for the entire period over which the routine PTFE module is attached; typically channel 1 (and 5 

on a SuperSASS). 

Trip blanks will not be collected for the MetOne unless they are requested by specific monitoring 

agencies for specific reasons, which each requestor must supply. Trip blanks will be generated 

for the URG 3000N at a frequency of 2 percent of the routine sample filter shipments. Again this 

frequency may be adjusted based on issues that arise.

Sites in the CSN will not acquire samples on any other days unless specifically directed to do so 

by network authorities. Should non-routine sampling be requested, such samples must be taken 

on days other than those set by the every-3rd-day schedule ,or every-6th

10.2.4 Collocation of samplers 

-day schedule, or taken on 

different samplers on the same day, and must be handled separately when submitted to the 

contracted support laboratory for analysis. 

Collocated samplers provide a set of PM2.5 speciation data, originating from a separate but 

otherwise identical sampler, which can be used to estimate the precision of the total sample 

collection, handling, and analysis/data reporting process. The locations of these sites and all of 

the CSN sites are available on the AMTIC website. The original design included two sites for 

every approved speciation sampler. As of 2009, only MetOne and URG 3000N samplers are 

collocated at these sites. The collocated QA samplers are operated every 6th

The original design of the speciation trends network called for collocation at 10 percent of the 

sites, which ultimately led to six collocation sites. The EPA has determined that better 

representation of the entire network is needed; therefore, a design change is under way which 

will leave collocated speciation samplers at two to four of the NCore sites. The remaining two to 

four collocation samplers will be deployed on an annual rotating basis to other sites around the 

country. This design strategy may change slightly based on results over the first 2 years. Other 

options include: 

 day to coincide with 

the start and end run times of the site’s primary sampler. Samples and data from the collocated 

sampler will be handled in exactly the same way as those from the primary sampler. Section 14.0 

discusses the calculation of precision in more detail. 

• Decreasing the duration and increasing the number of sites that participate each year;

 

third week-end following, the Friday event is abandoned for sampling on Monday and recovering the sample on 

Tuesday. 
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• Adding additional samplers to the collocation fleet to allow more sites to sample

collocated for 12 months 

• Revise the ratio of permanent collocation to rotating collocation sites based on needs 

assessed by the EPA as informed by SLTs, CASAC and organizations conducting health 

studies. 

10.2.5 Deviations From the Sampling Plan

Because one of the major goals of NCore sites of the CSN network is to determine trends in 

PM2.5 chemical speciation concentrations over time and within geographical areas, deviations 

from the sampling plan are allowed only upon prior consultation with and approval of the EPA. 

Should an occasional operational problem occur at a site, the site operator must note this in the 

field site notebook and on the field data form that is returned to the contracted support laboratory 

with the sample filters so the resulting analytical data can be flagged. Unapproved, continued 

deviations from the sampling plan at one or more sites will give rise to a review of the site

agency’s operating plan, the personnel involved, and a request for prompt corrective action. 

Furthermore, the data sets acquired during periods when deviations from the sampling plan 

occurred or operational problems were encountered may be sequestered and not used in trends 

analysis studies.

10.3 References 

U.S. Environmental Protection Agency. 1997. Guidance for Network Design and Optimum Site 

Exposure for PM2.5 and PM10. Publication No. EPA-454/R-99-022. December 1997. Available 

at: www.epa.gov/ttn/amtic/files/ambient/pm25/network/r-99-022.pdf. 

U.S. Environmental Protection Agency. 1999. Particulate Matter (PM2.5) Speciation Guidance 

Document. Final Draft. October 7, 1999. Available at: 

www.epa.gov/ttn/amtic/files/ambient/pm25/spec/specfinl.pdf. 
PM2.5 CSN QAPP

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11.0 Sampling Methods Requirements

The Chemical Speciation Network (CSN) provides for measurement of the mass and chemical 

component concentrations of fine particulate matter with an aerodynamic diameter less than or 

equal to a nominal 2.5 μm (PM2.5) in ambient air over a 24-hour period. At the inception of the 

CSN, three different brands of PM2.5

11.1 Sample Collection and Preparation

speciation monitors were in use. These three samplers were

subjected to bench testing and to comprehensive, multi-city field test in which all the samplers 

were positioned in a close array. They collected filter samples for several events. The results 

from each sampler were compared with each of the others and against the Federal Reference 

Method (FRM) and IMPROVE samplers. All of the samplers met the requirements stated in the 

EPA requisition for speciation samplers. Now (as of 2011), the sampler fleet consists of the 

MetOne SASS or Super SASS and the URG 3000N for EC/OC measurements. Use of the old 

legacy URG MASS, Andersen RAAS, and Thermo-Fisher’s RP Partisol Model 2300 has ended. 

Standard operating procedures (SOPs) for setup, operation, and quality control of the most often 

used samplers are given in Appendix A to this Quality Assurance Project Plan (QAPP); SOPs for 

other legacy samplers are available on the EPA Ambient Monitoring Technical Information 

Center (AMTIC) website. 

11.1.1 Preparation 

Before a site visit, the operator must gather sampling modules containing the filter, data forms, 

and sampler verification equipment to check flow, temperature, and pressure (if a quality control 

(QC) check is scheduled). The sampling modules must be transported to the sites in a protected 

environment and not subjected to high temperatures. 

Shipment of sampling modules to the laboratory will require the use of ice substitutes and 

insulated containers. The operator must freeze the ice packs prior to use. During transport 

to/from the sites, the ice substitutes may be placed in an electric transport cooler to maintain their 

frozen state.

11.1.2 Field Sample Collection

The speciation sampler will be permanently installed within 1 to 4 m of the site’s routine FRM 

sampler. All NCore sites will have a PM2.5 FRM sampler present. The proper operation of the 

speciation samplers and the collocated FRM sampler must be confirmed before the first run. A 

testing and acceptance checklist appears in Section 15.0 of this QAPP. Sampling modules will be 

installed. At NCore and the other remaining trends sites, the samplers will run every 3rd day or on 

the “alternate 1 in 3 schedule,” from midnight-to-midnight on local standard time the whole 

year. Refer to Appendix A for details on setup and operation of the sampler, handling of filter 

sampling modules, hand-entry of data, downloading of electronic files, and sampler QC check 

requirements.
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11.1.3 Sampler Recorded Measurements

Table 11-1 lists the information that is provided by any of the speciation samplers. This 

information will be stored in the sampler’s memory and can be downloaded to disks. Essential 

information will also be transcribed from the display screen of the sampler and hand-entered on 

to a custody and field data form. This form is described in Section 12.0 of this QAPP. 

Table 11-1. Summary of Information Provided by Speciation Sampler 

Information to be Provided Units

Availability Provided to 

AQS

Anytime End of Period Visual Display Database

Flow rate, average, for the 

sample period

L/min ∗ (optional)  (required) ∗

Flow rate, CV, for the sample 

period

L/min ∗  ∗ ●

Flow rate, 5-min average out of 

specification (FLAG)

   ●

Sample volume, total m ∗ 3   ●

Temperature, ambient, min., 

max., average, for the sample 

period

°C ∗   ●

Barometric pressure, ambient, 

min., max., average, for the 

sample period

mmHg ∗   ●

Filter temperature, differential, 

30-min interval, out of 

specification (FLAG)

∗   ●

Date and time yr/mo/d/h/

min

 —  —

Sample start and stop time 

settings

yr/mo/d/h/

min

  

Sample period start time yr/mo/d/h/

min

—   ●

Elapsed sample time h min    ●

Elapsed sample time out of 

specification (FLAG)

—   ●

Power interruptions >1 min, 

start time of first ten 

interruptions

h min ∗  ∗

User-entered information, such 

as sampler and site 

identification

   ●

The sample volume is essential to determining the concentration of the species. The total volume 

of air collected by a speciation sampler will vary by brand and sampling channel. Samples are 

expected to be 24 hours in duration; however, in some cases, a shorter sample period may be 

necessary, but it should not be less than 23 hours or more than 25 hours. Because capture of the 
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fine particulate is predicated on a particular sampler channel’s design flow, deviations of greater 

than 10 percent will set a flag for that sample period. Further, if a sampling period is less than 23 

hours or greater than 25 hours, the sample will be flagged. Other conditions may cause a flag to 

be set. These include power losses and extreme difference in ambient and sampler interior 

temperatures.

11.1.4 Sampling Module Transportation 

The used sampling modules must be stored in a protective transport container and transported to 

the contract laboratory as soon as possible. Sampling modules should be shipped out by 

overnight express within 48 hours following the end of a sample run. Samples are shipped with 

cold packs designed to maintain the sample temperature at 4o

11.1.5 Field Maintenance and Calibration

C. If an agency must deviate from 

sending the sample out within 48 hours, please see the discussion in Section 6.4.3. 

A maintenance schedule must be developed for field sampling equipment and verification 

devices. See Section 15.0 of this QAPP for more information. Consult the operator’s manuals, 

the SOPs in Appendix A, and Section 16.0 of this QAPP for requirements and procedures for 

calibration of temperature and pressure sensors and the flow rates of sampling channels.

11.2 Sampling/Measurement System Corrective Action Process

11.2.1 Corrections to the SOPs

The state and local agency field site operators and their supervisors are responsible for 

implementing this QAPP and the field SOPs and are, in part, responsible for the quality of the 

data. If changes or corrections are suggested for the SOP methods or QAPP, state or regional

personnel will notify the Chemical Speciation QA Lead in the Office of Air Quality Planning 

and Standards (OAQPS) Coordination Office. The QA Team members will review the 

information and convey the issue to an ad hoc Chemical Speciation Workgroup consisting of 

volunteer EPA and state, local and/or Tribal site operators and data managers, convened by the 

OAQPS Speciation QA lead. The workgroup will review the proposed change and attempt to 

classify the change according to the effect the change would have on the data. Class types 

follow: 

Class 1—The change improves the data and the new procedure replaces the current procedure. If 

found to be acceptable by the workgroup, a new SOP will be issued that can be inserted into the 

QAPP. The document control information in the heading will contain a new revision number and 

date. A quality bulletin will be filled out describing the change and distributed to all affected 

personnel. 

Class 2—The change provides for an alternative that does not affect the quality of the data but 

may provide for efficiencies in some circumstances or be cost-effective. If found to be 

acceptable by the workgroup, the original SOP will not be altered, but an addendum to the 

procedure will be issued that describes the modification and provides for the use of the 

alternative method.
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Class 3

Upon agreement by workgroup to institute a change, hard copies of Class 1 and 2 changes will 

be distributed using a quality bulletin such as that illustrated in Figure 11-1. The CSN laboratory, 

each site, and the management of each site will be notified. New versions of SOPs will be 

conveyed to CSN participants with instructions to discard the old version. 

—The change is grammatical in nature and does not reflect a change in the procedure. 

The changes will be highlighted and modified during a Class 1 change (where appropriate) or 

corrected during the development of a full revision to the document. 

11.2.2 Data Operations 

Corrective action measures in field operations of the CSN will be taken to ensure the data quality 

objectives are attained. Potentially, there are many types of sampling and measurement system 

corrective actions. Table 11-2 lists common problems and a few of the corrective actions needed 

for a well-run chemical speciation network. 

11.3 Avoiding Sample Contamination; Temperature and Holding Time 

Requirements

This section details the requirements needed to prevent sample contamination, the temperature 

preservation requirements, and the permissible holding times to limit degradation of the sample 

catch. 

11.3.1 Sample Contamination Prevention 

The CSN must have rigid requirements for preventing sample contamination. Powder-free antistatic gloves are worn while handling filter cassettes or sampling modules in the laboratory. 

Once the filter cassette or sampling module leaves the laboratory, it must not be opened due to 

the potential for filter damage or contamination. Sampling modules (used with the MetOne 

SASS and Super SASS, and the URG 3000N) will be capped and protected in plastic sealable 

bags during shipment to and from the site. When used cassettes or sampling modules are 

removed from the sampler, they must be promptly capped or otherwise protected to prevent 

contamination from dusts, gases, or abrasion. The site operator’s hands must be clean when 

handling sampling modules and it is suggested that they be cleaned immediately before the 

sample handling step. It is recommended that clean disposable gloves be used. 
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Quality Bulletin

Number 

Date 

Page of 

Supersedes No. 

Dated 

Replace and Discard Original

Add Material to Document

 

Notes:

 PM2.5 CSN QA Team Leader

 Retain this bulletin until further notice 

 This bulletin will be invalid after (Date) 

 This bulletin will be incorporated into quality

 Procedure No. _________ by (Date) ________ 

Figure 11-1. Quality bulletin. 

Subject:
PM2.5 CSN QAPP

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11.3.2 Temperature Preservation and Holding Time Requirements 

During shipment from the laboratory to the sample location, there are no specific requirements 

for temperature control; however, the filters or sampling modules should remain in their 

protective containers and inside the transport container. Excessive heat must be avoided (e.g., do 

not leave in direct sunlight or a closed-up car during summer). During the sampling (24-hour 

period), the filters will be subject to ambient temperatures and should not exceed the ambient 

temperature by more than 5oC for more than 30 minutes continuously. If this occurs, a flag 

should be set automatically by the sampler. 

Sampling modules should be removed from the sampler within 48 hours after the sampling 

period ends. If this time limit is missed, the sample will be processed but a flag will be applied to 

the data. An exception will also be when the sampler is run sequentially and filters are retrieved 

after the second event occurs (within 110 hours of the first two sequentially programmed events). 

Refer to Section 6.4 for information on how to handle shipment time exceptions. The 

temperature of sampling modules must be brought to 4oC as soon as possible and the shipment 

package, cooled to 4ο

Table 11-2. CSN Field Operations Corrective Procedures

C, should be ready for pickup by the courier service as soon as possible, 

unless the samples will be transported back to the field office and stored in a refrigerator (i.e., 

Friday sample collection).

Item Problem(s) Action Notification

Sampler failure Unacceptable performance. 

Repair/replacement 

needed. 

Repair or replace sampler or 

component at factory. Obtain 

spare sampler.

Notify contracted support 

lab at both trade-out 

and trade-in.

Sample flow rate 

verification(s)

Out of specification (+5 % 

of reference standard) or

outside ± 5% of design 

flow rate.

1. Completely remove flow rate 

measurement adapter; 

reconnect and perform flow rate 

check again

1. Document on QA/QC 

field data form

2. Perform leak test 2. Document on QA/QC 

field data form

3. Recalibrate flow rate 3. Document on field 

calibration data form 

and notify supervisor

Leak test Leak outside acceptable 

tolerance

1. Completely remove flow rate 

measurement adapter; 

reconnect and perform leak test 

again

1. Document in field 

notebook and on 

QA/QC field data form 

2. Inspect all seals and O-rings; 

replace as necessary and 

perform leak test again

2. Document in field 

notebook and on 

QA/QC field data form; 

flag data since last 

successful leak test.

3. Check sampler with different 

leak test device if applicable

3. Document in field 

notebook and on 

QA/QC field data form
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Item Problem(s) Action Notification

Sample flow rate Consistently low flows 

documented during 

sample run

1. Check programming of sampler 

flow rate

1. Document in field 

notebook and on 

QA/QC field data sheet

2. Check flow with a flow rate 

verification filter in place and 

determine if actual flow is 

within acceptance limits

2. Document in field 

notebook and on 

QA/QC field data sheet

Ambient temperature 

sensor verification 

and filter 

temperature sensor 

verification

Out of specification (+2ο 1. Recalibrate sensor; replace 

sensor; Consult with 

manufacturer for 

troubleshooting, repair or 

replacement.

C 

of standard)

1. Document in field 

notebook and on 

QA/QC field data form

Filter temperature 

should approximate 

ambient 

temperature

Filter Temperature 5ο For MetOne, Check filter temp 

sensor with independent device; 

Check for excessive heat source 

near sampling head. 

C > 

ambient temperature for 

more than 30 minutes

1. Document in Field 

notebook, and on 

CAFDF. Consult with 

mfgr. If occurs more 

than once.

Ambient pressure 

verification

Out of specification (+10

mmHg of standard)

1. Make certain pressure sensors 

are exposed to the ambient air 

and are not in direct sunlight

1. Document in field 

notebook and on 

QA/QC field data form

2. Call local airport or other 

source of ambient pressure data 

and compare that pressure to 

pressure data from monitors 

sensor; pressure correction may 

be required

2. Document in field 

notebook and on 

QA/QC field data form

3. Connect new pressure sensor 3. Document as above

Elapsed sample time Out of specification 

(+ 5 min)

1. Check programming; verify 

power outages

2. Reset

Elapsed sample time Sample did not run, or 

elapsed time was outside 

limits of 24 ± 1 hours

1. Check programming 1. Document on data sheet

2. Try programming sample run to 

start while operator is at site; 

ensure the transport filter is in 

the unit

2. Document in field 

notebook

Power Power interruptions 1. Check line voltage

Power Liquid-crystal display 

(LCD) panel on, but 

sampler not working

1. Check circuit breaker; some 

samples have battery backup 

for data but will not work 

without AC power

1. Document in field 

notebook

Data downloading Data will not transfer to 

laptop computer or other 

storage device

1. Document key information on 

sample data sheet and 

additional information in site 

notebook. Make certain 

problems are resolved before 

data are written over in sampler 

microprocessor
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12.0 Sample Handling and Custody Requirements

12.1 Introduction

This section describes sample handling and custody procedures that are necessary to ensure that: 

 Chemical Speciation Network (CSN) site operators properly handle the sampling 

components from the time of receipt at the field office until they are released to the 

shipping agency for return to the CSN laboratory. 

 Field sites use Chain of Custody (COC) documentation; subsequent laboratory COC 

is maintained for each sample, beginning with placement of the filters in the sampler 

collection modules and extending through all analytical steps to final sample archival.

12. 2 Filter Handling and Custody Procedures Prior to Sampling Event

Care must be taken when handling, storing, and transporting filters at all stages in their use due 

to the small mass of particles collected on exposed filters, the potential for sample losses due to 

rough handling or sample volatilization, and the potential for weight gain due to contamination 

or uptake of reactive gases on the filter and particulate matter surfaces. Care must also be 

exercised in handling denuders to ensure acidic gases are quantitatively removed from the 

sample air stream and that the denuder’s coating does not dislodge and fall onto the sample filter. 

Sample handling procedures must be consistently followed in order to provide data meeting the 

data quality objectives. These procedures are discussed below following the order of activity 

from the point where it is ready to be loaded up to the sampling event. 

12.2.1 Procedures in the CSN Laboratory 

The contracted service laboratory loads the filter cassettes. The 46 mm filters go into the MetOne 

canisters and the 25 mm filters go into cassettes that are fixed in the URG cartridges. This avoids 

any need for the field operators to physically handle or touch the filter.

Details on how the contract laboratory handles the denuders and filters, loads the filters into 

sampling modules, and packages the components for shipment to the field office are given in the 

CSN contracted support laboratory’s standard operating procedures (SOPs) and Quality 

Assurance Project Plan (QAPP), available on the EPA Ambient Monitoring Technical 

Information Center (AMTIC) website. 

Sample custody procedures are required to avoid misplacement of samples or confusion of one 

sample with another, and to provide documentation to assist in detection and resolution of COC 

problems. A sample is considered to be in custody if it is in one’s actual physical possession or 

stored in a secured area restricted to authorized personnel. 

Each set of sampling modules and other equipment supplied by the laboratory (such as cyclones 

and denuders) will be accompanied by a carbonless three-part, PM2.5 chain of custody and field 

data form. This form will contain the filter identification number, filter type, container (module 

or cassette) identification number, and date by which the sampling media must be used. An 

example form is illustrated in Figure 12-1 and its contents are explained in Table 12-1. The 
PM2.5 CSN QAPP

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laboratory fills in much of the information required in parts A, B, and C of the form and retains 

the third copy. The information on the custody form is ultimately entered into a sample tracking 

system, where an electronic record is kept. 

Note that the use of quartz fiber filters (MetOne channels 3 or 7 on Figure 12-1) has been phased 

out in all but approximately six monitoring sites. The sites that continue to use channel 3 on the 

MetOne SASS or SuperSASS are collecting data for historical comparisons of the two methods. 

The URG 3000N is now used to collect carbon and carbon-containing PM2.5

12.2.2 Procedures at the Field Office

particulate on 

quartz filters. Refer to Appendix A-3 for details on the custody and field data form for the 

URG3000N sampler. 

Upon receipt at the field office of a set of sampling components for a particular speciation 

sampler, the CSN site operator must carry out the following documentation and handling steps: 

 Enter receipt of the shipment in the operator's field notebook, noting the date and time 

of receipt and any air bill or other identifying numbers associated with the shipment. 

 See Section 12.2.1 for information about a second sampler (the URG 3000N) that has

replaced the quartz filter channel on the 3-channel speciation sampler. The free 

channel may be used for special studies.

 Inspect the exterior of the shipping container, note any evident damage, and record 

observations in the operator's field notebook. 

 Open the shipping container and ensure that a COC and field data form is present for 

each set of sampler components sent in the shipment. Also check to be sure shipping 

items such as ice substitute gel packs and a minimum/maximum thermometer (if 

required) are present. Ensure each identifying number printed on the COC form

corresponds to an enclosed sampling channel component. Do not use any sampling 

component whose identifying bar code number is not listed on the COC form. Notify 

the CSN support laboratory about any discrepancies. Remove the gel packs and 

freeze them at -18°C (0°F).

It has been noted by support laboratory, that the interior temperature of some of the 

containers received in the laboratory has been above 4°C. This problem may be due 

to the gel packs not being frozen long enough or at a cold enough temperature. It is 

recommended that gel packs be frozen for at least 3 days at a temperature of -18°C. 

This will ensure that the filters do arrive at the support laboratory at temperatures at 

or below 4°C.

 Sign and date the custody record portion of the COC form. 
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 Store all components for a sampler run together in a container in an air-conditioned 

secure area for later transport to the site. Adopt a first-in, first-out use schedule. 

Sampling components should be stored and tracked so that the correct set of sampling 

components reaches the designated field collection site for use on the designated 

sampling day. 

Do not interchange sampler channel components intended for use with a particular speciation 

sampler at a particular site with components for any other sampler or site. The CSN contracted 

support laboratory has labeled each sampler channel component for use at a particular site. 

Should an interchange occur, the CSN site operator must fully document the variance and inform 

the support laboratory so the analytical results can be associated with the correct sampler and 

site. 

12.3 Sample Handling and Custody Procedures for Collection of Samples

The following procedures are brief descriptions of standard operating procedures. For more 

detailed information about the process of removing sampling modules and denuders from a 

sampler, filling in field data forms, downloading data electronically, and packaging samples in a 

cooled container for shipment, refer to the SOPs in Appendix A to this QAPP, to SOPs 

concerning sample packaging and shipment in the contracted support laboratory’s QAPP, and to 

the sampler’s operating manual.

12.3.1 Installation of Filters

Sampling components/modules must be used at the field collection site on the sampling date 

specified on the COC and data form. Unused sampling modules and denuders should remain 

sealed or capped and kept from exposure to ambient air, temperature extremes, or vibrations. 

Upon arrival at the site to set up a sampling event, the CSN site operator should follow the SOP 

written for the sampler and to the sampler’s operation manual. Refer to Appendix A SOPs for 

instructions for the installation of sampling modules and denuders and programming of the 

sampler. There are quality control (QC) procedures that may take place at prescribed frequencies 

which may coincide with the installation of the sampling filters. Examples would be flow rate 

checks, temperature probe and pressure sensor checks. These will be completed with appropriate 

reporting forms. If a problem is discovered, the operator will take whatever steps are necessary 

to initiate the agency’s corrective response plan. Collecting filter samples with a sampler that is 

not performing as designed, generates data of little value. 

Once the sampling modules are installed at the site and the sampler is programmed to begin 

operation, the operator should complete the appropriate sections of the COC data form.

12.3.2 Post-sampling Procedures at the Field Collection Site

Within 48 hours after the end of a sampling period, the CSN site operator should remove the 

sampling modules from the sampler. On an alternate schedule is it possible that retrieval may 

only be possible after 56-64 hours following a Friday or Monday holiday. 

At the site, the operator must complete the following: 
PM2.5 CSN QAPP

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 Read selected data from the sampler’s display screen and enter them in Section E of 

the custody and field data form. Double-check all entries against the sampler display. 

Print clearly. Be certain the entries are clear on the second and third pages of the 

carbonless form. Refer to the custody and field data form example in Figure 12-1 and 

to Table 12-1 for details. A site may have more than one PM2.5

 Remove the filter cassettes or sampling modules from the sampler. Briefly examine 

the cassette or module for damage and ensure it is, in fact, the correct module for the 

sampling channel from which it was removed. 

speciation sampler 

and, thus, the operator must complete additional field data forms. 

 Place the sampling modules in protective container(s); cap the denuders if they are to 

be returned. Place all sampling materials in the shipping/transport container 

containing ice substitutes, but do not seal. 

 Download data from the sampler to a laptop computer and then transfer it to a labeled 

portable flash storage device. Alternatively, MetOne manufacturers a data transfer 

device to which data can be downloaded for later transfer to a computer and then a 

portable flash storage device. 

 Return to the field office to complete packing and shipping arrangements. There are 

some sites that accommodate all the facilities needed to prepare the sample(s) for 

shipping immediately upon retrieval, in which case, the operator would proceed to the 

next set of procedures immediately.
PM2.5 CSN QAPP

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Figure 12-1 CSN Custody and Field Data Form for MetOne SASS Sampler 
PM2.5 CSN QAPP

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Figure 12-2 CSN Custody and Field Data Form for URG 3000N Sampler
PM2.5 CSN QAPP

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Table 12-1. Explanation of CSN Custody and Field Data Form

CAFDF Section Explanation of Section Contents

Top of form The custody/data form number will be unique to each sample set and assigned in 

advance by the laboratory. The 3-part carbonless form will be distributed as follows: 

 Top copy (white original) -- returned to the CSN support laboratory

 Second copy (yellow) -- retained by the field site office

 Third copy (pink) -- retained by the originator

A. Custody Record Acknowledge relinquishing and receiving custody in this section. Persons should 

sign their name (legibly) and record the date.

B. Site and Sampler 

Information

Information about the site and the date the sampler modules are to be used. Most of 

this information will be pre-entered by the laboratory.

C. Sampler Channel 

Components

The sampling components needed for a particular sampler and its multi-channel 

sampling arrangement are listed here. They are identified by bar code tracking 

number and by a free-form description. The brand of the sampler is identified. This 

information will be entered by the laboratory, preprinted on the form. A separate 

custody/data form will be used for each set of sampling modules intended for routine 

sampling, field blank studies, trip blank studies, and special studies.

D. Start, End, and 

Retrieval Times

These entries are made by the site operator. The start and end times correspond to 

those programmed into the sampler during the setup phase. The operator must 

enter these data clearly and must double-check the values against the sampler 

display screen. The retrieval date and time indicate when the sampling modules 

were removed from the sampler. 

E. Sampler Channel 

Information

Postsampling information can be transcribed by hand directly from the display 

screen of the sampler. The operator is responsible for making these entries at the site. 

The sample volumes will be used by the support laboratory to compute analyte 

concentrations. The SLT agencies will use these data in levels 2 and 3 validations to 

identify problems with the sampler. Again, the operator must enter these data 

clearly and must double-check the values against the sampler display screen.

F. Comments This section offers a place to record further notes on any part of the form as well as 

observations of abnormally high emissions in the vicinity. The person recording 

information here should refer to the sections of the form. Detailed information 

should also be recorded in the field or laboratory notebook and referenced to the 

unique custody/data form number, location, sampler, and sampling date.

12.3.3 Post-sampling Shipping Procedures 

Within 48 hours following the end of the sampling period (or within 24 hours after the second 

sampling period of a sequential set), the CSN site operator will: return the modules to the field 

office (which may be the monitoring site); complete all paperwork; seal the COC data form in a 

plastic bag and tape the bag on the inside of the transport container, and package the modules 

and denuders in the container for pickup by the shipping agency. Illustrated packing instructions 

for the modules can be found in Appendix A. Please see Appendix A for details on packing the 

modules for shipment to the contracted support laboratory. At the field office, the operator must 

complete the following:
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 Retain the second page of the three-part COC data form and package the top copy in 

the shipping container. Package the sampling modules, insert the ice packs in the 

shipping container, and take the container to a drop point or arrange for pickup by the 

contracted overnight air shipping company. Chain of custody seals on the shipping 

coolers or containers are not required. 

 Complete the shipping air bill, attach it to the shipping container, and present the 

package to the shipping agent.

 It is important to avoid shipping on Fridays. If a sample must be recovered on a 

Friday, place the sample in cold storage—between 0-4o

12.3.4 Procedures in the CSN Laboratory 

C, and ship it on Monday. 

Special circumstances should be discussed with the SHAL of the lab services 

contractor.

The CSN contracted support laboratory’s procedures for receiving the sampling components and 

field data, disassembling the sampling modules, and handling the filters and denuders after their 

distribution to the various laboratories are covered in the CSN laboratory’s QAPP, which is 

posted on the EPA AMTIC website. 

12.4 Filter and Sample Archival in the CSN Support Laboratory

The contracted support laboratory’s data base will assign a tracking number to all sample filters. 

Extracts and remnants of filters will be archived in cold storage. Custody procedures for 

inventorying and archiving these materials are given in the support laboratory’s document 

Quality Assurance Project Plan: Chemical Speciation of PM2.5 Filter Samples. 
PM2.5 CSN QAPP

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13.0 Analytical Methods Requirements

Analytical methods requirements have been extracted from the Quality Assurance Project Plan 

(QAPP) for the contracted support laboratory which serves the Chemical Speciation Network 

(CSN) and other state, local and/or Tribal (SLT) agency speciation sampling programs. (See 

http://www.epa.gov/ttn/amtic/specguid.html.) They are listed below: 

“B.4 Analytical Methods Requirements

B.4.1 Gravimetric Mass Determination

Standard Operating Procedure for PM2.5 Gravimetric Analysis describes the procedure to be 

used for gravimetric mass determination in RTI’s laboratory.

B.4.2 EDXRF Analysis for Elements

Standard operating procedures used by RTI and CHESTER LabNet for EDXRF analysis are 

listed below:

RTI

Standard Operating Procedures for X-Ray Fluorescence Analysis of PM2.5 Deposits on Teflon 

Filters

CHESTER LabNet

• Standard Operating Procedures for the Sample Receipt and Log In 

• Standard Operating Procedures for the Analysis of Elements in Air Particulates by XRF 

(Kevex 771)

• Standard Operating Procedures for the Analysis of Elements in Air Particulates by XRF 

(Kevex 770 and 772) 

• Standard Operating Procedures for the Kevex Spectrometer Data Generation, 

Interpretation, and Reporting 

• Standard Operating Procedure for the Kevex XRF Spectrometer Calibration 

B.4.3 Extraction and Analysis of Anions and Cations

For an overview of RTI’s laboratory facility and procedures for extraction and analysis of anions 

and cations, including nitrate and sulfate, see: 

• Standard Operating Procedure for Cleaning Nylon Filters Used for Collection of PM2.5 

Material 

• Standard Operating Procedures for PM2.5 Anion Analysis 

• Standard Operating Procedures for PM2.5 Cation Analysis

B.4.4 Carbon Analysis

RTI’s laboratory facility and procedures for organic, elemental, carbonate, and total carbon 

analysis by the CSN TOT method are detailed in the Standard Operating Procedure for the 

Determination of Organic, Elemental, and Total Carbon in Particulate Matter Using a 

Thermal/Optical-Transmittal Carbon Analyzer. 
PM2.5 CSN QAPP

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DRI’s laboratory facility and procedures for OC/EC analysis by the IMPROVE_A/TOR-TOT 

method are detailed in the Standard Operating Procedure for Thermal/Optical Reflectance 

Carbon Analysis of Aerosol Filter Samples. 

RTI’s laboratory facility and procedures for OC/EC analysis by the IMPROVE_A/TOR-TOT 

method are detailed in three SOPs:

Standard Operating Procedures for Temperature Calibration of the Sample Thermocouple in 

a Sunset Laboratory or a DRI Model 2001 Carbon Aerosol Analyzer

Standard Operating Procedure for the Determination of Carbon Fractions in Particulate 

Matter Using the IMPROVE_A Heating Protocol on a Sunset Laboratory Dual-Mode Analyzer 

Standard Operating Procedure for the Determination of Carbon Fractions in Particulate 

Matter Using the IMPROVE_A Heating Protocol on a DRI Model 2001 Analyzer 

While the CSN/TOT analysis and the IMPROVE/TOR-TOT analysis are similar in technical 

approach, and both require heating ramps under non-oxidizing conditions followed by heating 

ramps under oxidizing conditions, the two methods are fundamentally different in the way they 

define carbon fractions. The CSN/TOT analysis is a timed analysis with fixed times at each 

temperature in the heating profile, and the IMPROVE/TOR-TOT analysis is an event-driven 

analysis with the sample remaining at a given temperature until evolution of carbon from the 

filter drops to near zero. A CSN/TOT analysis runs for a total of 12 minutes; an 

IMPROVE_A/TOR-TOT analysis may take anywhere from 15 minutes to 70 minutes. The 

maximum temperatures for the various fractions are also different as are the way that “Peaks” are 

defined. For the CSN/TOT analysis, the five OC peaks are defined as their contributions to OC. 

For CSN/TOT, the sum of the five OC peaks is always equal to OC. For the IMPROVE_A/TORTOT method, the four OC peaks and the three EC peaks are independently calculated without 

regard to the OC/EC split and pyrolyzed carbon has a negative value if the OC/EC split comes 

before the addition of oxygen. Table B.4.1 below describes and compares the carbon fractions 

measured for both methods and the conditions (e.g., non-oxidizing or oxidizing atmosphere and 

maximum temperature) under which each fraction is measured. 

B.4.5 Semi-volatile Organic Compounds

SVOCs will be analyzed by RTI’s subcontractor DRI. The analysis is detailed in DRI’s Standard 

Operating Procedures for Analysis of SVOC by GC/MS. 

B.4.6 Characterization of Particles by Electron and Optical Microscopy

RTI will provide SEM and optical microscopy for characterization of particulate samples. RTI 

has extensive experience in the analysis of airborne PM by both optical and electron microscopy 

techniques, having analyzed a large number of PM10 filters by optical microscopy for several 

state air quality agencies and a significant number of air filters for commercial firms.

B.4.6.1 Scanning Electron Microscopy

SEM can be employed to characterize individual particles collected on a filter. Particles may be 

sized and the morphology described on an individual basis. The composition of a particle may be 
PM2.5 CSN QAPP

Section No. 13

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determined by EDXRF. Characterization of a large number of particles provides information as 

to the particle size, distribution, and chemistry of the PM. Any of several filter media can be used 

to collect particulate material, but smooth-surface filters such as polycarbonate filters are far 

superior for the purposes of analysis by SEM. The procedures for analysis by particulate material 

by SEM are described in detail in Standard Operating Procedure for Sample Preparation and 

Analysis of PM10 and PM2.5 Samples by Scanning Electron Microscopy. 

B.4.6.2 Optical Microscopy

The RTI optical microscopy laboratory is fully equipped with both stereo binocular and 

polarizing light microscopes (PLM) capable of both reflected and transmitted light analysis. 

Photomicrography capabilities allow for documentation of particle characteristics. No RTI SOP 

currently exists for optical examination of filter media. Procedures will be carried out at the 

direction of the DOPOs, and reporting criteria and formats will be established at the time of the 

initial requests. Analysis by optical microscopy allows for examination of particles having

apparent diameters less than 0.25 μm. Optical characteristics such as color, refractive indices,

bi-refringence, and morphology (size and shape) can be determined, which may aid in the 

identification of particles. The Teflon filter commonly employed in PM2.5 sampling is not a 

suitable substrate for analysis by optical microscopy because the thickness and translucent nature 

of the filter severely limits the transmittal of light. Additionally, the surface of the filter is highly 

irregular, making it very difficult to observe individual particles. Other filter media such as 

mixed cellulose ester (MCE) or polycarbonate provide substrates that are more suitable for 

analysis by optical microscopy. Refer to that QAPP, Quality Assurance Plan: Chemical 

Speciation of PM2.5 Filter Samples, for more information. The contracted laboratory’s QAPP is 

available on the EPA’s AMTIC website: http://www.epa.gov/ttn/amtic/specguid.html. “ 

The CSN laboratory’s technical management and staff organization are presented in Section 4.0 

of this QAPP and the contract support lab’s QAPP. Refer to Section 4.3 and Figure 4-2 for more 

information. 
PM2.5 CSN QAPP

Section No. 14

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14.0 Quality Control Requirements

Quality control (QC) is the overall system of technical activities that measures the performance of an 

ongoing process against established standards to verify that such performance meets the stated 

requirements established by the data user or stakeholder. In the case of the Chemical Speciation Network 

(CSN), QC activities are used to ensure and document that the measurement uncertainties, as discussed in 

Section 7.0, are maintained within specified limits so that the data quality objective for trend detection can 

ultimately be met.

There are three distinct but interrelated functions that the PM2.5 CSN QC program requires of state, local 

and/or Tribal (SLT) field site participants, as follows:

1. The site operator and his or her supervisor must make every effort to keep the sampler 

maintained, cleaned, and operating properly; to retrieve samples according to the network 

schedule; and to ship (cold as prescribed) the samples, field blanks, and trip blanks with 

supporting hand-entered and computer-downloaded data to the CSN contracted support 

laboratory on schedule. 

2. The site operator must control the sampler’s collection process through proper handling of 

cassettes and sampling modules, by properly calibrating samplers, and by conducting both 

scheduled and as-needed performance checks for leaks, flow rate, temperature, and pressure. 

Any out-of-tolerance findings must be followed by corrective actions. 

3. The third function is carrying out validation of data sets sent from the CSN support laboratory 

to the SLT contacts and then reporting the data quality statistics that describe how well the 

accuracy, bias, precision, and completeness goals have been met. 

Table 14-1 contains a complete listing of field QC parameters, their frequency of assessment or period of 

performance, and the acceptance criteria or advisory limits, i.e., measurement quality objectives (MQOs). 

The Contracted Support Laboratory QC procedures are included in its Quality Assurance Plan Chemical 

Speciation of PM2.5 Filters which is available on the EPA Ambient Monitoring technical Information 

Cemter (AMTIC) website at http://www.epa.gov/ttn/amtic/specguid.html. 

The MQOs have been established using two sets of criteria. Some of the MQOs were derived to be 

consistent with the data quality objective (DQO) for identifying a trend of 5 percent (in either direction) 

can be made after 5 years of sampling. Other MQOs are based on requirements for PM2.5 monitoring, set 

forth in the Code of Federal Regulations, or by standards of good practice described in Section 2.12 of the 

U.S. Environmental Protection Agency Quality Assurance Handbook for Air Pollution Measurement 

Systems (U.S. EPA, 1998) available through the AMTIC website. The strategic plan for the Speciation 

Trends Network (STN) (U.S. EPA, 1999) set out the initial QC requirements for field and laboratory 

activities. Those requirements are herein applied to the chemical speciation sites in the NCore network. 

Some acceptability limits have been made more rigorous and a few additional requirements have been 

added due to the historical performance of the network. For consistency, the EPA recommends that all 

chemical speciation sampling sites adopt these MQOs with the exception of monitoring frequency Table 

14-1 also lists the action to be taken if a QC check shows a parameter to be outside of acceptance limits or 

outside of advisory limits, and how the corrective action is demonstrated and documented. Specific 

procedures for implementing field QC activities are in the standard operation procedures (SOPs) in
PM2.5 CSN QAPP

Section No. 14

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Appendix A to this Quality Assurance Project Plan (QAPP). The remainder of this section describes the 

types of QC checks called for in the PM2.5 CSN and the procedures used to calculate values for the 

principal QC indicators. The QC results should be recorded on a form or in a field notebook dedicated to 

this purpose. Some will be included on monthly performance check forms or audit reports and uploaded to 

a website from which data can be extracted, formatted and then posted to the EPA’s Air Quality System. It 

is recommended that results of the QC checks be entered into a control chart or graph to help visualize 

changes or drifts in sensor responses and to alert the site operator to the need for preventive maintenance, 

repair, or replacement of a speciation sampler. Detailed information on multipoint calibrations and repairs 

should be recorded in the field notebook. 
PM2.5 CSN QAPP

Section No. 14

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Table 14-1. MQOs and Associated QC Activities for the PM2.5 CSN

Measurement Frequency

Acceptance Criteria 

(MQO) or Advisory 

Limit 

Corrective Action if Out 

of Specification

Samples or 

Channels

Filter visual checks

by Shipping and 

Handling laboratory

before and after 

each exposure

free of visible defects record in laboratory

database; contaminated 

filter usually discarded 

prior to use; exposed filters 

are flagged or invalidated 

all filter types

Collocation with

another chemical

speciation sampler: 

The result is used to 

calculate precision, 

reported as CV in 

terms of a variation 

in the relative 

percent differences 

in concentrations 

measured by the 

two collocated 

samplers. (This is 

different from the 

CV of flow rates 

explained below.) 

Evaluation of 

precision results

As of 2007, about 

4% of CSN (6 

sites) were 

conducting

collocated 

sampling on a 1-

in-6-day basis(a)

Single event 

Monthly (5 

sampling events)

Annual

see Tables 7.1 and 

7.1a for all maximum

precision limits of 

PM2.5 concentration 

and various chemical 

species concentrations

expressed as % CV

(b) 

Total Carbon 15%

Sulfate ion 10%

Nitrate ions 10%

Trace elements 20%

If Avg. CV (of a 

sampling event) > 2σ 

of the previous 3 

year’s average of CVs 

for the sampling site 

If CV > 1.05 σ of the 

previous 3 year’s 

average CV 

If CV > 0.5σ of the 

previous 3 year’s 

average CV or the 

DQO whichever is 

greater

Present data to ad hoc 

workgroup to determine if 

the acceptance limits are 

appropriate. Review trends 

analysis data to determine 

if a 5% trend over 5 years 

is discernable. If yes, 

readjust % CV 

requirements.

 

Review analytical history 

with contract support lab.

Review flow checks and 

flow CV’s for individual 

sampling events. Field 

blanks for evidence of 

contamination. Review 

Shipping procedures and 

delivery records. Initiate 

TSA of site and lab retain 

data or invalidate based on 

conclusions 

all sampling 

media
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Measurement Frequency

Acceptance Criteria 

(MQO) or Advisory 

Limit 

Corrective Action if Out 

of Specification

Samples or 

Channels

Temperature:

Check Monthly ± 2oC of a certified 

transfer standard

note on QC data form; 

troubleshoot; recalibrate or 

replace sensor and conduct 

recheck; Consult with 

manufacturer if outside of 

limits in 2 of any 3 

contiguous months.

all temperature 

sensors

Audit Quarterly ± 2oC of a NISTtraceable standard that 

is independent of the 

monthly check 

standard

note on data form; review 

monthly performance 

checks; recalibrate or 

replace sensor; re-audit 

after calibration or 

replacement. Consult with 

manufacturer if outside of 

limits in 2 of any 3 

contiguous months.

all temperature 

sensors

Pressure:

Check Monthly ± 10 mmHg vs.

certified NISTtraceable transfer 

standard

note on data form; 

recalibrate or and replace 

sensor if not responsive; 

and conduct recheck. 

Consult with manufacturer 

if outside of limits in 2 of 

any 3 contiguous months.

barometric 

pressure sensor

Audit Quarterly ± 10 mmHg vs. a 

NIST-traceable 

standard that is 

independent of the 

monthly check 

standard

note on data form; review 

monthly performance 

checks; advise 

recalibration or 

replacement of sensor; reaudit after calibration or 

replacement. Consult with 

manufacturer if outside of 

limits in 2 of any 3 

contiguous months.

barometric 

pressure sensor
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Measurement Frequency

Acceptance Criteria 

(MQO) or Advisory 

Limit 

Corrective Action if Out 

of Specification

Samples or 

Channels

Flow Rate:

Average CV 

Operator Check (d)

& Review 

Single event

flow rate check

Operator Check(e) 

Review after every 

event

Month

MetOne (c)

If CV > 2% of set 

flow , or The avg diff 

between sequential 

pairs of flow readings 

is > 0.13 liters/min)

URG 3000N

If CV > 1% of set 

flow calculated from 

data polled after first 

five minutes

± 5% of NIST 

Traceable standard

Conduct flow check. 

Note deviation on data 

form; review last 6 

monthly flow checks and 

CV data from previous 2 

months monitoring results. 

See Figure 14.1 for 

decision tree

all flow 

channels

-----------------

Flow rate 

one-point audit (e)

Semi-Annual, but 

no intervening 

periods greater 

than 7 months; 

none less than 5 

months unless 

there are more than 

2 audits per year 

± 5% vs. a standard 

that is independent of 

the monthly check 

standard; an 

independent transfer 

standard

Note on audit form; review 

monthly flow rate checks 

performance checks. Use 

decision tree for evaluating 

performance history. See 

Figure 14.1. Advise 

recalibration, repair or 

replacement of sampler. 

Re-audit after calibration 

or replacement of sampler 

or replacement of flow 

related components. 

all flow 

channels
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Measurement Frequency

Acceptance Criteria 

(MQO) or Advisory 

Limit 

Corrective Action if Out 

of Specification

Samples or 

Channels

Blanks(f):

trip blanks

MetOne

Mass, elements, & 

ions 

Carbon (URG3000) 

Eliminated in lieu 

of SHAL blanks 

0% (subject to 

change if

significant

contamination is 

detected) 

 

2%

refer to support 

laboratory QAPP. 

If collected, 15 μg/ 

filter 

5.64 μg/filter (g)

Review SHAL blanks and 

SHAL loading and 

unloading procedures N/A

one per channel

one per 

cartridge

field blanks

MetOne

Mass, 

elements, 

& ions

Carbon (URG3000)

3% or one set 

every 10 sampling 

days (subject to 

change)

10% 

10% 

backup 

filters

30 μg mass per filter; 

other limits apply to 

chemical species 

concentrations (refer 

to lab QAPP)

6.0 ug/filter (g)

retroactive troubleshooting 

and/or data validation after 

notification by support 

laboratory

one per channel

Carbon sampler 

uses only one 

channel per 

event

SHAL Blanks MetOne 2% of all 

PTFE modules; 

(nylon filter 

modules assumed 

= 0.0 ug/filter) 

URG 3000N Same 

as Trip Blanks 

MetOne—to be 

established as avg of 

up to 3 years 

preceding current year 

+ 2 Std Dev.

URG 3000N— 

1.8 μg/filter(h)

Review SHAL blanks and 

SHAL loading and 

unloading procedures

PTFE Module

Randomly 

select one of 

loaded cassettes

(a) The number and location of sites that have produced collocated measurements in the CSN have been constant 

through the life of the program at least through 2011. It is anticipated that some of the sites may be relieved of this 

duty and a number of samplers redeployed to other sites for 1-year terms. 

(b) See 40CFR part 58 appendix A section 4.2.1. 

(c) This is a new QC check instituted as a warning mechanism for abnormal or deteriorating sampler performance. 

The Average Flow CV is reported by the sampler at the end of every sampling event along with max/min 

temperatures and pressure. The MetOne and the URG calculates the CV from an average of all polled data from 

the onset of the sampling event. The average CV has always been computed by the MetOne and recorded on the 

even COC and field data form. It will be included in the batch event result files upon implementation of the new 

MQOs specified in this QAPP revision, approximately January 1, 2012. 

(d) The maximum expected CV for the MetOne was reported in a conversation between Dennis Crumpler, EPA, 

OAQPS and Michael Putnam, Technical Service Manager for MetOne, September 26, 2011. The expected CV for 
PM2.5 CSN QAPP

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the URG flow rate should be less than 1% based on a couple of years of data captured from the URG memory 

card.

(e) The one-point flow rate check should be taken when sampler is supposed to be operating at its design flowrate

(6.7 L/min in the case of the MetOne SASS sampler, and 22.0 L/min for the URG3000N); monthly flow check or 

audit result should be within ± 5% of design flow. 

(f) Over the first 10 years of the program, the frequency of blank generation has been decreased based on the 

consistency of the data that has been generated from them and the routinely low contamination values. An SLT 

and EPA may call for additional trip and or field blanks if results suggest evidence of contamination at one or both 

steps in the process.

(g) Based on the highest mean+2σ value (1 std dev added to the mean) in the first 3 years of operation. See Annual 

Data Summary Report for the Chemical Speciation of PM2.5 Filter Samples Project at 

http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/

(h) Based on the first year 2010 of SHAL data provided by RTI and DRI. 
PM2.5 CSN QAPP

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14.1 Quality Control Checks

14.1.1 Checks

A parameter check, as used in this QAPP, is described as a verification, through the of a NIST traceable 

reference standard, that the sampling instrument is operating within acceptance limits. Usually, if the 

check shows a failure to meet specification, troubleshooting and instrument recalibration and final 

verification should follow. Calibration is discussed in Section 16. Figure 14-1 is the current report form 

that can be used to record and report the QC checks that should occur on a monthly basis. This form may 

be revised occasionally to reflect improvements in procedures either in the field or in data handling. The 

actual form is an Excel Workbook that can be downloaded from a website that is managed by the lab 

support contractor for the CSN. (This website has restricted access to only those agencies or their 

contractors that perform QC checks and audits.) 

14.1.2 Audits and Independent Checks

The chemical speciation sampler(s) will be audited with an independent, National Institute of Standards 

and Technology (NIST)-traceable transfer standard on at least a semi-annual basis. NIST-traceable 

transfer standards are commercially available. Flow rate, temperature, and barometric pressure will be 

checked. For samplers with multiple flow channels, each channel and the associated sensors will be 
PM2.5 CSN QAPP

Section No. 14

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audited. The transfer standards may be verified against an agency’s primary reference standard annually 

but transfer standards should be certified by an independent metrology lab or the manufacturer’s facility 

every third year. Primary standards against which transfer standards are verified must be recertified or 

recalibrated annually. Recertification or recalibration can occur at the manufacturer’s facility or at a 

metrology laboratory that uses current NIST-traceable equipment of a higher precision and accuracy. 

The CSN laboratory must also assess the accuracy of its analytical measurements. This will include 

assessment of field blanks and other samples supplied by the EPA quality assurance (QA) laboratory. 

Refer to the CSN laboratory QAPP for more information. 

14.2 QC Samples

Several types of standard QC samples are defined. The field program will mainly be concerned with 

blanks sent from time to time by the CSN support laboratory to assess the effects of field operations and 

shipping and handling. 
PM2.5 CSN QAPP

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Figure 14-2. CSN QA/QC Report Form

Chemical Speciation Network

Flow Check Worksheet

MetOne SASS - Primary Sampler version 25

Note - Cyan fields are entered from URG worksheet or calculated - yellow fields are to be filled in here

Location Date

AQS Site ID Missing Date, Site Name, Site Code, or POC

AQS Sampler POC 5

Site Information

Sampler Type (Model)

Operator(s) Affiliation

Check Type

Sampler S/N

Head S/N

Pump S/N

Last Calibration Date

Reference Standards

Flow Reference Std Model Standard S/N

Specify if "Other" Calibration Date

Temperature Ref Std Model Standard S/N

Specify if "Other" Calibration Date

BP Std Model Standard S/N

Specify if "Other" Calibration Date

Significant 

Findings:

General 

Findings:

Select From Dropdown List

Select From Dropdown List

Select From Dropdown List

Flow Verification by Site Operator

Select From Dropdown List
PM2.5 CSN QAPP

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Flow Check

For the reference standard, enter "UR" for under range and "OR" for over range flow readings.

L/min % Difference Within ± 10%?

Lower Limit Ref Std Upper Limit SASS SASS - Ref Pass Fail

Channel 1 NA NA

Channel 2 NA NA

Channel 3 NA NA

Channel 4 NA NA

Channel 5 NA NA

Channel 6 NA NA

Channel 7 NA NA

Channel 8 NA NA

Retest after Calibration

L/min % Difference Within ± 10%?

Lower Limit Ref Std Upper Limit SASS SASS - Ref Pass Fail

Channel 1 NA NA

Channel 2 NA NA

Channel 3 NA NA

Channel 4 NA NA

Channel 5 NA NA

Channel 6 NA NA

Channel 7 NA NA

Channel 8 NA NA

MetOne SASS - Primary Sampler

Clock Check

 5 minutes or less?

Ref Std SASS Pass Fail

Check Time

Date 1/0/1900 Missing Sampler Date!

Recalib Time

Date 1/0/1900

Leak Test

Initial Check After Correction

A L/min B L/min Pass Fail A Fail B

Channel 1 Channel 1

Channel 2 Channel 2

Channel 3 Channel 3

Channel 4 Channel 4

Channel 5 Channel 5

Channel 6 Channel 6

Channel 7 Channel 7

Channel 8 Channel 8

 Greater than 0.10 L/min fails

If Local Time is under daylight savings, convert Ref Std to Local Standard Time. Daylight Saving Time begins 

for most of the United States at 2:00 a.m. on the first Sunday of April. Time reverts to standard time at 2:00 a.m. 

on the last Sunday of Octobe

Difference 

Minutes

Time (hh:mm)
PM2.5 CSN QAPP

Section No. 14

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MetOne SASS - Primary Sampler

Reference Standard vs Design Flow

L/min % Difference Within ± 10%?

Lower Limit SASS Upper Limit Ref Std Ref-Design Pass Fail

Channel 1 6.03 6.7 7.37

Channel 2 6.03 6.7 7.37

Channel 3 6.03 6.7 7.37

Channel 4 6.03 6.7 7.37

Channel 5 6.03 6.7 7.37

Channel 6 6.03 6.7 7.37

Channel 7 6.03 6.7 7.37

Channel 8 6.03 6.7 7.37

Retest after Calibration

L/min % Difference Within ± 10%?

Lower Limit SASS Upper Limit Ref Std Ref-Design Pass Fail

Channel 1 6.03 6.7 7.37

Channel 2 6.03 6.7 7.37

Channel 3 6.03 6.7 7.37

Channel 4 6.03 6.7 7.37

Channel 5 6.03 6.7 7.37

Channel 6 6.03 6.7 7.37

Channel 7 6.03 6.7 7.37

Channel 8 6.03 6.7 7.37

Ambient Temperature Check

Degrees C

Lower Limit Ref Std Upper Limit SASS Difference Pass Fail

NA NA

Retest After Recalibration

NA NA

Within ± 2 degrees?
PM2.5 CSN QAPP

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MetOne SASS - Primary Sampler

Filter Temperature Check

Degrees C

Lower Limit Ref Std Upper Limit SASS Difference Pass Fail

Channel 1 NA NA

Channel 2 NA NA

Channel 3 NA NA

Channel 4 NA NA

Channel 5 NA NA

Channel 6 NA NA

Channel 7 NA NA

Channel 8 NA NA

Retest After Recalibration

Channel 1 NA NA

Channel 2 NA NA

Channel 3 NA NA

Channel 4 NA NA

Channel 5 NA NA

Channel 6 NA NA

Channel 7 NA NA

Channel 8 NA NA

Pressure Check

mm Hg

Lower Limit Ref Std Upper Limit SASS Difference Pass Fail

NA NA

Retest after recalibration

NA NA

Within ± 2 degrees?

 Within ± 10 mm?

14.2.1 Blanks

Field Blanks—These provide an estimate of total measurement system contamination. By comparing 

information from laboratory and SHAL blanks against the field blanks, the amount of contamination due 

to field activities can be estimated. In addition, if trip blanks are utilized, one can further evaluate 

contamination occurring during field operations. Field blanks, loaded in sampling modules, for each type 

of filter will be sent from the laboratory. The field operator is to handle the field blank sampling module 

just as he/she would a module to be exposed but without drawing a sample through it. Corrective actions 

will be taken when excessive contamination is found on field blanks. 

The CSN support laboratory will also determine blank concentrations of analytes for each lot of TeflonTM, 

nylon, or quartz fiber filters received. The CSN support laboratory’s QAPP and its SOPs discuss the 

procedures.

Trip Blanks—These provide an estimate of measurement system contamination during transport to and 

from the field sites. Trip blanks are usually instituted when field blank contamination is a problem or to 

understand the measurement uncertainty introduced by contamination during transport. Trip blanks are
PM2.5 CSN QAPP

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sent to the field as a normal sample but remain unopened. They are processed as a normal field sample 

and sent back to the support laboratory and treated as a routine sample from the point of sample receipt 

and beyond. As a practical matter, trip blanks are a measure of contamination introduced during the 

loading of filters into cassettes and cassettes into the sampling modules or cartridges. The number of trip 

blanks as percentage of the total number of filters (of each type) has been reduced over the life of the CSN 

due to the very small values that have been observed. The MQO plan, as of 2011, is to eliminate the trip 

blanks for the MetOne filters and reduce the URG trip blanks to 2 percent of the routine filters that are 

shipped for sampling. If episodes of sustained high loads of contamination occur trip blanks may be 

reinstituted to assist in determining the source(s) of contaminants. 

SHAL Blanks―These blanks are generated by the lab service contractor to assess how much 

contamination might be introduced to the filters during the loading into the cassettes and canisters or 

cartridges. These are more informative than trip blanks as a rule. They will replace the MetOne trip blanks 

that were collected as QC controls during the first 12 years of the STN. The URG 3000N deployment 

instituted SHAL blanks at its inception in 2008. 

14.3 Collocated Samplers

Collocated sampling occurs at approximately 4 percent of sites in the CSN (6 sites listed in Section 7) and 

4 of which are in the NCore network. Data sets from collocated samplers are intended to assess the 

precision of the total sampling, analysis, and data handling process, but they can also be very useful in 

troubleshooting sampler siting and operational problems. Thus, such data are useful in detecting quality 

problems that may not be evident from the results of periodic QC checks of flow rates, temperature, and 

pressure. Refer to Section 14.4.2 through 14.4.4 for discussion and procedures for estimating bias and 

precision from collocated sampler data sets.

14.4 Calculations of Accuracy, Bias, Precision, and Completeness

Accuracy is defined as the degree of agreement between an observed value and a true value or an accepted 

reference value. It includes a combination of random error (precision) and systematic error (bias). The 

following four accuracy/bias-related checks and audits are conducted in the chemical speciation program:

Flow Rate, Temperature, Barometric Pressure, and Other Checks Against a NIST-Traceable 

Standard 

The ability to separate PM2.5 from larger size particles is due to the inherent design of the separation 

device (whether a cyclone or impactor) in a given sampler. The performance of the separation device is a 

function of the flow rate, i.e., velocity of the air stream that is conducted through it. Consequently, the 

ability of the sampler to maintain the designed flow rate is a critical performance parameter. The periodic 

measurement of the sampler’s actual flow rate by a NIST-traceable reference standard constitutes the most 

accepted surrogate for measuring the accuracy of the sampler’s results. In this case, the deviation might be 

called a bias since the cut point of the PM would be directionally influenced by whether the velocity is 

less than or greater than the design value for the given separator. A single flow check or audit, however, 

only indicates the potential bias by the sampler since the last flow check or audit in which the flow was 

within advisory limits or acceptance criteria. Systematic bias by the sampler can only be established by a 

series of flow checks and calibrations. If the flow checks reveal that the flow rate varies plus and minus of 

the calibration set point then there is no systematic bias. If the flow checks reveal the flow rate always 

drifts in one direction from the calibration set point, then there is a systematic bias. However, it should 
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never fall outside of acceptance limits without a remedial follow-up. Consequently, long-term bias should 

not occur. 

< Collocation with a Federal Reference Method (FRM) sampler (gravimetric only)

 < Collocation with another PM2.5 speciation sampler (all analytes)

< Gravimetric balance checks and other laboratory performance audits. 

Balances are challenged with class 1 metallic reference standards. Analytical procedures are challenged 

with known reference and internal standards and by interlaboratory performance evaluations of single 

blind samples prepared by a facilitating laboratory, EPA’s Office of Radiation and Indoor Air/National 

Air and Radiation Environmental Laboratory in Montgomery, Alabama. 

14.4.1 Percent Difference of a Single Measurement

Specifically for: Temperature; 

 Barometric pressure; 

 Other checks against a known standard

The error inherent in any single measurement is a function of both the underlying bias and the imprecision 

(noise) in the measurement. Only after repeated measurements over a period of time is it possible to 

separate bias and precision. 

 

The percent difference, di, is calculated from a standard of known value or an accepted reference value. 

Calculate the percentage difference (di) for a single calibration check, i, using the following equation: 

Equation 1

 d meas audit

audit i = − ⋅100

 

Where:

 di = percentage difference for a single parameter check

audit = parametric value as measured by the audit standard used in the QC check 

meas = parametric value indicated by the monitoring organization’s instrument 

With respect to the CSN, Equation 1 applies to concentrations or flow rates, and not to Temperature (T) 

and Barometric Pressure (P). For T and P, agreement is usually expressed in terms of absolute differences 

in measurements (i.e., within +/- 2oC or within 10 mm Hg). 

Flow rate: 
PM2.5 CSN QAPP

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d audit design

design if = − ⋅ 100

Equation 1 could be used to characterize a test of the sampler’s calibrated flow rate. This determination is 

adequate if the sampler’s “meas” flow is at or near the design value for achieving the proper separation 

and collection of PM2.5 for the separation device used with that sampler. However, if the “meas” flow is 

substantially different than the design flow rate it may actually pass the acceptance criteria according to 

the equation in 40 CFR part 58 Appendix A for flow check, but it could generate a significantly inaccurate 

sample of PM2.5. For example, if a MetOne speciation sampler says its flow rate is 9.8 lpm and the flow 

standard indicates it is 10.0, the value is a perfectly acceptable 2.0 percent low but the cut point is 10 

percent or more lower than it should be, because the actual flow rate is 30 percent too high. In other 

words, the sampler is performing perfectly wrong. However, the audit value needs to be compared to the 

design flow rate of the sampler to have any real relevance to accuracy. Consequently, a second equation 

should also be used for single point flow rate checks and audits: 

Equation 1a

 

 

Where:

 difr = percentage difference for a single flow rate check

audit = actual flow rate of sampler based on the measurement by a NIST-Traceable

standard

design = the design flow rate of the sampler as specified by the manufacturer

14.4.2 Percent Difference for Collocation with a Federal Reference Method (FRM) Sampler 

(Gravimetric Only) and Collocation With Another PM2.5 Speciation Sampler (All 

Analytes) 

If one takes the position that any given FRM sampler is a representation of the true PM2.5 mass sampled at 

its location, the comparison of the total mass derived from the FRM sampler could arguably be a basis for 

a relative accuracy or bias of a speciation sampler that is collocated with it. If a number of collocated 

measurements indicate that the total masses measured by both are essentially equal, then we can postulate 

that at least the speciation samplers are relatively accurate with respect to the FRM total mass 

measurements. If they are different, then we must determine if the difference is systematic, a true bias, or 

if it is random. It has been established that the masses determined by FRM vs. the CS samplers are 

statistically different.1

 

1 See Evaluation of PM2.5 Chemical Speciation Samplers for Use in the EPA National PM2.5 Chemical Speciation Network. 

EPA-454/R-01-005 <http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/fourcty.pdf>

 The dominant sampler in the speciation network, the MetOne SASS or SuperSASS, 

does not use the same flow rate as the PM2.5 speciation samplers based on the FRM design; it is 

considerably lower, i.e., 6.7 liters per minute. Therefore, it uses a differently designed separator than a 

PM2.5 FRM sampler. The speciation samplers that were designed to pull 16.67 liters per minute through a 

Teflon filter were replaced by MetOne SASS samplers in 2008. The comparison of the total gravimetric 

mass derived from a speciation sampler to that obtained by a collocated FRM sampler may be more 

accurately described as a measurement of bias. It must be noted that the recovery, shipping and storage 
PM2.5 CSN QAPP

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procedures of speciation filters is also different than FRM PM2.5 filters, which could also create more 

randomness due to the character of the aerosols that are collected in different areas of the country. There 

are no other independent constituent analyses so that a similarly calculated bias for the ions and carbon are 

not possible.

Precision is estimated for manual instrumentation via duplicate measurements from ostensibly identical 

collocated samplers providing filter samples containing analytes above minimum detectable 

concentrations. 

Since there are only six collocation sites across the CSN, precision can only be aggregated at the network 

level on a quarterly, annual, and the multi-year basis. For each collocated data pair, the relative percent 

difference, di, is calculated by Equation 2. 

Equation 2

( ) d

X Y

X Y i

i i

i i

= −

+ ⋅ / 2

100

Where: 

 di = the percent difference of concentration of the selected analyte (μg/m3) determined for the 

samplers, divided by the average of the two concentrations, 

 Xi = the concentration of the primary sampler, and 

Yi = the concentration value from the, i.e., the collocated sampler

14.4.3 Calculation of Bias 

Bias is a systematic deviation from the true value. Data must be averaged or aggregated over a period of 

time or over a set of measurements in order to assess bias. Bias can be used to assess systematic errors of a 

single sampler, a reporting organization, or an entire network. For example flow rate checks over a year 

can provide some sense of whether the network sampler(s) flow rate drifts positive or negative from the 

calibration value over a period of time. When the chemical speciation network was first deployed there 

were several sites to which all three of the legacy samplers were deployed to determine if there was a 

relative bias introduced by one, two or all of them. A report suggested that bias was present but was siteand constituent-specific. 2

The following equation is used to calculate bias:

 

Equation 3

bias AB t

AS

n

= + ⋅ 0 95 n −1. ,

where n is the number of single point checks being aggregated; t0.95,n-1 is the 95th quantile of a tdistribution with n-1 degrees of freedom; the quantity AB is the mean of the absolute values of the di’s 

 

2 Evaluation of PM2.5 Chemical Speciation Samplers for Use in the EPA National PM2.5 Chemical Speciation Network, Paul 

A. Solomon, et.al EPA-454/R-01-005, May 2001. http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/fourcty.pdf. 
PM2.5 CSN QAPP

Section No. 14

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(calculated by Equation 2) and is expressed in Equation 4 as follows: 

Equation 4

and the quantity AS is the standard deviation of the absolute value of the di’s and is calculated using 

Equation 5 as follows: 

Equation 5

 

 

Since the bias statistic as calculated in Equation 3 above uses absolute values, it does not have a tendency 

(negative or positive bias) associated with it. A sign will be designated by rank ordering the percent 

differences (di’s) of the QC check samples from a given site for a particular assessment interval. Calculate 

the 25th and 75th percentiles of the percent differences for each site. The absolute bias upper bound should 

be flagged as positive if both percentiles are positive and negative if both percentiles are negative. The 

absolute bias upper bound would not be flagged if the 25th and 75th percentiles are of different signs (i.e., 

straddling zero). 

Bias can also be expressed as a percentage of the standard or expected value. This definition is applicable 

to flow rate, temperature, barometric pressure, and derived quantities such as air volume through a filter. 

Laboratory biases can be calculated in a similar way. 

14.4.4 Calculation of Precision 

Precision defines the random variability of a set of measurements and excludes systematic bias. The 

precision estimate is used to assess the one-point QC checks for repeated parametric measurements or 

laboratory measurements of target analytes (soil elements, nitrate, sulfate, ammonium, OC, and EC). The 

precision estimator is the coefficient of variation upper bound and is calculated using Equation 6 as 

follows: 

AB

n

d i

i

n

= ⋅

=

∑1

1

( ) AS

n d d

n n

i

i

n

i

i

n

=

⋅ −















−

= =

∑ ∑ 2

1 1

2

1
PM2.5 CSN QAPP

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Equation 6

 

 

where χ2

0.1,n-1 is the 10th percentile of a chi-squared distribution with n-1 degrees of freedom. 

Precision can be used to assess the random errors inherent in a single sampler, a reporting organization, or 

an entire network. Random errors, characterized by the precision calculations, can be used as input to the 

DQO model for the assessment of data trends. Excessive variability or noise in data can also indicate 

equipment malfunction and the need for corrective action. 

There are several other ways of expressing precision of a measurement, including the CV and the 

confidence interval. The precision of a measurement is often a function of several different sources of 

random variation. For example, the precision of a calculated particulate concentration may be a function 

of the variability of measurement in calculating the flow rate, sampling temperature, and pressure or the 

variability introduced in shipping/handling and by the laboratory. Assessment of these errors is beyond the 

scope of this QAPP but should be considered when performing advanced statistical analysis of the data.

14.4.4 Calculation of Completeness 

The goal for completeness is 75 percent. Meeting the DQO for identification of a systematic trend in the 

data requires that the data meet minimum completeness criteria. Data must span the time range of interest, 

and there must be a sufficient number of measurements to reduce the statistical uncertainties. The DQO 

analysis found that 1-in-3 day sampling was sufficient to meet the DQO for assessing a data trend after 

5 years provided other uncertainties described above are controlled. Significant data loss, however, could 

compromise the ability to assess the DQO. 

Completeness should be assessed quarterly and annually as shown in the following equation: 

where

%C = percentage completeness

 Nt = the total number of possible or potential measurements in the data set 

 Ninvalid = the number of missing or invalidated measurements 

Assessment of completeness is applicable to derived measurements such as elemental concentration in the 

air (for assessment of the DQO). Maintaining the level of data completeness ensures that the minimum

number of valid concentration data points are available to meet the DQO for speciation trends 

identification after 5 years of monitoring. To be counted for completeness, a sample must have passed all 

of the various screens in the data validation process. Thus, a particular sample can be invalidated in 

( ) 2

1,1.0

1

2

1

2

1

12 −

= = − ⋅ −





 



 −⋅

=

∑ ∑

n

n

i

n

i

i i

n

nn

ddn

CV

χ

%C

N N

N

t invalid

t

= − × 100
PM2.5 CSN QAPP

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several different ways. Completeness assessment is an important element in the oversight of operational 

and laboratory activities. Poor or marginal completeness figures should prompt the reporting organization 

to re-evaluate and improve operating procedures.

14.5 References

U.S. EPA (Environmental Protection Agency). 1998. Quality Assurance Guidance Document 2.12. 

Monitoring PM2.5 in Ambient Air Using Designated Reference or Class I Equivalent Methods. April 1998. 

U.S. EPA (Environmental Protection Agency). 1999. Strategic Plan: Development of the Particulate 

Matter (PM2.5) Quality System for the Chemical Speciation Monitoring Trend Sites. April 16, 1999. 

U.S. EPA (Environmental Protection Agency). 2006. Code of Federal Regulations, Part 58, Appendix A, 

Section 4, “Calculations for Data Quality Assessment.”
PM2.5 CSN QAPP

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15.0 Sampler/Equipment, Testing, Inspection and Maintenance 

Requirements

This section discusses procedures to test, inspect, and maintain PM2.5 

15.1 Testing and Acceptance Criteria

speciation samplers and

support equipment to be used at Chemical Speciation Network (CSN) field sites.

The CSN employs a set of testing and acceptance criteria that were used to accept Federal 

Reference Method PM2.5 gravimetric samplers at 40CFR Part 53, Section 53.34. Table 15-1 lists 

the 13-step procedure by which final acceptance of each of the three originally deployed 

speciation sampler occurred. URG 3000N samplers added to the CSN program in 2007-2009 

were not available for participation in the original intercomparison studies. However, they were 

subjected to a similar initial field tests and the first 59 were run side-by-side with MetOne SASS 

or SuperSASS samplers (on which quartz filters were loaded at channel 3) for a period of at least 

10 sampling events. The collocated events were reduced in deployments 2 & 3. At one point, 13 

CSN sites also have run IMPROVE samplers for network intercomparison data. These sites 

provided yet another set of sampling results to compare with the performance of the URG 3000N 

samplers. The standard operating procedure for the URG 3000N and the Operators Manual both 

provide start-up testing and acceptance criteria. See 

http://www.epa.gov/ttn/amtic/spectraining.html. 

Sampler calibration and verification devices also will require testing and acceptance upon 

receipt. Each of the following devices must arrive with a certificate of National Institute of 

Standards and Technology (NIST) traceability, an instruction booklet, and a warranty statement. 

Simple testing and acceptance methods are listed below:

 Flow rate transfer standard (check against another flow rate standard). 

 Temperature transfer standard (check against a NIST-traceable thermometer,

(preferably a thermistor or thermocouple-based sensor that does not use mercury), ice 

bath, or other temperature standard). 

 Pressure transfer standard (check against another barometer or against a corrected 

barometric pressure reading from a nearby national weather station).

Testing and acceptance criteria for the CSN contracted support laboratory are discussed in the 

Quality Assurance Project Plan (QAPP) prepared by the CSN support laboratory. 

15.2 Maintenance

Many items require maintenance in the CSN. Preventive maintenance should be practiced in 

accordance with the “manufacturer’s instructions” given in the operators’ manuals. This section 

describes maintenance items for CSN field equipment. The CSN contracted support laboratory’s

QAPP discusses laboratory equipment maintenance. Maintenance of speciation samplers is

becoming increasingly important as the equipment ages. CSN site operators and managers 
PM2.5 CSN QAPP

Section No. 15

Revision No.: 1.2.0

Date: 10/11

Page 2 of 4

should read and follow maintenance instructions given in the sampler operator’s manual and 

updates and any maintenance bulletins that may be issued. Table 15-2 lists field items known to 

require preventive maintenance and periodic recertification. Others may be added to this list as 

experience is gained. A 3-year factory service program for maintenance of samplers is planned 

for implementation. 

Table 15-1. Testing and Acceptance Criteria Checklist for PM2.5 Speciation Samplers

Check or Criteria Yes? No?

1. Check the enclosed packing list. Were all parts included in the delivery of the 

sampler? (Including filter packs, denuders, and an operator’s manual)

2. Were any of the enclosed parts broken during shipment of the sampler?

3. Check the enclosed assembly instructions. Did all the parts fit together during 

assembly of the sampler?

4. Does the sampler’s pump turn on when supplied with electrical power?

5. Using an independent timer, check to ensure the timer (clock) operates properly. 

Check to see if the timer will automatically turn the sampler on and off during a 

fixed time by setting the timer to turn the sampler on and off for a short period 

while the operator observes. 

6. Does the sampler’s computer (display screen) boot up and operate properly? Check 

to see if the computer (microprocessor) has working software (firmware) by 

performing manual input of information to the sampler through the keyboard and 

observe the results on the display screen.

7. Does the computer download information properly? Check this process by 

attempting to download stored information through the RS232 port to a computer 

and then to other data transfer devices; or . 

8. Does the internal cooling fan operate properly? Check this function by supplying 

electrical power to the unit and listening for and observing the fan turn on and off.

9. Do the temperature sensors operate properly? Check this function by comparing 

sensor readings to an independent thermometer (or by warming the sensor tip 

between your fingers to see if the temperature rises).

10. Does the filter holder (sampling module, cassette, or filter pack) hold the filter 

correctly and does it connect easily and snugly to other components of the sampling 

stream? Check this function by installing a filter in the sampling module and by 

connecting the module to the sampling manifold, denuder, and so on. 

11. Does the sampler’s casing or other enclosure protect internal units from the 

weather? Check by visually inspecting the unit’s latches, locks, seals, and gaskets 

for gaps, holes, and leaks. Do not disassemble the unit.

12. Does the support structure (base, tripod, and so on) hold the sampling unit secure, 

upright, and level?

13. When all sampler parts are assembled and operated as a unit, does the sampler 

function properly? Check this function by assembling the unit per instructions, 

installing a filter or sampling module, setting the timer, activating the sampler, and 

running it for 24 hours as would be done for routine sampling.

Certifying Official’s Signature __________________Date______ Circle one →→ Accept? Reject?
PM2.5 CSN QAPP

Section No. 15

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Date: 10/11

Page 3 of 4

Table 15-2. Preventive Maintenance and Recertification of CSN Field Equipment

Maintenance Item Recommended Frequency

PM2.5 Speciation Samplers

2. 3. Check sampling inlets, and URG downtubes for bugs and obstructions, and 

water intrusion 

Each visit to site

1. Clean sampler inlet surfaces.

2. Examine O-rings.

3. Clean interior of sampler case (if applicable). 

4. Inspect denuder for breakage (RASS and MASS only). Replace denuders with 

freshly coated ones and return used denuder to laboratory for refurbishment.

5. Inspect and service cooling air intake filter and fans.

Every 30 sampling events 

or more often as needed or 

as specified by the network

1. Inspect O-rings of inlet assembly (if applicable). Apply very light coat of 

vacuum grease if required.

2. Clean sampler downtube (unless it contains a denuder).

3. Inspect and service O-rings of inlet and water seal gasket at downtube entry to 

case if applicable. 

4. Clean cyclones and manifolds upstream of sampler module.

5. Inspect and service O-rings in sampler head or platform assembly of URG 

3000N. 

6. Inspect and service vacuum tubing, tube fittings, and other connections to 

pump and electrical components.

7. Overhaul or replace sampling pump and solenoids.

Quarterly (every 3 months)

Per vendor guidance

Calibration and Check Devices

NIST-traceable flow rate transfer standard

1. Recertify vs. NIST standards.

2. Replace batteries (if applicable).

3. Visually check orifices for dust or breakage.

NIST-traceable temperature transfer standards (digital thermometer)

1. Recertify vs. NIST standards.

2. Replace batteries.

3. Inspect probe tip and connecting cord.

NIST-traceable pressure transfer standard

1. Recertify vs. NIST standards.

2. Replace batteries.

Annually

As needed

Each use

Annually

As needed

Each use

Annually

As needed

15.3 Critical Spare Parts

Maintain an inventory of critical spare parts at the field office to prevent sampler downtime or 

interruption of the required QC checks. The CSN contracted support laboratory will also 

maintain a spare parts inventory to service the sampler modules and denuders. The field site 

should send the laboratory any spare parts associated with the components the support laboratory 

is supplying to the site (for example, O-rings that are part of the sampling module that is sent 

back and forth between the contracted support laboratory and field site) so that these components 

may be serviced at the contracted support laboratory.
PM2.5 CSN QAPP

Section No. 15

Revision No.: 1.2.0

Date: 10/11

Page 4 of 4

 Speciation sampler

O-rings for downtube connections (if applicable) 

Vacuum/pressure tubing and connecting compression or other types of fittings 

Filter packs or cassettes (to be forwarded to CSN support laboratory) 

Denuders (to be forwarded to CSN support laboratory) 

Sampling lines/tubing (as applicable)

Fuses

 Digital thermometer, pressure device and flow transfer standard 

Spare batteries

Spare temperature probe

Spare tubing 
PM2.5 CSN QAPP

Section No. 16

Revision No.: 1.2.0

Date: 10/11

Page 1 of 6

16.0 Instrument Calibration and Frequency

16.1 Overview

Calibration is the comparison of a measurement standard or instrument with another reference 

standard, a reference material, or reference instrument to quantify and report, any difference or 

variation (deviation) from the reference value. The purpose of calibration is to minimize bias; 

therefore, calibration may include adjustment of the performing measurement device or 

instrument so that it measures and reports values that closely replicate those same values 

represented by standard reference materials or reference devices. For PM2.5

1. Certifying the calibration standard and/or transfer standard against an authoritative 

standard (usually those produced by the National Institute of Standards and 

Technology (NIST) or reference standards certified to be a certain accuracy based on 

procedures developed by the NIST).

chemical speciation 

instruments, calibration activities follow a two-step process:

2. Comparing the routine sampling or analytical instrument against a calibration or 

transfer standard.

Parameters of the chemical speciation samplers that are subject to routine calibration checks in 

the field include the following:

 Flow rate (all filter channels). 

 Ambient temperature (one per instrument). 

 Filter or manifold temperature (one per channel or instrument). 

 Barometric pressure (one per instrument). 

Calibrations that involve permanent changes due to instrument adjustments should only be 

initiated when it is obvious that a measurement parameter does not meet its acceptance criteria. 

Therefore, the Chemical Speciation Network (CSN) uses a two-tiered approach to calibration 

that involves the following: 

 Checks (see Section 14) to ensure that calibration is within acceptance criteria.

 Multipoint calibration when there is a failure during a one-point check or audit. 

Instrument adjustments occur during multipoint calibrations and are followed by a 

one-point check to ensure that the transfer check standard is also operating properly. 

16.2 Calibration and Verification of Field Instrumentation

Calibrations and checks for the chemical speciation samplers should generally follow the 

schedule set for the PM2.5 Federal Reference Method (FRM) total mass monitoring program. The 

speciation samplers are similar to the PM2.5 FRM filter-based samplers in that they draw air 

through a filter. They also measure and record ambient temperature, barometric pressure, 

date/time and elapsed time of the sampling event. The samplers also poll the flow rate on a 
PM2.5 CSN QAPP

Section No. 16

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Page 2 of 6

prescribed schedule and calculate the coefficient of variation in flow over the entire sampling 

event. They may differ from the PM2.5 

After receipt and acceptance of a new chemical speciation sampler, single point calibrations of 

temperature, barometric pressure, and multipoint calibrations of the flow rate sensors will be 

performed. After installation, regular checks and maintenance are carried out by the CSN site 

operator at the specified intervals. During each quarter, an internal audit is performed using an 

independent set of standards. These checks are detailed along with the acceptance criteria in 

Table 16-1. 

FRM samplers; however, with respect to the flow rates, 

the number of sampling channels that need to be calibrated, and the number and location of 

internal temperature sensors, and the filter media that is used to collect the filtrate in each 

different channel. The URG 3000N is patterned after the IMPROVE network’s C module that 

collects carbon.

The following calibrations are performed in the field: 

 Verification/calibration of sampler’s temperature probes and against the working 

temperature standard,

 Verification/calibration of the sampler’s barometric pressure sensor against the 

working pressure standard, 

 Verification/calibration of volumetric flow rate meter in the sampler against the 

working flow rate standard, and 

 Verification of the sampler’s internal clock against an accurate timepiece.

Temperature Probes—Each CSN chemical speciation sampler has both ambient and internal 

temperature probes. The CSN site operators will perform one-point field verifications of both 

sensors as needed or at least every month using a digital NIST-traceable temperature probe. A 

quarterly temperature audit will be performed using an independent temperature standard. 

Barometric Pressure—A NIST-traceable digital handheld pressure indicator will be used in the 

field for one-point check of the sampler’s pressure sensor as needed or at least every month. A 

quarterly pressure audit will be performed using an independent pressure standard. A NISTtraceable digital manometer will be used in the field office or field as a primary standard.

Time Sensor—The time sensor should be within + 5 min of a watch that has been recently 

checked and set. Time (operator’s watch) can be set against an atomic clock that can be found on 

the Internet (available online at http://www.time.gov) or through a phone number (303-499-

7111). 

Flow Rate—As needed or at least monthly, a one-point flow rate verification will be performed 

for each sampling stream using a NIST-traceable flow rate transfer standard. A quarterly flow 

rate audit will be performed using an independent flow rate standard. The NIST-traceable 

calibration standard will be used in the field office or field as a primary standard to perform 

multipoint calibrations once a year or after a one-point verification failure.
PM2.5 CSN QAPP

Section No. 16

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Page 3 of 6

Calibration Standards

Temperature, barometric pressure, and flow rate transfer standards that are used to perform 

routine verifications of CSN chemical speciation samplers should be recertified at the same 

intervals as the transfer standards for the PM

—Calibration standards for the temperature, barometric pressure, and flow 

rate verifications and calibrations are given in Table 16-2. All calibration standards must be 

recertified annually. The recertifications must be traceable to NIST. These recertifications may 

be done by the standards’ manufacturer or by a third-party metrology laboratory and must be 

performed in accordance with American National Standard for Calibration - Calibration 

Laboratories and Measuring and Test Equipment - General Requirements (ANSI/NCSl 

Publication No. Z540-1-1994). Records of all certifications must be maintained, including the 

identity of the NIST reference, the procedure used to establish traceability, and a certificate of 

traceability.

2.5 gravimetric samplers. When both gravimetric 

samplers and chemical speciation samplers are situated at the same monitoring location, the same 

equipment and transfer standards may be used for both sets of samplers (if they are compatible 

with all samplers). 

Calibration Procedures—Procedures for temperature, barometric pressure, and clock/timer 

calibrations are typically identical to those used for the PM2.5 gravimetric samplers from the 

same manufacturer, and it may be possible to follow standard operating procedures (SOPs) 

developed for the gravimetric samplers. Procedures for performing flow rate calibrations and 

leak checks for the chemical speciation samplers may differ from the gravimetric sampler by the 

same manufacturer. Chemical speciation samplers typically have several different air sampling 

streams, each of which is used to sample a different group of chemical species. Whenever 

possible, the individual flow rates should be calibrated independently of each other. In some 

models, however, this may not be possible due to the use of vacuum manifolds and passive flow 

rate controls (e.g., flow control orifices). The manufacturer’s procedures for flow rate calibration 

should be followed. 

Calibration Frequency—See Table 16-1 for a summary of calibration frequencies.

Documentation

16. 3 Calibration and Verification of Laboratory Instrumentation

—All verifications and calibrations, as well as sampler and calibration equipment 

maintenance, will be documented in field data records and notebooks and annotated with the 

flags required in Appendix L of 40 Code of Federal Regulations (CFR) Part 50, the 

manufacturer’s operating instruction manual, and any others indicated in the field and laboratory 

SOPs (refer to Appendices of this Quality Assurance Project Plan for SOPs). The records will 

normally be controlled by the CSN site operators, and they will be located in the field offices or 

field collection sites when in use. Eventually, all calibration records will be appropriately filed 

(see Section 9.0). 

Calibration and verification of laboratory analytical equipment will follow the procedures given 

in Quality Assurance Project Plan: Chemical Speciation of PM2.5 Filter Samples, prepared by 

the CSN contracted support laboratory. 
PM2.5 CSN QAPP

Section No. 16

Revision No.: 1.2.0

Date: 10/11

Page 4 of 6

Table 16-1. Acceptance Criteria and Calibration and Maintenance Frequencies for 

PM2.5 Chemical Speciation Samplers

Criteria

Acceptance

Criterion or 

advisory limits Frequency SOP Comments

Field Calibrations and Routine Checks (by Operator or Site Supervisor)

One-point flow rate 

check at design flow 

rate 

±5% of transfer 

standard; and ±5% 

of design flow rate

Monthly Same as for gravimetric 

samplers. Applies to all flow 

channels.

External leak 

check(a)

MetOne : ≤ 0.1 

L/min

URG < 0.55 L/min

Both signal 

pass/fail;

Conducted with 

monthly flow check

Same as for gravimetric 

samplers. Applies to all flow 

channels.

Internal leak check MetOne : ≤ 0.1 

L/min

URG < 0.55 L/min

Both signal 

pass/fail;

If external leak 

check fails

Refer to 

MFGR’s 

operating 

manual

Same as for gravimetric 

samplers. Performed as a 

troubleshooting procedure 

only. May not be applicable 

to all sampler designs.

One-point 

temperature check

±2 °C of standard Monthly Same as for gravimetric 

samplers. Applies to all 

temperature sensors.

Pressure verification ±10 mmHg Monthly Same as for gravimetric 

samplers.

Clock/timer 

verification

1 min/mo Monthly Same as for gravimetric 

samplers.

Other calibrations as 

specified by 

manufacturer

per manufacturer’s 

SOP

Per manufacturer’s 

SOP

Quarterly Checks and Audits (by Auditor or person 2 mgmt. tiers from operator, using different equipment)

External leak 

check(a)

MetOne : ≤ 0.1 

L/min

URG < 0.55 L/min

Both signal 

pass/fail;

Semi-annual unless 

failed audit then at 

least quarterly until 

passes for 2 quarters

Same as for gravimetric 

samplers. Applies to all flow 

channels.

Internal leak check MetOne : ≤ 0.1 

L/min

URG < 0.55 L/min

Both signal 

pass/fail;

If external leak 

check fails

Refer to 

MFGR’s 

operating 

manual

Same as for gravimetric 

samplers. Performed as a 

troubleshooting procedure 

only. May not be applicable 

to all sampler designs.

Temperature audit ±2 °C Semi-annual unless 

failed audit then at 

least quarterly until 

passes for 2 quarters

Same as for gravimetric 

samplers.
PM2.5 CSN QAPP

Section No. 16

Revision No.: 1.2.0

Date: 10/11

Page 5 of 6

Criteria

Acceptance

Criterion or 

advisory limits Frequency SOP Comments

Pressure audit ±10 mmHg Semi-annual unless 

failed audit then at 

least quarterly until 

passes for 2 quarters

Same as for gravimetric 

samplers.

Flow rate audit ±5% of audit 

standard 

±5% of design flow 

rate

Semi-annual unless 

failed audit then at 

least quarterly until 

passes for 2 quarters

Same as for gravimetric 

samplers. Applies to all flow 

channels.

Initial Installation Calibration and recalibrations thereafter

Temperature 

calibration

±2°C of standard On installation, 

annually, or if 

verification/audit 

indicates drift or 

failure

Applies to ambient 

temperature and all internal 

filter temperature sensors.

Pressure calibration ±10 mmHg On installation, then 

annually, or if 

verification/audit 

indicates drift or 

failure

Same as for gravimetric 

samplers.

Multipoint flow rate 

calibration; URG 

only; MetOne 

utilizes single point

±2% of transfer 

standard at each 

flow rate

On installation, 

annual , or if 

verification/audit 

indicates drift or 

failure

Applies to all flow channels 

individually.

Design flow rate 

adjustment

±2% of design flow 

rate

As needed Applies to all flow channels 

individually.

Sampler Maintenance

Inlet/downtube 

cleaning

cleaned Lesser of every 15 

sampling events or 

every quarter 

Same as for gravimetric 

samplers.

Filter chamber 

cleaning

cleaned Monthly If applicable to sampler 

design.

Cyclone and 

manifold cleaning

cleaned Approximately 

every 30 use days

Consult operator’s manual

Pump box air supply 

fan filter cleaning

cleaned/changed if 

present

Monthly

Manufacturerrecommended 

maintenance

per manufacturer’s 

SOP

Per manufacturer’s 

SOP

Recertification of Standards (audit and calibration)*

Flow rate transfer 

standard

±2% of NISTtraceable standardAnnually Same as for gravimetric

samplers.
PM2.5 CSN QAPP

Section No. 16

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Date: 10/11

Page 6 of 6

Criteria

Acceptance

Criterion or 

advisory limits Frequency SOP Comments

Field thermometer ±0.1 °C resolution, 

±0.5 °C accuracy

Annually Same as for gravimetric 

samplers.

Field barometer ±1 mmHg 

resolution, 

±5 mmHg accuracy

Annually Same as for gravimetric 

samplers.

Table 16-2. Calibration Standards for PM2.5 Chemical Speciation Samplers

Description of 

Calibration Standard

QA Objective

Acceptance

Criterionb

Listed Uncertainty

for Calibration

Standard

Manufacturer

of Calibration

Standard

Model Number

of Calibration

Standard

Digital thermometer ±0.5°C

Digital pressure gauge ±0.7%c

Flow meters ±2%

a The MetOne provides a failure message based on a leak rate of > 0.1 liters per minute. The URG 3000N has 

programmed a test based on loss of vacuum of the sealed sample train which roughly equals an infiltration rate of 

0.08 liters per minute.

b

 Acceptance criteria taken from Table 16-1 of the Quality Assurance Project Plan for the Federal PM2.5

Performance Evaluation Program (U.S. EPA, OAQPS Revision 1, December 2007. c The pressure criterion (±5 mmHg) is equivalent to ±0.7% of atmospheric pressure (760 mmHg).
PM2.5 CSN QAPP

Section No. 17

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Date: 10/11

Page 1 of 3

17.0 Inspection/Acceptance for Supplies and Consumables

17.1 Purpose

The purpose of this section is to establish and document a system for inspecting and accepting all 

supplies and consumables that may directly or indirectly affect the quality of operations at a 

PM2.5 site of the Chemical Speciation Network (CSN). The monitoring network relies on various 

supplies and consumables that are critical to its operation. This section gives details on the 

supplies and consumables, their acceptance criteria, and the required documentation for tracking 

the process. Note that the inspection and acceptance procedures for the filters, of which high 

quality and consistency of performance is inextricably tied to data quality, is covered in the 

Quality Assurance Project Plan (QAPP) for the Contract Support lab’s operations. See 

http://www.epa.gov/ttn/amtic/specguid.html. 

17.2 Critical Supplies and Consumables for Field Site Operations

This section describes the supplies needed by the field sites. The choice of field supplies and 

consumables is, in part, dictated by the choice of speciation sampler. Table 17-1 lists the major 

items of equipment needed for the CSN. The state, local and/or Tribal (SLT) office must keep an 

inventory of all supplies and the warranty period and certifications of equipment and can use 

Table 17-1 for this activity. Since participants in the CSN are also operating routine samplers for 

the mass PM2.5

The contracted support laboratory will care for and track the cassettes and filter modules used in 

servicing the sampling and analysis needs of the sites but will not carry them on its own 

inventory list. For more information, refer to the support laboratory’s QAPP and standard 

operating procedures that are available on the EPA’s AMTIC website.

 program, the calibration and check standards may be used for the CSN since they 

should meet the performance standards. 

As consumables run low or replacement purchases are required, the site operator will be 

responsible for assisting in the procurement of these items by following the policies and 

procedures of the SLT agency. The operator should purchase the same model equipment and 

spare parts and the same consumables as were initially acquired, unless told to do otherwise. 

17.3 Acceptance Criteria

Selection of major pieces of capital equipment is based on the item’s advertised specifications 

and performance in analysis of particulate matter and particulate matter extracts. Newly received 

field equipment will be inspected to ensure all parts are present and undamaged. If damage has 

occurred in shipping, the shipping agent will be notified. All new equipment for field or 

laboratory use should carry a warranty for a 6-month to 1-year period. Refurbished equipment 

should also be inspected carefully and subjected to operational tests since the warranty on such 

equipment may not be as comprehensive. 
PM2.5 CSN QAPP

Section No. 17

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Date: 10/11

Page 2 of 3

Table 17-1. Inventory List for CSN Field Equipment and Supplies

Quantity 

per Site 

Operator Equipment and Supply Description

Vendor/

Catalog No. Make/Model No.

Speciation Sampling Equipment and Supplies

1 Speciation sampler (a capital equipment item)

1 Speciation sampler operating manual

6 sets Filter cassettes or sampling modules for speciation 

sampler 

Dependent 

on sampler 

type

Denuders for acid gases. Magnesium oxide coated 

aluminum honeycomb denuders in the case of the SASS

sampler for which approximately 6 will be required.

Custody and field data form for each sample run

(supplied by contracted support laboratory)

Sample shipping containers/ice packs (supplied by

contracted support laboratory)

Max./min. thermometer (if required)

Mounting Equipment and Tools

1 Tool kit

1 Jig for separating and rejoining URG Cassettes for Flow 

Calibration/leak check cartridge

Supplied by EPA 

OAQPS

Calibration/Check Standards and Related Equipment

1 Flow rate adapter (size depends on sampler brand)

1 or more Flow transfer standard (wet or dry type)

1 Pressure transfer standard (portable barometer)

1 Digital thermometer (or thermocouple calibrator)

1 per site 

and 1 for 

Audits

URG Flow Calibration/leak check cartridge See “Operation 

Manual” Parts list

Spare Parts

O-rings, tubing, fuses, impactor oil (if applicable), 

impactor filters (if applicable), compression fittings

Filters for Audit and Calibration cassettes and cartridges Request from EPA, 

OAQPS

Cleaning and Maintenance Supplies and Equipment

Distilled water in spray bottle

Lint-free cloths and lint-free laboratory wipes

Additional warranty periods may be purchased; check equipment stated to be NIST-traceable 

that is subject to wear and tear during use (for example, temperature, pressure, and flow rate 
PM2.5 CSN QAPP

Section No. 17

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Page 3 of 3

check devices). Such equipment should be returned annually to the vendor or an appropriate 

metrology laboratory for cleaning, servicing, and recertification vs. NIST standards. 

SLT agency personnel should use procurement logs for purchases of new equipment and 

consumables. These logs should also indicate whether the items were accepted or rejected. In 

addition, the laboratory and field personnel must keep an equipment inventory form that lists 

each piece of equipment and its warranty dates. 
PM2.5 CSN QAPP

Section No. 18

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Page 1 of 2

18.0 Data Acquisition Requirements (Nondirect Measurements)

This section identifies the types of indirectly acquired data needed for implementation and 

continuation of the Chemical Speciation Network (CSN). These data are obtained from 

nonmeasurement sources and historic or concurrently acquired databases not under the direct 

control of the CSN. 

18.1 Acquisition of Nondirect Measurement Data

The CSN will produce almost all required data through its own field and laboratory operations. 

Some data, however, will come from outside the network. This section lists several such data 

sources, considers the quality of the data, and gives cautionary notes. 

18.1.1 Chemical and Physical Properties Data 

Chemical and physical properties data and values of fundamental constants are often needed in 

ambient air studies. Examples of acceptable sources for fundamental units and constants and the 

relationships between metric and U.S. or British units are: 

 National Institute of Standards and Technology (available online at www.nist.gov). 

 International Organization for Standardization (ISO) (available online at 

www.iso.ch), International Union of Pure and Applied Chemistry (IUPAC) (available 

online at www.iupac.org), American National Standards Institute (ANSI) 

(www.ansi.org), and other national and international standards organizations. 

 U.S. Environmental Protection Agency (available online at www.epa.gov) sources. 

 Current editions of handbooks on chemistry and physics such as the Handbook of 

Chemistry and Physics (CRC Press). 

18.1.2 Sampler Operation and Manufacturers’ Literature

Important information is found in the manufacturers’ literature and operating manuals. Manuals 

for the speciation samplers, the devices used to verify a sampler’s proper operation (temperature 

sensors, pressure gauges, and flow meters) and to calibrate it, data acquisition devices (laptop 

computers and the programs they contain), and all analytical instrumentation used in the 

laboratory will be available. 

18.1.3 Site Location Information 

The highest priority objective of the PM2.5 CSN data is the development of common spatial and 

seasonal/annual compilations and displays of the concentrations of fine particle constituents 

across the major urban areas of the country that can be used to determine if trends exist. 

Characterization of PM2.5 constituents in rural or regional environments (especially when data 

sets are combined with IMPROVE network data) is also possible if some sites are in transport 

and/or background locations. To select the best locations for chemical speciation sites (especially 

any new sites), the network designers rely on several external sources of information to minimize 

the collection of samples with components that are uncharacteristic of urban areas. Information 
PM2.5 CSN QAPP

Section No. 18

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Date: 11/11

Page 2 of 2

about local emissions sources will be needed, for example, to avoid locating a sampler too close 

to a particle source such as a chimney, an industrial vent, a major highway, or a dusty unpaved 

road. Information in state, local and/or Tribal agency data bases could be appropriate, but this 

information needs to be spot-checked for accuracy by visiting the proposed site and surveying 

the immediate (within a 300-m radius) area for hot spots of particulate emissions and other 

sources or air flow impediments that are not recorded on older maps or in data bases. The 

meteorological characteristics near a site should be checked by reviewing several years of data 

from the nearest NOAA or NWS site in order to assess seasonal variations. In cases where the 

site is quite far for the nearest government weather station, it may be necessary to set up and 

operate meteorological sensors for wind speed and direction to characterize the 

micrometeorology of the location. 
PM2.5 CSN QAPP

Section No. 19

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Page 1 of 17

19.0 Data Management

19.1 Overview

This section presents information on how field and analytical data for the Chemical Speciation 

Network (CSN) will be managed. It does not address any data sets obtained outside the network 

nor does it include management of data that may be given in summary and interpretive reports of 

special studies. This section addresses these common data management topics: recording, 

transformation, transmittal, reduction, validation, analysis, management, storage, and retrieval. 

The CSN sampling data will ultimately be hosted by the Air Quality System (AQS). Flow audits 

must be reported to AQS as well, and monthly flow verifications can voluntarily be submitted. 

Detailed chain of custody (COC) and quality assurance/quality control (QA/QC) data collected 

in association with the sampling data and network operations are hosted by a nonpublic data base 

accessible to only state, local and/or Tribal (SLT) monitoring agencies. The CSN Contracted 

Analytical Support Laboratory is the depot for incoming field data associated with ambient 

sampling data as well as the QA/QC data collected by the monitoring agencies for validation of 

the results. The CSN Contracted Analytical Support Laboratory’s Quality Assurance Project Plan 

(QAPP) for Chemical Speciation of PM2.5

Sample and QA/QC data for the CSN come from several sources at both the CSN Contracted 

Support Laboratory and its subcontractors, and the organizations that perform the field 

operations. The general flow of data between organizations and data systems is illustrated in 

Figure 19-1. This figure emphasizes the organizational responsibilities, data base systems, and 

major operations. The CSN Support Laboratory, shown at the top of Figure 19-1, is responsible 

for integrating data from the various analytical laboratories (mass, ions, carbon, and elements)

with the shipping/receiving and chain-of-custody information for the sample module sets 

provided to the field sampling personnel in (Monitoring Agencies) and SLT agencies. After 

 Filter Samples provides additional information about 

how the data is generated and managed. 

level 0 and level 1 validation, the data are posted monthly to a password-protected data base that 

is accessible to the Delivery Order Project Officers (DOPOs) and their respective SLT

Monitoring Agencies for completion of data validation. The contract support lab notifies the 

DOPOs who, in turn, notify each SLT Monitoring Agency of the availability of the data for

review. The SLT agencies conduct levels 2 and 3 validations and notify the contract laboratory 

that data sets are acceptable or they identify invalid data, or other issues, which must be 

addressed before the data is ready for posting on the AQS. A non-response indicates acceptance 

by estoppel. The support laboratory uploads the data to the AQS data base with appropriate flags 

as required. 

The following list describes the data management activities in more detail. In many cases, double 

entry methods are used and comparisons are made to reduce typographical errors and resolve 

near-illegible or faint handwritten information. This list is presented in chronological order: 

1. Presampling Laboratory Activities. This stage is conducted by the CSN support 

laboratory and first includes inputting information to the laboratory data base 

management system (DBMS) for weight values for the TeflonTM filters, filter lot 
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Figure 19.1 The general flow of data between organizations

Fully validated 

data to 

Contract Lab

Filter Lot 

Acceptance 

Records

Filter Preexposure 

Weights

Data Validation 

Level 0 & 1

CSN Contract 

Laboratory 

DBMS

SHAL Shipping 

Records

Chain of Custody 

Data Records

Analytical Results

Distribution to the 

MO’s to Final 

Validation

AQS Upload

MO Data

System

Final Data 

Validation 

All levels

Internal QA/QC Data

COCD Forms

Logbooks

Shipping Records

Audit Results

CA. Data, etc.

STN Laboratory

Monitoring Organization

Monthly Data 

Reports in 

hardcopy and 

electronic format

Sampler Verification

and Audit Reports

DOPO

acceptance test results, quality control (QC) information such as the background 

concentrations of analytes on blank Teflon filters, washed nylon filters, and ovenfired quartz fiber filters, as well as records of laboratory temperature and humidity 

conditions during weighing sessions. Secondly, information about express shipping 

and from the COC forms is entered so that shipments of filter-containing modules to 

and from the various SLT agencies can be tracked.

2. Field Activities. These data are initially handwritten on the COC (CAFDS) form and 

upon receipt with the filter samples, are input, using double entry, by the CSN

support laboratory to the laboratory DBMS. Items include data on operation of the 

speciation sampler (sample identification numbers, volume of air sampled, ambient 
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air temperature, sampling flags indicating nonstandard operation, and so on) as well 

as operator's notes that can be used for validating the data. All data necessary for the 

laboratory to calculate concentration values and to validate data will be entered on the 

form, which is illustrated in the sampler operation SOPs contained in appendices to 

this QAPP.

3. Postsampling Laboratory Activities

4. 

. The CSN laboratory will enter the analytical 

chemistry data for particle mass, elements, ions, and carbon species into the DBMS in 

this stage. Data from QC operations such as results of multipoint calibrations and 

linearity or span checks and analysis of duplicate samples, split samples, blanks, and 

spiked samples are also entered.

Data Verification and Validation at the CSN Laboratory.

5. 

Data verification and 

validation will be carried out at both the CSN support laboratory and at the 

Monitoring Agencies. The CSN support laboratory will base its validation on the 

original COC forms, shipping records, and analytical QA/QC information. These 

activities are explained in Section 22.0 of this QAPP. 

Data Reporting to the DOPO. The CSN laboratory will post its validated data 

monthly on a password-protected secure website which is accessible to the DOPO 

and designated personnel in each SLT agency. Data from the laboratory and field are 

combined at this stage of operations and are expressed in terms of concentration units 

such as micrograms per cubic meter (μg/m3

6. 

) of air. The electronic data set will be in 

the AQS format and is accompanied by a QC report that further describes the flagging 

of the data.

Data Validation Activities at the SLT Monitoring Agencies. The Monitoring Agencies 

will further validate the data sets at levels 2 and 3, based on its internal records, 

analytical results of collocated sampling, and additional screening tests. These 

activities are described in Section 22.0 of this QAPP. 

19.2 Data Management Activities at the CSN Contracted Support 

Laboratory

Data management activities in the CSN support laboratory are described in the QAPP for 

laboratory operations and support. The current support laboratory QAPP is available on the EPA 

AMTIC website. 

19.3 Data Management Activities at the Monitoring Agency

This section describes in more detail the data management activities and responsibilities of the 

SLT Monitoring Agencies. These data management activities should be conducted in accordance 

with the recommended practices for data management described in Section 19.4. 
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19.3.1 Shipping and Receiving Records

The first stage of data management activities at the Monitoring Agency begins with receipt of a 

sampling module set containing a partially completed COC and field data sheet form(s), which 

could be combined into one. The Monitoring Agency records whenever a set of sampling 

modules and URG cartridges is received or shipped. Recording the following information in a 

notebook kept at the Monitoring Agency’s shipping/receiving area is recommended:

Before Sampling: 

 Date that each unexposed set of sampling modules is received. 

 Site name or number and sampling date that the module set is to be used. 

 Condition of the shipping container (if the container was damaged in shipment, the 

CSN support laboratory should be notified through the DOPO). 

 Warehousing area, if the set of sampling modules is not to be picked up immediately. 

 Person to whom the set of sampling modules is released for installation at the 

monitoring site (the site operator or someone who will take the modules to the site). 

After Sampling: 

 Person bringing the exposed set of sampling modules back to the shipping area. 

 Site name or number and sampling date that the sampling module set was exposed. 

 Condition of the modules and the external shipping container. 

 Whether the ice substitute was pre-cooled as required. 

 Overnight express air bill number and destination (the CSN support laboratory's 

address should be pre-printed on air bills supplied in each module set). 

 Date and time that the cooled container package was released to the overnight express 

representative. 

 One copy of the multi-part COC form should be retained by the Monitoring Agency 

and checked to ensure that all information is complete and legible. 

These shipping and receiving records may be necessary references in case there is a discrepancy 

later in data attribution. Each Monitoring Agency should develop its own system for maintaining 

shipping and receiving records. 
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19.3.2 Custody and Field Data Form 

The COC and Field Data Sheet are shown in the sampler-specific SOPs in Appendix A and in 

Section 12.0 of this QAPP. The field operator is responsible for filling the form(s) completely 

and accurately. The handwritten notations on the form are the only source that the CSN

laboratory will have for critical information, including the following:

 Site/date that sampling actually occurred (usually preprinted on the custody and field 

data form, but the operator may indicate changes). 

 Total volume(s) sampled for each of the sampling channels. 

 Average temperature(s), flow(s), barometric pressure and other information provided 

by the PM2.5

 The CV of the sampler’s flow rate for sampling period. 

sampler during the sampling period and the maximum and minimum 

values.

 Actual sampling time. 

 Data validation flags issued by the sampler. 

 Information about any field and/or trip blanks included with the set of sampling 

modules. 

 Operator's name and free-form notes. 

The COC and Field Data Form are formatted so that there is a specific space for each item noted 

above and is customized for the different speciation samplers in the CSN program. The operator 

will repack the exposed modules and return the top copy of the COC in the cooler package. The 

operator is responsible for keeping one copy of the COC form and returning it to the designated 

person at the Monitoring Agency for filing and later use in data validation.

19.3.3 Data Management Activities During Data Validation by the Monitoring Agency

Every month the DOPOs will inform their respective SLT Monitoring Agencies that the next 

“Batch” of data sets are available for review on the password-protected website. (The Contractor 

has 45 calendar days to receive, analyze, and post data for states review on an interim passwordprotected data base.) The website is divided into a set of subdirectories, one for each CSN 

monitoring site. In addition to a detailed spreadsheet of the sampling data acquired for the period 

covering that batch, each subdirectory will contain the site’s data summary and QC report 

prepared by the CSN support laboratory. The data summary will include an electronic file of 

partially validated, AQS-formatted data that will require further validation by the Monitoring 

Agency. The CSN laboratory will have performed the following level 0 and level 1 validation on 

the delivered data: 

 Data attribution and COC verification. 

 Validation of laboratory analytical data. 

 Screening for data input/output problems. 
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Refer to Section 22 of this QAPP or the CSN support laboratory QAPP and its accompanying 

data management SOPs for a full description of the data validation procedures that are applied

and the checklist that is used. 

The QC report delivered with the data file includes the following information (if any) that the 

Monitoring Agency will need in order to complete the data validation: 

 Data records with missing or uncertain attribution or COC information (principally 

the site/date of exposure or defective/incomplete COC). 

 Data records marked questionable or invalid due to sampler data flags. 

 Data records marked questionable or invalid due to laboratory problems. 

 Data records marked as possible outliers as a result of data screens applied by the 

CSN support laboratory. 

The Monitoring Agency will use its in-house records such as monthly performance verifications 

and audits to examine data that have been flagged for attribution, sampler flags, and outliers. It is 

possible that other data, such as operator's notes, shipping/receiving records, and QA/QC 

records, can be used to validate the questioned data. There is usually little that can be done if a 

measurement is assigned an invalidation flag due to a laboratory problem. Questions about flags 

applied by the CSN support laboratory should be sent through the DOPO. 

After reviewing the CSN support laboratory's QC information, the SLT Monitoring Agency must 

perform further validation on the data set. 

The specific procedures used for data validation are described in Section 22.0 of this QAPP. 

Data management methods and means for ensuring correct inputs/outputs during data handling 

are described in Section 19.4. 

19.3.4 Reporting Data to AQS

After the data set has undergone levels 2 and 3 validation, each Monitoring Agency is 

responsible for re-reporting appropriate revisions to the CSN support laboratory before the data 

are loaded into AQS. The Monitoring Agency will have 45 days to review the data and respond 

back to the support laboratory. The DOPO should be notified when the approval of the data takes 

place or changes are reported to the CSN support laboratory. The support laboratory will have 15 

days to upload data into AQS. This process is delineated in the lab service contract “reports of 

work” provisions. 

19.4 Recommended Data Management Practices

This section describes recommended data handling practices that are applicable to the CSN

support laboratory and to the Monitoring Agencies. It is expected that all organizations 

participating in the CSN program will follow guidelines similar to those specified by EPA as 

good automated laboratory practices (GALPs).
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19.4.1 Manual Data Entry 

Manually entered data will include entries from the COC forms and chemical analyst's notes and 

calculated concentrations for certain analyses. Hand-recorded data must necessarily also be 

manually entered. The following techniques apply to manual data entry: 

 100 Percent Data Verification on Input



—Manually entered data will be reviewed, 

preferably by a different operator, before it is committed to the data base. Analytical 

data, however, may be entered and proofed by the analyst who is responsible for 

generating the data. Large amounts of data entered in bulk, such as a group of COC

and field data forms entered by a data clerk, will be verified by duplicate entry in 

which two clerks enter the same data. The two sets of inputs are then compared and 

discrepancies are resolved. 

Range Checking

19.4.2 Electronic Data Entry

—Many parameters lend themselves to checking for reasonable 

range during or after data input. Properties of data sets, such as minimum and 

maximum values, median and average values are easily calculated by spreadsheet 

programs. This type of checking is frequently very useful for manual entry into screen 

forms to catch misplaced decimal points, incorrect units, and omitted or extra digits.

Current procedures include manual recording of meta data and parametric sampling data 

associated with each sampling event by the operator. The lab service contractor enters these data 

into the data base which relates it by monitoring site ID and filter number. The data entry 

personnel are trained to perform the levels 0 and 1 validation steps as the data are entered. It is a 

convenient time and at a point where anomalies can be easily recognized. Queries can be made 

prior to further filter handling and analyses. These data are then made available to the 

Monitoring Agency for its use in performing levels 2 and 3 validations. 

Migration to full electronic data transfer is possible. A full set of parametric sampling event 

information is retained in the memory of the speciation sampler. It can be retrieved by use of a 

download program and a laptop computer or portable data transfer device connected to the 

sampler’s RS232 port. (Sampler upgrades in the future will likely include use of flash drives or 

other portable storage devices; USB ports have replaced serial ports on all current day 

computers. They can usually be connected to serial ports with a transition cable and some 

software.) The data may be stored on a portable data storage device which can be shipped with 

the filter canisters and cartridges to the lab service contractor, but the ability to integrate the 

more thorough level 0 and level 1 validation is lost. The lab service contractor will extract 

parametric data associated with the sampling event and post it with the sampling results (see 

below). A copy of the data will be retained by the site operator. No further checking of data 

integrity will be done for electronic file transfers because these are internally validated by the 

transmission medium. 
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Although migration to full electronic data transfer is possible, the ability to integrate the more 

thorough level 0 and level 1 validation by a human is lost. Furthermore, any information entered 

by the site operator (AQS code, filter numbers, etc.) still has to be added to the data base. 

The laboratory services contractor posts data sets of analytical results and sampling field and 

meta data to a restricted website data base which is password-accessible to the SLT Monitoring 

Agencies. Each data set will be subjected to a level 2 and level 3 validation by its Monitoring 

Agency before the data set is approved for uploading to AQS. 

19.4.3 Sample and Data Tracking 

Within the CSN support laboratory, a laboratory information management system (LIMS) tracks 

the cycle of activity for any filter for any sampling date and provide the history and present 

status of each sample. Analytical samples will be internally tracked using a batch-oriented 

internal COC form. Module sets sent from the CSN support laboratory to the Monitoring 

Agencies are tracked in the laboratory's data base system. These processes are described further 

in the CSN support laboratory’s QAPP and the data management SOP. 

Each Monitoring Agency must also develop methods for tracking, shipping, and receiving data 

and for filing custody and field data forms, audit reports, and other CSN-related paperwork. 

These records may be hardcopy or electronic, at the organization's discretion. Adoption of 

procedures similar to those already in use for other programs such as the National PM2.5

19.4.4 Data Recording, Security, and Archiving 

Monitoring Network is encouraged. File, data records, and document retention is covered in 

Section 9.0 of this QAPP. 

SLT Monitoring Agencies and the CSN contracted support laboratory should address data 

security in their data management processes for CSN and other reportable environmental data. 

The processes sand practices should be recorded in the organization’s QAPP for participating in 

the CSN. It will include, but not be limited to, practices such as the following (or equivalent): 

 Organizations must perform regular backups of the CSN data base pertaining to their 

monitoring site(s). 

 As insurance against fires and other problems affecting an entire building, data 

backup sets should be kept off-site.

 Weekly full backups of the data base, with nightly incremental backups of changed 

information, are recommended (at a minimum). 

 Use of passwords should be required and enforced. Passwords should be issued to 

each individual user of the data system that contains the CSN data. 

 Access to computers or networks containing unreleased CSN data should be 

password-restricted, if possible, to authorized users. 

 Access to unreleased CSN data should be restricted to personnel working on the CSN

program. 
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Archival of raw data and other program information is important because it allows the processing 

and validation of questioned data items to be reconstructed in the event of challenge or for 

research purposes. Table 19-1 summarizes the data and records that must be retained by the CSN 

contracted support laboratory or Monitoring Agency for the life of the contract or for the term

required by contractual agreement, (often 5 years). The Location or Responsibility column of 

Table 19-1 describes a typical location where such information is often stored; however, it may 

be preferable to store some information in a more centralized location. Laboratory data records 

should be stored in a secure location with limited personnel access and with protection against 

fire and natural disasters or with suitable backup copies stored separately. 

19.5 Data Validation

19.5.1 Validation Checks and Procedures

Data validation is a combination of checking that data processing operations have been carried 

out properly and of monitoring the quality of field and laboratory operations. If a problem is 

identified, the data can be corrected or invalidated, and corrective actions can be taken to prevent 

its recurrence. The following considerations relative to data management practices during data 

validation will apply:

 Flags denoting error conditions or QA status will be associated with each observation 

down to the level of individual analyses, but flags must never overwrite the data 

values so that recovery and review of the original data will be possible. However, if a 

value is deemed invalid, based upon associated flags and other evaluations, a null 

data code will be substituted for the original value during entry to AQS. 
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Table 19-1. Suggested Support Laboratory Data Record Archival Summary 

Type of Record

Laboratory

MONITORING 

AGENCY

Data Archival Location or Responsibility

Completed chain of custody/field data forms T T Lab: sample handling and archival

laboratory; MONITORING AGENCY: CSN

Manager's files

Shipping records T T Shipping department files

Internal custody forms T Lab: sample handling and archival laboratory

Analytical and weighing raw data and instrument 

traces

T Analytical laboratories and gravimetric 

laboratory files

Analytical and weighing control charts T Laboratory files

Weighing room environmental records T Weighing laboratory files

Certificates for all equipment and materials 

standards (e.g., NIST or manufacturer's certificate)

T T Laboratory or QA Officer's files

Instrument calibration and QC records T T Laboratory or QA Officer's files

Instrument maintenance and service records T T Laboratory or field organization's files

Audit trails generated during data validation T T Data processing department's and/or QA 

Manager’s files

QA records, including audit checklists and audit 

reports

T T QA files

Copies or files of all partially validated data sets 

sent from the CSN support laboratory to the DOPO

T CSN support laboratory Program Manager's 

files

Copies or files of all fully validated data sets sent 

from the Monitoring Agencies to the support 

laboratory for transfer to AQS

T MONITORING AGENCY’s CSN Manager's 

files

Purchasing records related to the CSN program T CSN support laboratory Program Manager's 

files

Correspondence with the DOPO, including 

consolidated sample requests

T T MONITORING AGENCY: CSN Manager's 

files

Support Lab: Program Manager's files

Correspondence and business records with 

subcontractors involved with the CSN

T Support laboratory Program Manager's files

Training records T T Program Manger's files

Levels 2 & 3 Data validation must include 100 percent manual review of both flagged and 

unflagged data. A summary of various data to be validated and suggested methods are given in 

Table 19-2. A qualified reviewer, such as a qualified analyst or the QA Officer, should also 

examine randomly selected data transfer operations, according to Table 19-3 for reasonableness 

before it is reported out of the organization. Completeness checks of the data set must be 

included in the validation system. These checks are often automated screening programs, 
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particularly for within-record checks. The Monitoring Agency should verify the completeness of 

the data set created by the CSN support laboratory by checking that all exposures have been 

accounted for by comparison with its COC and field data forms and other records. An audit trail 

is strongly recommended to document all changes made to the data set during validation 

operations. Audit trails are described later in this section.

Table 19-2. Validation Check Summaries

Type of Data Check

Electronic 

Transmission and 

Storage Manual Checks

Automated 

Checks

Data parity and transmission protocol checks 

Data review  

Date and time consistency  

Completeness of required fields  

Range checking 

Statistical outlier checking 

Manual inspection of charts and reports 

Sample batch data validation 

Refer to Sections 22.0 and 23.0 of this QAPP for specific data validation procedures to be 

applied. Validation procedures applicable to the CSN laboratory are described in the contracted 

support laboratory’s QAPP.

Table 19-3. Data Transfer Operations

Description of Data 

Transfer Originator Recipient QA Measures Applied

Keying weighing data and 

chemical analysis results 

into the CSN laboratory's 

data base

Laboratory analyst 

(handwritten data forms)

Laboratory analyst (enters 

data into the data base 

using screen forms)

100 percent review; 

random checks by the QA 

Manager or staff

Electronic data transfers Between computers or 

over networks

-- Parity checking; 

transmission protocols; 

test messages

Filter receipt, custody and 

field data forms

Site operator Laboratory data clerk Filter numbers are 

verified; data checked for 

completeness and 

accuracy; duplicate key 

entry for custody and field 

data forms

Verifications/calibrations and audit date
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Description of Data 

Transfer Originator Recipient QA Measures Applied

 Field site sampler Field site operator or

Field auditor

Results that are outside of 

advisory or acceptance 

limits are reported to 

personnel responsible for 

remediation and 

maintenance.

Reports are transferred to 

support contractor who 

posts data to AQS and in 

QA data facility.

Values are reported to the 

SLT data reviewers who 

have the final decision on 

accepting or invalidating 

monitoring data

Critical Field data entries 

are checked by field 

operator. SLT QA person 

reviews performance 

verification and audit 

results prior to reporting 

to the support contractor 

for loading into AQS. 

 Laboratory 

instruments

Laboratory auditor; 

Laboratory analysts 

Laboratory data clerk

Results that are outside of 

advisory or acceptance 

limits are reported to 

personnel responsible for 

remediation and 

maintenance.

QC Check values are 

reported to the SLT data 

reviewers who have the 

final decision on 

accepting or invalidating 

monitoring data

Laboratory data checked 

by laboratory supervisor 

and spot-checked by QA 

staff

AQS data summaries Laboratory data clerk and 

data supervisor

AQS (EPA) (via the 

DOPO)

Entries checked by 

laboratory data clerk and 

data supervisor; OAQPS 

QA Officer

Finalized AQS data 

summaries

CSN laboratory AQS Checked by the 

laboratory’s Program 

Manager or QA Officer

19.5.2 Data Flagging

As a result of data validation, individual items will be marked by a variety of validation flags that 

generally indicate that the item is suspicious or invalid. Invalid data should not be reported to 

AQS. The CSN support laboratory data base may contain a superset of the AQS flags for internal 

use to facilitate QC reporting; however, these flags will be mapped onto the set of approved AQS

flags before they are released from the support laboratory. A summary of AQS data flags is 

given in Table 19-4.
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Table 19-4. Summary of AQS Data Flags for PM2.5

FLAG RTI_DESCRIPTION AQS_VALIDITY

_CODE

AQS_NULL_V

ALUE_CODE

AQS_DESCRIPTION

1

2

3

4

5

6

AAR

AB

AC

AD

AE

AF

AG

AH

AI

AJ

AK

AL

AM

AN

AO

AP

AQ

AR

AS

Critical Criteria Not Met

Operational criteria not met

Possible field contamination

Possible lab contamination

Outlier - cause unknown

Data prior to QAPP approval

Above Analytical Range

Technician Unavailable

Construction/Repairs In Area

Shelter Storm Damage

Shelter Temperature Outside Limits

Scheduled But Not Collected

Sample Time Out Of Limits

Sample Flow Rate Out Of Limits

Insufficient Data (Can't Calculate)

Filter Damage

Filter Leak

Voided By Operator

Miscellaneous Void

Machine Malfunction

Bad Weather

Vandalism

Collection Error

Lab Error

Poor Quality Assurance Results

1

2

3

4

5

6

AM

AB

AC

AD

AE

AF

AG

AH

AI

AJ

AK

AL

AM

AN

AO

AP

AQ

AR

AS

CFR/Critical Criteria Deviation

Operational Deviation

Field Issue

Lab Issue

Outlier

QAPP Issue

Miscellaneous Void

Technician Unavailable

Construction/Repairs In Area

Shelter Storm Damage

Shelter Temperature Outside Limits

Scheduled But Not Collected

Sample Time Out Of Limits

Sample Flow Rate Out Of Limits

Insufficient Data (Can't Calculate)

Filter Damage

Filter Leak

Voided By Operator

Miscellaneous Void

Machine Malfunction

Bad Weather

Vandalism

Collection Error

Lab Error

Poor Quality Assurance Results
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FLAG RTI_DESCRIPTION AQS_VALIDITY

_CODE

AQS_NULL_V

ALUE_CODE

AQS_DESCRIPTION

AU

AV

AW

AZ

BA

BB

BE

BI

BJ

DCI

DMA

DSI

FBS

FMC

FNA

FSB

FSL

IA

IB

IC

ID

IE

IF

IG

IH

II

IJ

Monitoring Waived

Power Failure (Powr)

Wildlife Damage

Q C Audit (Audt)

Maintenance/Routine Repairs

Unable To Reach Site

Building/Site Repair

Lost Or Damaged In Transit

Operator Error

Channel Invalid

Module assembled in correctly

Shipment Invalid

Field or Trip Blank appears to be actual sample

Moisture contamination

Field operator designates no analysis

Sample is blank

Sample lost

African Dust

Asian Dust

Chem. Spills and Industrial Accidents

Cleanup After a Major Disaster

Demolition

Fire - Canadian

Fire - Mexico/Central America

Fireworks

High Pollen Count

High Winds

3

IA

IB

IC

ID

IE

IF

IG

IH

II

IJ

AU

AV

AW

AZ

BA

BB

BE

BI

BJ

AQ

AR

BI

AQ

AL

AQ

BI

Monitoring Waived

Power Failure (Powr)

Wildlife Damage

Q C Audit (Audt)

Maintenance/Routine Repairs

Unable To Reach Site

Building/Site Repair

Lost Or Damaged In Transit

Operator Error

Collection Error

Lab Error

Lost Or Damaged In Transit

Collection Error

Field Issue

Voided By Operator

Collection Error

Lost Or Damaged In Transit

African Dust

Asian Dust

Chem. Spills and Industrial Accidents

Cleanup After a Major Disaster

Demolition

Fire - Canadian

Fire - Mexico/Central America

Fireworks

High Pollen Count

High Winds
PM2.5 CSN QAPP

Section No. 19

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FLAG RTI_DESCRIPTION AQS_VALIDITY

_CODE

AQS_NULL_V

ALUE_CODE

AQS_DESCRIPTION

IK

IL

IM

IN

IO

IP

IQ

IR

IS

IT

IU

LFH

LFT

LHT

QAC

QCR

QL1

QMB

SA

T

V

W

X

Y

Infrequent Large Gatherings

Other

Prescribed Fire

Seismic Activity

Stratospheric Ozone Intrusion

Structural Fire

Terrorist Act

Unique Traffic Disruption

Volcanic Eruptions

Wildfire-U. S.

Wildland Fire Use Fire-U. S.

Filter inspection flags* - Holes in filter

Filter inspection flags* - Tear

Lab holding times exceeded

Cation/Anion total charge ratio out of limits

Between-analyte correlations

Outlier detected by QAO based on Level 1 check

Total mass balance outside limits

Storm Approaching

Multiple Flags; Misc.

Validated Value

Flow Rate Average Out Of Spec.

Filter Temperature Difference Out Of Spec.

Elapsed Sample Time Out Of Spec.

IK

IL

IM

IN

IO

IP

IQ

IR

IS

IT

IU

2

5

5

5

5

T

V

W

X

Y

AJ

AJ

SA

Infrequent Large Gatherings

Other

Prescribed Fire

Seismic Activity

Stratospheric Ozone Intrusion

Structural Fire

Terrorist Act

Unique Traffic Disruption

Volcanic Eruptions

Wildfire-U. S.

Wildland Fire Use Fire-U. S.

Filter Damage

Filter Damage

Operational Deviation

Outlier

Outlier

Outlier

Outlier

Storm Approaching

Multiple Flags; Misc.

Validated Value

Flow Rate Average Out Of Spec.

Filter Temperature Difference Out Of Spec.

Elapsed Sample Time Out Of Spec.
PM2.5 CSN QAPP

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19.5.3 Audit Trails

The audit trail is an important means for documenting changes to a data set made during 

validation. The audit trail is important for establishing the reason for data changes, the authority 

under which the change was made, and the data values before and after the change was applied. 

Organizations are strongly urged to implement audit trails for the CSN program. Typical reasons 

for making audit trail entries include the following:

 Corrections of data input due to human error. 

 Application of revised calibration factors to sample results from an analytical run 

queue. 

 Addition of new or supplementary data. 

 Flagging of data that are invalid or suspect based on manual examination or 

automated validation of the data. 

 Logging of the date and time when automated data validation programs are run. 

Audit trail records usually include the following fields: 

 Operator’s identify (identification code). 

 Date and time of the change. 

 Table and field names for the changed datum. 

 Complete identifying information for the item changed (date, time, and so on). 

 Value of the item before and after the change (or image of the entire record before 

and after the change).

19.6 Data Transformations

Calculations for transforming analytical data in units of mass per filter or mass per volume of

extraction solution to concentration units are relatively straightforward. Table 19-5 summarizes 

transformations applied to analytical data to produce volume, mass, and concentration data. 

Information about measurement uncertainties and method detection limits (MDLs) often 

accompany summaries of such data.

Table 19-5. Raw Data Calculations 

Parameter Units Conversion type Equation

Volume of air 

sampled through 

filter

m Calculated from average flow rate (Q 3 avg) in L/min and 

total elapsed sampling time, 10 minutes, multiplied by 

the unit conversion (m3

V

/L)

a = Qavg × t × 10-3

Total mass on filter 

(PM2.5

μg

) 

Calculated from filter postsampling weight (Mf) and 

filter presampling weight (Mi

PM

) in mg, multiplied by the 

unit conversion (1000 μg/mg)

2.5 = (Mf - Mi) × 103
PM2.5 CSN QAPP

Section No. 19

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PM2.5 concentration 

(CPM2.5

μg/m

)

Calculated from laboratory data and sampled air 

volume

3 CPM2.5 = PM2.5/Va

NOTE: Table 19-5 is applicable to the general categories of analytes to be produced by the 

CSN program. Calculations within these categories are similar. Standard calculations such as 

unit conversions and equations for calculating standard statistics are not provided. Calculations 

involved in instrument calibrations are described in the respective SOPs and operating manuals 

for the PM2.5

19.7 Data Reduction

 speciation sampler. 

Data reduction is the process of aggregating and summarizing results so they can be understood 

and interpreted. For the activities covered, if data reduction is performed primarily to assess the 

quality or uncertainty of the ambient concentration data. 

 Average PM2.5

 Bias and precision statistics based on accumulated FRM and speciated PM

mass or species concentration for comparison against averages of the 

same parameters over previous time periods to determine the reasonableness of 

results.

2.5 

 Data completeness reports based on the number of valid samples collected and 

analyzed during a defined period of time versus the expected number of samples. 

data and 

sampler flow rate statistics. 

19.8 Data Analysis

For the activities covered by this QAPP, data analysis techniques and products will be limited to 

those designed to assess the quality or uncertainty of the ambient concentration data. Tools to 

ascertain the air quality trends or make air quality assessments are beyond the scope of the CSN

QAPP. Feedback from data analysts is necessary, however, to determine if the data quality 

objectives have been met in allowing an interpretation of the data at the confidence level that was 

originally projected. This will be covered in Section 24. 

19.9 Data Storage and Retrieval

The CSN’s contracted support laboratory’s data storage and retrieval techniques with respect to 

the recorded sampling and analytical data are described in the laboratory QAPP and SOPs. 

Data storage and retrieval techniques for the Monitoring Agencies should be described in their 

system documentation or through in-house SOPs developed for the CSN program. 

Documentation of data storage and retrieval should include a summary of the type of data, the 

media on which they are stored, security measures for safeguarding the data against destruction 

and access by unauthorized persons, and the retention time for the data. 
PM2.5 CSN QAPP

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20.0 Assessment and Response Actions

20.1 Types of Assessments

The following types of assessments will be performed within the Chemical Speciation Network 

(CSN): 

 Management systems reviews (MSRs). 

 Network reviews. 

 Technical systems audits (TSAs). 

 Performance evaluations (PEs). 

 Audits of data quality (ADQs). 

 Data quality assessments (DQAs). 

MSRs are described in Guidance for Preparing, Conducting, and Reporting the Results of 

Management Systems Reviews (U.S. Environmental Protection Agency Publication No. EPA 

QA/G-3). TSAs, PEs, and ADQs are described in Guidance on Technical Audits and Related 

Assessments for Environmental Data Operations (EPA Publication No. EPA QA/G-7). DQAs 

are described in Guidance for Data Quality Assessment (EPA Publication No. EPA QA/G-9). 

Information in these documents follows the specifications and guidance given in the American 

Society for Quality Publication ANSI/ASQC E4-1994. The EPA’s Office of Environmental 

Information (OEI) periodically reviews and revises these documents. The current versions or 

their equivalent documents are accessible through OEI’s webpages at 

http://www.epa.gov/quality/index.html. 

20.2 Assessment Frequency

Assessments will be performed at the frequency described in Table 20-1. 
PM2.5 CSN QAPP

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Table 20-1. Assessment Summary

Assessing Agency Type of Assessment Entity Assessed Frequency

A. Laboratory and Network Operations

OAQPS/NAREL TSA, MSRs and

PEs of laboratory operations

Contracted support laboratories and 

Laboratories of participating 

Monitoring agencies

PE’sAnnually

TSA/MSRs Every 

3 years

OAQPS 

(w/contractor 

support)

DQAs All data and QA Data DQA’s Annually

Regional Offices MSRs State and Local agencies, Once every 3 

years

Regional Offices w 

Monitoring 

Agencies

Network Reviews State and local agencies Once every 5 

years

B. Field Operations

State, Local, or 

Tribal Monitoring 

Agencies†

TSAs of field operations Monitoring sites Annually*

State, Local, or 

Tribal Agencies

Performance Audits of field 

operations Every Sampler Semi-annual* 

†EPA Regional Offices during their 3-year MSR, or OAQPS on an ad hoc basis as needed, will conduct federal 

level TSAs

* If a sampler fails an audit, or 2 monthly performance verifications, the audit frequency should be increased to 

quarterly until the sampler performs satisfactorily in 2 consecutive audits. 

20.3 Acceptance Criteria

The acceptance criteria for assessments were originally based on the data quality objectives 

(DQOs) and measurement quality objectives (MQOs) established for the network (Section 7.0). 

Historical performance has provided a basis to make a few adjustments. Further adjustments

could result from performance assessments and data results compiled over specified time 

periods, e.g., annual, 3 years or 5 years. Table 11-2 in Section 11.0 and Table 14-2 summarize

the acceptance limits (and some advisory limits) for field operation of the speciation samplers. If 

monitoring organizations recognize significant performance issues or changes in data 

characteristics that in turn changes their disposition toward an MQO or DQO, they should 

present the issue to their EPA Regional CSN contact and the Office of Air Quality Planning and 

Standards (OAQPS). 

Methods for and results of assessments of CSN field operations can be found on the Ambient 

Monitoring Technical Information Center (AMTIC) website 

(http://www.epa.gov/ttn/amtic/specguid.html). Documents at this site include “IMPROVE 

Technical Systems and Field Audit Procedures,” “MetOne SASS and URG Technical Systems 

and Field Audit Procedures,” as well as Technical Systems Audit Questionnaires. 
PM2.5 CSN QAPP

Section No. 20

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The assessment of acceptability of CSN and IMPROVE laboratory operations is conducted by 

the EPA personnel of the National Air and Radiation Environmental Laboratory (NAREL), 

Montgomery, Alabama. Examples of laboratory assessments (both systems and performance 

evaluations) are available at the EPA AMTIC website under the title “PM2.5 

20.4 Assessment Personnel

Speciation Lab 

Audit Reports and Assessments” (http://www.epa.gov/ttn/amtic/pmspec.html).

Assessors should have a minimum of 4 years of full-time appropriate and practical experience 

(not including training) in air quality monitoring, including at least 2 years in quality assurance 

activities.

Lead assessors should have technical experience with the samplers as well as assessment and 

quality system experience. Other assessment team members also may have such experience, or 

they may have only technical experience and currently be receiving assessment and QA training. 

Lead assessors should have knowledge and understanding of the applicable environmental 

statutes and regulations. They should be familiar with the EPA management systems and with 

the organizational and operating procedures for environmental data collection. Lead assessors 

should have a working knowledge of the technical assessment techniques for examining, 

questioning, evaluating, and reporting environmental data operations and for following up on 

response actions. They need to understand the assessment planning process. They also need 

technical understanding of the PM2.5 CSN. In general, they need to be able to evaluate the PM2.5

CSN's scope of work, its management system structure, and its operating procedures and to 

judge the PM2.5

Assessment team members should be familiar with technical assessment concepts and techniques 

and with the structure and operating procedures for environmental data collection. They should 

have technical knowledge of the PM

CSN's adequacy compared to this Quality Assurance Project Plan (QAPP). 

2.5

Technical specialists, who have specialized knowledge of PM

CSN. Depending on the scope of the technical 

assessment, assessors may need to meet additional qualifications, including health and safety 

requirements.

2.5 CSN and basic knowledge of 

assessment techniques and procedures, may participate in assessments. They may need basic 

training in assessment techniques and procedures. Under the direct supervision of the lead 

assessor, they may help prepare the technical portions of assessment checklists and may conduct 

the technical portions of an assessment. They can verify findings and observations that are made 

by other assessment team members concerning any specialized technical aspects of the PM2.5

CSN. 
PM2.5 CSN QAPP

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Three general standards for assessors are as follows:

 The assessors assigned to conduct a specific assessment should collectively possess 

adequate professional proficiency for the tasks required. This standard places 

responsibility on the assessors’ organization to ensure that the assessment is 

conducted by assessors who collectively have the technical knowledge and 

assessment skills necessary for the assessment. This standard applies to the assessors 

as a group, not necessarily to every individual assessor. Assessors should have 

specific training regarding the procedures and reporting requirements for field and 

laboratory assessments. The EPA OAQPS provides a comprehensive training course 

for CSN and IMPROVE network auditors (assessors). Monitoring Agencies should 

enroll their assessors in this training course at least once and conduct periodic 

refreshers or evaluations of the assessors. IMPROVE Auditors will be required to 

attend an initial certification course and participate in an annual reevaluation 

conducted by the EPA.

 The assessors should be organizationally independent from the operations being 

assessed, and able to maintain an independent attitude and appearance. This standard 

places responsibility on the assessors' organization and on individual assessors to 

maintain independence so that assessment findings will be both objective and viewed 

as objective by knowledgeable third parties. See 40 CFR part 58, appendix A, section 

2.2. 

 The assessors should use due professional care in conducting the assessment and in 

preparing related reports. This standard places responsibility on the assessors' 

organization and on individual assessors to follow all applicable standards in 

conducting assessments. Assessors should use sound professional judgment in 

determining and interpreting the standards that are to be applied to the assessment. 

The authority and independence of assessors, and the limits on their authority, must be clearly 

defined in the organization's quality documents. Assessment personnel should have sufficient 

authority, access to programs and managers, and organizational freedom to: 

 Identify and document problems that affect quality;

 Identify and cite noteworthy practices that may be shared with others to improve the 

quality of their operations and products; 

 Propose recommendations (if requested) for resolving problems that affect quality; 

 Independently confirm implementation and effectiveness of solutions; and 

 When problems are identified, provide documented assurance (if requested) to line 

management that further work performed will be monitored carefully until the 

deficiencies are suitably resolved.

Prior to an assessment, it is important to establish whether the assessors have the authority to 

stop or suspend work if they observe conditions that present a clear danger to personnel health or 
PM2.5 CSN QAPP

Section No. 20

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safety or that adversely affect data quality. If not, assessors need to know what communication 

they may be required to have with the authorized official who can stop work. Safety is 

paramount; no assessments will be made in any unsafe conditions. 

20.5 Assessment Reports

The product of an assessment is a written report. The objective of the report is to communicate 

assessment findings to the proper levels of management in the EPA and the assessed 

organization. The report must include: 

 Assessment/review title and number and any other identifying information; 

 The lead assessor, assessment team members, and the management and key personnel 

of the assessed organization;

 Background information about the PM2.5

 Summary and conclusions of the assessment and proposed response actions; and 

CSN activity being assessed, the purpose 

and date(s) of the assessment, the particular parameter evaluated, and a brief 

description of the assessment process; 

 Attachments and appendices that include all evaluation and finding information. 

Typically, two reports are produced: the draft findings report and the quality assurance final 

report. The lead assessor is responsible for producing the draft findings report and should 

organize the work to get the report written during the audit debriefing that should occur at the 

end of the audit. In this case, the draft findings report might simply be a listing of the positive 

findings as well as the findings that call for some corrective action. The EPA has developed an 

Excel workbook template that documents a full TSA, a sampler audit (and a set of performance 

verification checks). It is designed to expedite the reporting process and ultimately enable the 

results and findings to be posted in a password-protected data base. These Excel Workbooks are 

available to Monitoring Agency and EPA assessors. A full draft findings report for a should be 

written within 15 working days following the assessment. Each Monitoring Agency will have 

specific procedures for reporting results to the appropriate lines of management and remediation 

contacts as appropriate. Examples of PM2.5

The assessed organization should be given the maximum opportunity to respond to the draft 

findings report. This response should address the findings and discuss how any response actions 

will be resolved. If the assessed organization disagrees with the findings, the response can 

contain a rebuttal. Upon receipt of this response, the lead assessor should determine if the 

response adequately addresses the findings or, if a follow-up assessment is required, when it is 

appropriate to close out the assessment.

 speciation network assessment questionnaires and 

reports for field and laboratory reviews are available on the EPA AMTIC website at 

http://www.epa.gov/ttn/amtic/specguid.html and http://www.epa.gov/ttn/amtic/pmspec.html, 

respectively.

After the assessed organization's comments have been addressed, the final assessment report

should be prepared. The final assessment report should be similar in format to the draft findings 
PM2.5 CSN QAPP

Section No. 20

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report and should be based on the draft findings report. Typically, the assessed organization's 

response will be integrated into the summary of findings and response actions sections. The lead 

assessor is responsible for correcting any findings that are demonstrated to be incorrect by 

objective evidence to the contrary supplied by the assessed organization. Opinions of the 

assessed organization that differ from those of the assessors are not valid reasons to alter the 

report. The final assessment report should be uploaded to the Contract Support Lab’s quality 

assurance (QA) website. Flow audit results are extracted by the Contract Support Lab and posted 

to Air Quality System (AQS). The EPA Regional CSN contact will be notified of the availability 

of the assessment and if adverse findings have been unresolved. Documentation for TSAs and 

network reviews will be archived at the respective EPA Regional Offices or Monitoring 

Agencies for at least 10 years. The results of MSRs will be on file in assessor organizations’ QA 

filing system in accordance with their filing procedures. The MSR reports should be retained at 

least 5 years. 

20.7 Implementation of Response Actions

After an assessment, any necessary response actions should be timely and effective. In certain 

cases, it may be necessary to perform response actions as quickly as possible. Such cases may 

include adverse impacts on data quality or preventing data acquisition and/or risks to personnel 

health and safety. Verbal approval for remediation from responsible parties suffices under these 

conditions. Remediation is primarily the responsibility of the state, local, and/or Tribal (SLT) 

monitoring organization. If issues exist that impede the successful remediation of the 

nonconforming sampler or operational procedures, the EPA Regional CSN contact should be 

notified and a resolution coordinated. 

Response actions encompass immediate actions to eliminate problems such as errors in 

calibrations, weighing, and other internal procedural problems and long-range response actions 

instituted to improve overall data quality. Management of the assessed organization responsible 

for the assessed activities is responsible for ensuring that effective and timely response actions 

occur. The response actions should address the following: 

 Measures to correct each nonconformance,

 Identification of all root causes for significant deficiencies,

 Determination of the existence of similar deficiencies,

 Response actions to preclude recurrence of like or similar deficiencies,

 Assignment of response action responsibility, and 

 Completion dates for each response action. 

Management of the assessed organization should implement the response actions and provide 

objective evidence to the EPA of the effectiveness of the correction. Once such objective 

evidence is received, the assessment will be closed unless a reassessment is planned. In some 

cases, the assessment team may be needed to confirm the successful implementation of response 

actions.
PM2.5 CSN QAPP

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When an assessment or series of assessments leads to a finding or better procedure that, if 

implemented, would simplify the work and/or improve the entire network’s data, the finding will 

be submitted to an ad hoc workgroup composed of SLT and EPA personnel and facilitated by the 

OAQPS CSN program lead. This workgroup will develop specific procedures which will be 

implemented by a Quality Bulletin indicating a forthcoming change to a standard operating 

procedure and to a section of the QAPP. Refer to Section 11.2 of this QAPP for discussion and 

an example of a Quality Bulletin.
PM2.5 CSN QAPP

Section No. 20

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Figure 20-1 Assessment Finding Response Action Form 

Assessment Finding Response Form

Assessed Site or Laboratory ______________________:___________________

Assessment Title: ____ __________ Assessment #: ______ Finding #: _______

________________________________________________________________________

Finding:

Cause of the problem:

Actions taken or planned for correction:

Responsibilities and timetable for the above actions:

Prepared by: _______________________ Date: _____________

Signed by: _________________________ Date: _____________

Speciation QA Manager

Reviewed by: _______________________ Date: _____________

Response actions and remarks:

Is this assessment finding closed? ___________ When (date) ___________

Signed by: ______________________________________________________

File with official assessment records. Send copy to assessed organization.
PM2.5 CSN QAPP

Section No. 20

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20.8 References

American Society for Quality. 1994. Specifications and Guidelines for Quality Systems for 

Environmental Data Collection and Environmental Technology Programs. ANSI/ASQC E4-

1994. Milwaukee, WI. 

American Society for Quality. 2004. Quality Systems for Environmental Data and Technology 

Programs. ANSI/ASQ E4-2004. Milwaukee, WI. 

U.S. Environmental Protection Agency. 2003. Guidance on Assessing Quality Systems. EPA 

Publication No. EPA QA/G-3, EPA/240/R-03/002. Washington, DC. 

U.S. Environmental Protection Agency. 1998a et seq. Quality Assurance Handbook for Air 

Pollution Measurement Systems, Volume II: Part 1, Ambient Air Quality Monitoring Program 

Quality System Development. EPA Publication No. EPA-454/R-98-004. Washington, DC. 

U.S. Environmental Protection Agency. 1998b. SLAMS/NAMS/PAMS Network Review 

Guidance. EPA Publication No. EPA-454/R-98-003. Washington, DC. 

U.S. Environmental Protection Agency. 2006. Data Quality Assessment: A Reviewer’s Guide. 

EPA Publication No. EPA QA/G-9R, EPA/200/B-06/002. Washington, DC. 

U.S. Environmental Protection Agency. 2006. Data Quality Assessment: Statistical Tools for 

Practitioners. EPA Publication No. EPA QA/G-9S, EPA 240/B-06/003. Washington, DC. 

U.S. Environmental Protection Agency. 2002, reissued 2006. Guidance on Technical Audits and 

Related Assessments for Environmental Data Operations. EPA Publication No. EPA QA/G-7, 

EPA/600/R-99/080. Washington, DC.

U.S. Government Accountability Office. 2007. Government Auditing Standards. Washington, 

DC.
PM2.5 CSN QAPP

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21.0 Reports to Management

This section describes the quality-related reports and communications to management necessary 

to support PM2.5 Chemical Speciation Network (CSN) operations and the associated data 

acquisition, validation, assessment, and reporting. Effective communication among all personnel 

is an integral part of a quality system. Planned reports provide a structure for apprising 

management of the project schedule, the deviations from approved quality assurance (QA) and 

test plans, the impact of these deviations on data quality, and the potential uncertainties in 

decisions based on the data. These reporting documents should spell out the frequency of such 

checks, the personnel responsible for generating the report, and recipient of the information. 

Although the CSN has not been a regulatory network, the data produced by it might be used for 

regulatory programs in the future. Furthermore, the October 17, 2006, rule revisions to the 

monitoring regulations specifically name the CSN as monitoring sites that are subject to the 

reporting requirements at 40 CFR part 58.16. Participating agencies should, therefore, follow the 

quality control documentation guidelines applicable to other monitoring operations such as PM10

and PM2.5 federal reference method (FRM) network. This is particularly convenient when the 

speciation samplers are located at NCore and compliance network sites (e.g., state and local air 

monitoring station (SLAMS)). When speciation samplers are not located at such sites, and are 

not part of the NCore network, Monitoring Agencies are urged to consult with their Regional 

EPA QA management regarding the appropriate level of documentation. 

Table 21-1 shows this information for the key reports to management documentation for the 

CSN. These documents should be considered mandatory for samplers in the NCore network and 

strongly recommended for other CSN sites. Columns in the table are as follows:

• Type of Report – name or description of report. 

• Contents – brief summary of contents. 

• Author – organization responsible for producing the report. Each organization listed as 

Author or Recipient in Table 21-1 should develop procedures and schedules for 

preparation of the referenced reports to management, and should designate specific 

individuals with the responsibility. 

• Recipient – organization responsible for review and approval of the report. 

• Frequency – suggested or required frequency of reporting. 

• Posting – location of where electronic version the report or data will be posted for public 

access. 
PM2.5 CSN QAPP

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Table 21-1. Summary of Reports to Management for the CSN 

Type of Report Contents Author Recipient Frequency Posting

21.1 Annual 

Data Summary 

Report 

(Laboratory & 

Field 

operations) 

Executive summary. 

Statistical summaries of 

laboratory QC results; 

corrective actions; 

completeness summaries 

by site 

Precision, bias, and system 

and performance audit 

results.

Laboratories 

supporting the 

CSN

OAQPS Annual AMTIC

21.2 Annual QA 

Report to 

Management 

(Network 

Review)

Executive summary. 

Precision, bias or network 

data shifts, performance 

audit results, Unusual 

results of PE Tests and 

results of special studies 

OAQPS/

Monitoring 

QA Staff

OAQPS,

Regional EPA 

Office CSN 

Contacts

Annual AMTIC

21.3 Precision, 

Bias and 

Accuracy 

Quarterly 

Reports

Summary of precision, 

accuracy and bias tests 

(required for SLAMS/)

Monitoring 

Agency 

Regional EPA 

Office

Quarterly none

21.3 Laboratory 

Performance 

Evaluation and 

Technical 

Systems Audit 

Results

Evaluation and discussion 

of PE audit results for 

laboratories performing 

PM2.5 

EPA

chemical speciation

OAQPS Annual AMTIC

21.4 Site TSAs 

(External)

Evaluation of performance 

at individual sampling 

stations; design flow rate, 

temperature, and 

barometric pressure 

accuracy 

Monitoring 

Agency 

independent 

assessors

OAQPS Annual Flow rate 

audits 

posted on 

AQS

21.5 Routine 

Quality Control 

records

Operator's notebooks, site 

records, calibration 

records, etc.

Monitoring 

Agency 

Operations 

Personnel

Monitoring 

Agency QA 

Management

Maintained 

continuously

none

21. 6 Sampler 

performance 

Verifications

Operator reports Monitoring 

Site Operators 

or 

Technicians

Monitoring 

Agency QA 

Management 

Monthly or 

upon 

finding a 

critical 

failure

AQS 

posting is 

Optional 

but recommended

21.7 Data 

Validation 

Summaries

Listing of data for all sites 

operated by each 

monitoring agency

Analytical 

Laboratories

Monitoring 

Agency

monthly none
PM2.5 CSN QAPP

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21.8 Corrective 

Action Reports

and other 

performance 

related records

Field or laboratory 

activities.

Identification of problems, 

proposed solution, and 

results; results of invalid 

tests

Monitoring 

Agency 

Operations 

Personnel or 

CSN support 

laboratory 

Monitoring 

Agency QA 

Management

at monitoring 

agencies and 

OAQPS

as needed None, 

unless 

corrective 

action is 

necessary 

on a 

network 

wide basis

21.1 Annual Quality Control (QC) Summary Report (Laboratory)

The EPA's contracted support laboratory for the CSN program produces an annual report that 

details analytical quality measures as well as trip and field blank results, completeness 

summaries, and corrective actions. It also includes a summary of performance verifications, 

sampler audits and any noteworthy technical system audit (TSA) findings that appear to be 

systemic network issues. These reports are posted on the Ambient Monitoring Technical 

Information Center (AMTIC) website. Other laboratories performing analyses for the CSN are 

urged to produce similar documentation on an annual basis and to provide this information to the 

monitoring agencies.

 

21.2 Annual QA Report to Management (Network Review)

The Office of Air Quality Planning and Standards (OAQPS) Ambient Monitoring QA staff will 

compile an assessment each year summarizing the following: 

• Results from the collocated precision sites. 

• Results of TSAs and sampler performance audits. 

• Surprising or unusual shifts in ambient concentration results or blanks. 

• Surprising or unusual results from the performance evaluation tests of the participating 

network laboratories. 

• Results of special studies pointed at specific operating procedures or performance 

characteristics; e.g., shipping procedures, field blank collection, etc. 

• Collocated Sampler Comparison Results. 

21.3 Precision, Bias and Accuracy Reports

For the CSN, each monitoring organization must report to AIRS-AQS the results of all precision, 

bias and accuracy tests as described in Section 14 on a quarterly basis as set forth in 40 CFR 

Parts 58.16, and 40 CFR Part 58 Appendix A, Section 5. Precision from collocated samplers will 

be calculated quarterly, (although the raw data from the 6 collocated samplers across the CSN is 

submitted monthly). Since there are no independent measurements of ambient concentrations 

with which we could compare CSN results, bias and accuracy can only be is represented by 

surrogates of monthly flow checks and semiannual audits (or more frequently if chosen). 

Reporting of monthly flow checks are not mandated by the regulations, however, they can be 
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invaluable if an audit reveals that a sampler is, and has been, operating at a flow rate that 

invalidates the results. 

21.4 Laboratory Performance Evaluation and Technical Systems Audit 

Results

The EPA NAREL and OAQPS management perform periodic evaluations of the laboratories 

performing chemical speciation analyses for the CSN. Performance audits are performed on an 

annual basis. The schedule for completing these tests has varied from year to year due to the 

multiple labs that participate. Refer to the Quality Assurance Project Plan and standing operating 

procedures for EPA, ORIA, NAREL, Montgomery, Alabama.

21.5 Site TSAs (External) 

For the SLAMS program, external systems audits are conducted for each monitoring 

organization at least every 3 years by the EPA Regional Office as required by 40 CFR Part 58, 

Appendix A, Section 2.5. At least one CSN site should be audited during the review. The choice 

of sites in the PM2.5 chemical speciation program should be discussed with the responsible EPA 

Regional QA Coordinator, but first priority should be given to the speciation samplers at NCore 

sites. Appendix A-6 is a PDF version of an Excel spreadsheet that has been created to guide 

auditors through complete TSAs of the CSN monitoring sites and samplers, and electronically 

report the audit results to the lab support contractor so that the flow audit data (on whatever 

frequency the audits occur) can be posted to AQS. The national QA lead for the CSN or the 

current support lab contractor will have information as to how this spreadsheet can be acquired 

and the resulting report electronically transferred to the contract support lab. The worksheets and 

directions for their acquisition and use are also posted at 

http://www.epa.gov/ttn/amtic/specguid.html. 

21.6 Routine Quality Control Records

Routine quality control records such as operators' notebooks, control charts, calibration records, 

etc., are not considered reports to management; however, these materials must be maintained and 

made available for audits and reviews. Sampler performance verification results, however, are 

indicators of potential loss of data and should, therefore, be reported on a monthly basis with 

immediate notification of the supervisor who can deploy technicians to correct the problem. 

Appendix A-5 is a PDF version of an Excel spreadsheet that has been created to guide operators 

through QC checks of the sampler and electronically report them to the lab support contractor so 

that the monthly flow check data can be posted to AQS. The national QA lead for the CSN or the 

current support lab contractor will have information as to how this spreadsheet can be acquired 

and the resulting monthly worksheets reported. The worksheets and directions for their 

acquisition and use are also posted at http://www.epa.gov/ttn/amtic/specguid.html. 
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21.7 Data Validation Summaries

According to 40 CFR part 58.16 subparagraphs (a)-(c), all QA data collected at CSN sites in 

accordance with Appendix A will be reported in AQS. It will be consistent with the audit results 

submitted for the PM2.5 FRM/FEM network. 

The EPA contract laboratory for the CSN produces, as part of the levels 0 and 1 validation, 

creates a set of review data on a monthly basis for review by the individual agencies. The 

agencies have 45 days to review their monitoring data, the contract lab’s validation results. They 

may conduct their own levels 2 and 3 validation and submit corrections or questions. Sixty days 

after initial posting of the data (45 days plus 15), the data with any agency-required changes are 

posted on the AQS data base system for public access. The data validation summaries produced 

by the contract laboratory and the requested corrections and other correspondence are not 

published, but are maintained so that they are available for audits and reviews. Validated air 

quality data submitted for each reporting period will be entered into the AQS using the 

procedures described in the AQS Data Coding Manual. 

21.8 Corrective Action Reports and Performance-Related Records

A corrective action reporting system should be in place for all monitoring agencies. The 

Corrective Action Report procedure should be followed whenever a problem is found ,such as a 

safety issue that presents a risk to the site operators and auditors or an operational or procedural 

problem that will result in loss of data or generated invalid data. The Response/Corrective Action 

Report is one of the most important ongoing reports to operational management because it 

documents primary QA activities, provides valuable records of QA activities that can be used in 

preparing other summary reports, and may benefit other sites that encounter the same problem. 

The Corrective Action Report form should identify the originator, state the problem, and may 

suggest a solution. The form also indicates the name of the persons or persons who is/are

assigned to correct the problem, and the person responsible for verifying that the corrective 

action has been completed. Copies of the Response/Corrective Action Report should be 

distributed twice: first, promptly after the problem has been identified and corrective action has 

been scheduled, and second, when the correction has been completed. 

Corrective Action Reports (or equivalent) are normally not published but should be retained by 

the agencies for audits and reviews. Significant corrective actions should be included in the 

Annual Network Review discussed above, particularly when reportable data are affected.
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22.0 Data Review, Validation, and Verification Requirements

This section describes the verification and validation process, which is used to decide the degree 

to which each data item has met applicable quality specifications. The specific requirements for 

verification and validation are developed by estimating the potential effect that each error 

component may have on the usability of the associated data item, its contribution to the quality 

of the reduced and analyzed data, and its effect on attainment of the data quality objectives 

(DQOs). 

Verification and validation are not the same as data quality assessment or evaluation of the 

DQOs, processes which are described elsewhere in this Quality Assurance Project Plan (QAPP). 

Only after the data set has been verified and validated can it be fully assessed and/or used to 

address the specific scientific and regulatory questions embodied in the DQOs. 

Data validation summary reports should be included in regular quality control reports to 

management. These reports should include the following information, at a minimum: 

 Time interval covered by the report. 

 Site identification(s). 

 Sampler identification(s). 

 Total number of valid observations sent to the Air Quality System (AQS). 

 Number of flagged observations sent to AQS, categorized by analyte and flag. 

 Number of invalid observations (not sent to AQS), by analyte. 

 Statement of significant corrective actions taken.

22.1 Data Verification and Validation Responsibilities

Verification of data for the PM2.5 chemical Chemical Speciation Network (CSN) is the joint 

responsibility of the Monitoring Organization, which runs the field component of the program, 

and the CSN support laboratory, which analyzes the samples and calculates and reports the data. 

Table 22-1 describes the respective responsibilities of the field and laboratory components for 

data verification and validation. 
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Table 22-1 Data Verification Activities and Responsibilities for the CSN

Verification Activity State, Local or Tribal Monitoring Organization CSN Laboratory 

Data source attribution The Monitoring Organization should compare the 

information on the chain of custody (COC) and field 

data form with labels on modules received. Report 

any discrepancies to the CSN support laboratory.

. Verify that the 

site, date, time, and channel assignments 

are correct. Logbooks, reporting forms, 

data custody sheets, and electronic data 

transmittals should be checked for 

consistency. The COC forms should be corrected to reflect the 

actual module used for a particular sampling 

channel, if other than originally assigned by the 

laboratory.

Discrepancies in module assignment due to 

procedural errors in the field operation should be 

corrected and documented. 

The CSN support laboratory is responsible for generating the 

COC sheets and placing corresponding labels on sample 

modules sent to the field. The laboratory should respond 

immediately to notifications from the field of shipped

modules that do not agree with the COC sheet.

The support laboratory database management system 

(DBMS) will accommodate changes of module assignment 

reported by the field.

Discrepancies in module assignment due to procedural errors 

in the laboratory sample handling operation should be 

corrected and documented. 

Results for samples that cannot be positively identified must 

be flagged as invalid in AQS.

Site selection and monitor placement. The Monitoring Organization is responsible for 

ensuring that all siting criteria have been met when 

originally siting a CSN sampler. Continued 

compliance with siting criteria should be verified at 

least annually by the Monitoring Organization.

If the support laboratory is notified that a particular CSN

sampler is in violation of siting criteria, the corresponding 

AQS data may have to be flagged or invalidated. This 

decision should be made jointly by the Monitoring

Organization and EPA Regional Office with oversight 

responsibility for that MO . 
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Verification Activity State, Local or Tribal Monitoring Organization CSN Laboratory 

Integrity of sample handling. The Monitoring Organization should develop and 

follow SOPs for sample handling and/or follow 

those provided by the contracted support laboratory. 

It is very important that the PM

 This 

involves verification that the SOPs for 

sample handling have been followed so 

that the physical integrity of the sample 

and its correct identification are ensured. 

This requires that both the field and 

laboratory operations follow the approved 

SOPs and that any discrepancies are 

followed up and resolved. System Audits 

should include a step-by-step review of 

sample handling procedures. Data audits 

should include examination of original 

custody sheets and other records to look 

for discrepancies in sample identification.

2.5 sampler flow rate 

be within ± 5 % of the design flow rate.

The field operation should conduct internal audits 

and submit to external audits and reviews of its 

sample handling and data processing systems.

The field operation should cooperate with 

investigations of data integrity initiated by the CSN

support laboratory, U.S. Environmental Protection 

Agency (EPA), or others.

The CAR process should be followed when 

investigating isolated or systematic discrepancies. 

Systematic problems should be addressed by 

revision of the appropriate SOP.

The CSN laboratory should develop and follow SOPs for 

sampling module shipment and sample handling.

The laboratory should conduct internal audits and submit to 

external audits and reviews of its sample handling and data 

processing systems.

The CSN support laboratory should cooperate with 

investigations of data integrity initiated by a Monitoring

Organization, EPA, or others.

The CAR process should be followed when investigating 

isolated or systematic discrepancies. Systematic problems 

should be addressed by revision of the appropriate SOP.
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Verification Activity State, Local or Tribal Monitoring Organization CSN Laboratory 

Checks on sample containers and 

preservation methods. Specific checks on 

sample containers include examination 

for physical integrity and comparison 

with the COC and data sheet for correct 

identification. The chief preservation 

method for exposed sample modules is 

the use of a chilled ice substitute in 

insulated shipping containers to reduce 

the temperature to 4o

The field operation is responsible for checking the 

integrity of shipping containers and individual 

modules upon receipt or deployment at the site. The

CSN support laboratory should be notified 

immediately of any damage that may have occurred 

in shipment.

C.

The field operator is responsible for chilling the ice 

substitute prior to shipping the exposed sample 

modules back to the CSN support laboratory. 

The CAR process should be followed if a systematic 

problem is suspected.

The CSN support laboratory is responsible for properly 

packaging the modules in shipping containers that include 

the required number of ice substitutes.

The CSN support laboratory is responsible for notifying the 

carrier and initiating claims for shipping damage.

The CSN support laboratory is responsible for checking the 

condition of the shipping container, its interior temperature, 

and individual modules upon receipt from the field.

The CSN laboratory must note any discrepancies that might 

affect sample validity in the DBMS. The Monitoring

Organization should be notified if the problem might be due 

to packaging procedures.

The CAR process should be followed if a systematic 

problem is suspected.

This is typically ensured using systems audits, EPA 

Regional reviews, and results of performance audits. 

Failure on any of these checks could imply that some 

samples acquired prior to the check are suspect or 

invalid. It is very important that the PM

Procedures to ensure that data were 

generated as specified in the sampling or 

analysis SOP.

2.5 sampler 

flow rate be within ± 5 % of the design flow rate.

The CSN support laboratory and the EPA CSN

Regional Coordinator should be notified if serious 

procedural issues are raised.

The CAR process should be followed to document 

and rectify systematic procedural problems.

Integrity of laboratory analysis procedures is typically 

ensured using internal and external systems audits and 

results of performance audits. Failure on any of these could 

imply that some samples analyzed prior to the check are 

suspect or invalid. 

Monitoring Organization(s) with affected samples and the 

EPA Project Officer (PO) for the CSN support laboratory 

contract should be notified if serious procedural issues are 

raised.

The CAR process should be followed to document and 

rectify systematic procedural problems.
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Verification Activity State, Local or Tribal Monitoring Organization CSN Laboratory 

Systematic problems that lead to unacceptably large 

biases should be investigated and documented using 

the CAR process. 

Activities to determine how seriously a 

sample deviated beyond the acceptable 

limit so that the potential effect on the 

validity of data can be evaluated.

A person within the organization should be 

designated to investigate serious discrepancies 

affecting sample data. This designation should be 

formalized in the organization's quality management 

plan (QMP) or in an appropriate SOP.

The CSN support laboratory should be notified when 

a data discrepancy is first suspected and again when 

the discrepancy is quantified and the investigation is 

closed.

Although it would be impossible to prepare SOPs for 

assessing every contingency, the organizational 

responsibility and general approach for investigating 

discrepancies should be clearly documented.

Systematic problems that lead to unacceptably large biases 

should be investigated and documented using the CAR 

process. The support laboratory supervisor is usually in a 

position to investigate such occurrences, but this 

responsibility can also be delegated to a qualified analyst or 

to the project QA staff with the concurrence of the 

laboratory supervisor and the Services Program Manager.

Data should be corrected, flagged, or invalidated based on 

the best assessment of the individual situation. 

Corrections to previously sent data should be transmitted to 

AQS as soon as feasible. The EPA and the Monitoring

Organization should also be notified when its data in AQS 

are changed. 

Data corrections and flagging should be noted in regular QC 

reports to management. [Detailed summaries are prepared 

monthly and are reviewed by the CSN QA Officer. Annual 

QC reports are also prepared, containing summaries of data 

corrections and flagging, which are transmitted to EPA and 

posted on the public AMTIC website.]
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22.2 Corrective Action Reporting Process

Each Monitoring Organization and the CSN support laboratory should have a Corrective Action 

Reporting (CAR) process in place. Ideally, this process should closely resemble corrective action 

procedures used with other monitoring activities conducted by the organization. This process 

should consist of the following elements: 

 A description of the organizational responsibilities and procedures for instituting 

corrective actions for the CSN program. This would be appropriately placed in the 

organization's CSN standard operating procedures (SOPs) or in the QMP. If an 

adequate process already exists in the organization, it is not necessary to develop new 

procedures for the CSN. 

 A reporting form (i.e., the CAR form) describing the event or problem along with a 

suspected cause; a recommended solution is optional. Other information should 

include the date and the submitter's name. 

 A means for assigning responsibility for the corrective action investigation, as well as 

for scheduling and appropriating resources to it. 

 All active and just-completed CAR investigations should be reported in the next 

scheduled quality control (QC) report to management or equivalent document. Dates 

and sites of reportable data affected by the problem should be provided in detail. 

Delayed or canceled CAR investigations should be identified and the reason for 

delaying or canceling the investigation justified.

 The CAR files should be subject to regular audits and reviews. 

22.3 Use of QC Information for Verification and Validation

The various QC samples used with the CSN are also potential sources for verification/validation 

information. Table 22-2 summarizes QC information and its uses in data verification and 

validation. 

22.4 Use of Calibration Information for Verification and Validation

Calibrations can generate information that is useful in the verification and validation process. 

Because this information is often not directly associated with a particular sample, procedures 

must be in place to identify data that were dependent on a particular instrument when the 

calibration data indicate that the instrument's performance was suspect. These considerations 

apply to most analytical chemistry instruments; the balances used to weigh filters; and the field 

calibrations of flow, temperature, and barometric pressure. It is very important that the PM2.5

sampler flow rate be within ± 5 percent of the design flow rate. Each SOP that involves the use 

of quantitative calibrations must include the following considerations related to eventual use of 

that data for data verification and validation: 

 A mechanism for reporting calibrations that are out of specifications. 
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 A means for identifying all data that might be affected by the problem (all sample 

data back to the last acceptable calibration should initially be considered suspect; 

investigation may be required to estimate the maximum probable error and to decide 

on the validation status of sample data). 

 A set of acceptance limits on the calibration that address zero/offset, bias/gain/slope, 

and linearity/noise. 

 A procedure for verifying out-of-limits calibrations. 

Table 22-2. Quality Control Data for CSN Data Verification and Validation 

Type of QC 

Data Responsibility Usage for Verification and Validation

Field Blanks Joint lab and 

field

High field blank values may indicate high levels of contamination 

introduced by the sampler or the filter loading process. Data currently 

reported from the CSN program are not numerically corrected for field 

blank levels. The CSN support laboratory includes all field blank data in the 

monthly data reports that are sent to the Monitoring Organizations for 

review. Monitoring Organizations should raise questions with the CSN 

support laboratory if unexpectedly high blanks are found. Data may be 

flagged or invalidated based on the results of investigation.

Trip blank Joint lab and 

field (primarily 

lab)

High trip blanks (with or without a corresponding high field blank) may 

indicate a laboratory problem, or a problem with filter media, or with 

shipping and handling. Corrective actions should begin in the laboratory.

Data currently reported on the CSN program are not numerically corrected 

for field blank. The CSN support laboratory should investigate systematic 

high trip blanks. Data may be flagged or invalidated based on results of 

investigation. 

Sampler leak 

check failed

Field Leak checks of the MetOne and the URG 3000N samplers have been 

designed to indicate a pass or fail situation although either sampler can run 

if a failing leak is occurring. If a failing leak is detected during a leak check 

or audit, the person conducting the assessment should consult with the 

manufacturer’s operators manual for a troubleshooting guide or contact the 

technical service department. The period of time and number of sampling 

events that may have experienced the failing leak should be reported to the 

CSN support laboratory immediately so that data can be flagged or 

invalidated appropriately.

Sampler flow 

rate check/audit

results outside of 

acceptance 

criteria

Field The ability of a filter-based particle sampler to achieve the correct cut point 

is critically dependent on the sampling flow rate. It is very important that 

the PM2.5 sampler flow rate be within ± 10 % of its design flow rate. Flow 

Rate CV’s should be examined periodically and compared against the 

advisory limits established for the particular sampler. High CVs are an 

indicator that the flow rate may not have been within the ± 10 % limits. 

Severe departure from the normal CV would be grounds for invalidating 

results. Note advisory limits have been established at 5%. 
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Type of QC 

Data Responsibility Usage for Verification and Validation

Sampler 

temperature, 

barometric 

pressure sensor, 

or flow rate 

sensor failed

Field Sensor failures should be investigated as soon as they are detected. Sensor 

failures may directly affect the flow through one or more sampling modules 

and therefore must be documented. The operator discovering the problem 

should describe the error quantitatively, if possible. The operator should 

also try to determine when the sensor began to malfunction. Data back to 

the last successful check may be suspect. If it appears that the failure could 

cause an error of 10% or more in the sampler’s design flow rate, the 

problem should be brought to the attention of the CSN laboratory so that 

data can be flagged or invalidated appropriately and steps can be taken to 

promptly correct the problem. 

Filter integrity 

inspections

Lab and field Filters that fail the initial visual integrity inspection at the CSN laboratory

should not be used. If the filter has not been used for sampling, its number 

can be voided in the laboratory's DBMS and no further action is necessary. 

Failure of visual inspection after sampling usually results in data 

invalidation or flagging. The person making the inspection should document 

it on the COC and data form or in the analytical results data. Data entry 

personnel should make the appropriate entry when the data are input into the 

DBMS. The original analyst’s notes or COC form may have to be consulted 

during data validation to determine the seriousness of the problem and the 

validity status of the reported data.

Repeated or systematic filter failures may be caused by many different 

factors including rough handling, manufacturing defects, environmental 

factors during sampling (rain, insects, etc.), defective packing materials, or 

contamination in the sampler before or after sampling. Systematic problems 

should be investigated using the CAR process and documented in QC 

reports to management.

Laboratory QC 

samples

Laboratory A large number of routine QC samples are run in the gravimetric and 

chemical laboratories. In many cases, instrumentation problems detected by 

QC sample results can be corrected before any sample data are affected. The 

specific acceptance criteria for laboratory QC samples are generally 

determined by statistical methods (e.g., control charts or equivalent) or by

comparison against set limits defined in the method and given in the SOP.

These acceptance limits should be posted in the laboratory; each analyst is 

responsible for identifying out-of-specification QC results. 

Reserve aliquots or specimens of the original media should be retained until 

successful post-analysis QC results have been obtained. (Aliquots and 

specimens are also archived for a period of time under the CSN program, so 

reanalysis may be possible at a later time; however, the results are generally

less accurate and more costly to obtain than immediate reanalysis.)

If QC results indicate an unacceptable uncertainty regarding the true value

and the analysis cannot be reproduced, the data must be invalidated or 

flagged. 
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 Procedures for correcting data taken with defective calibrations. Errors other than 

simple drift in the instrument’s response factor, such as excess noise and calibration 

nonlinearity, should generally not be corrected by recalculation; instead, the 

instrument should be repaired and the samples rerun if possible. Recalculation of 

results due to shifts in the instrument’s response factor should be done only with the 

approval of the laboratory supervisor, and these changes should be documented 

appropriately by the laboratory. 

Other considerations regarding calibrations that facilitate their use in the data verification/ 

validation process include the following: 

 Calibrations should be performed within an acceptable time before and after analysis 

of field samples as specified in the SOP. The acceptable time window is typically a 

function of the instrument's drift characteristics.

 Calibrations, other QC samples, and field samples should be done in proper sequence; 

for example; the positions of vials in an auto-sampler should be double-checked and 

all vials should be labeled if possible. 

 Calibration points must bracket the concentration range of interest and should be 

spaced according to the needs of the method as defined in the SOP. Note that only 

one-point flow rate calibrations are possible with the MetOne sampler. The URG 

3000N provides for a three-point calibration. If either will not retain the calibration 

the manufacturer should be contacted for guidance on troubleshooting and repairs. 

The Contract Support Lab should be informed of sampling events that were affected 

by incorrect flow rates due to poor calibration. 

 Enough points should be included in a multipoint calibration to assess noise and 

linearity (it may not be necessary to assess noise and linearity on a daily basis, 

depending on the type of instrument).

22.5 Level 0 Verification and Validation

Basic review of data with respect to their origin, documentation, and critical criteria is referred to 

as "level 0" verification and is performed by the CSN support laboratory. The criteria to be 

applied during level 0 verification of the data set are summarized below: 

 Data source attribution—Verify that the site, date, time, and channel assignments are 

correct. Logbooks, reporting forms, data and chain of custody sheets, and electronic 

data transmittals should be consulted if a problem of attribution is suspected. 
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 COC verification—All COC forms for filters and denuders will be checked for 

completeness at the CSN support laboratory before they are entered into the data base 

and archived. Missing information should be identified by the data entry operator and 

brought to the attention of the Sample Handling and Archival Laboratory (SHAL) 

supervisor. The laboratory QC supervisor or designee should determine the validity of 

any samples for which mandatory COC and field data information is missing. It may 

be necessary to contact the state, local, and/or Tribal (SLT) Monitoring Organization 

to attempt to fill in this information.

 Holding times and conditions—The shipping and receiving documentation for all 

PM2.5

 Data transmission and recording integrity—Each error in data integrity that is 

identified must be investigated and corrected and/or appropriate actions taken. The 

CSN support laboratory QA manager should determine whether an uncorrectable data 

transmission error affects data validity. The CAR process should be used with 

problems of a systematic nature.

chemical speciation samples (filters and denuders) should be checked to verify 

that holding times have been met and that required storage conditions such as 

temperature met the requirements. Data should be flagged in AQS if holding times 

and shipping/storage conditions were violated. The CSN support laboratory quality 

assurance (QA) manager, in consultation with the EPA and the laboratory 

supervisor(s), will decide the validity of any samples for which these conditions have 

been violated. 

 Calibration status of sampler and sensors—The Monitoring Organization must have a 

means for verifying that PM2.5

 Audit status—The Monitoring Organization must verify that all monthly, quarterly, 

and other scheduled audits defined in the applicable SOP or QAPP have been 

performed on time. Samples taken when a systems audit or transfer standard 

recertification was past due must be appropriately flagged in AQS. It is the 

responsibility of the Monitoring Organization to identify such data to the CSN

laboratory because audit records are typically not available to the CSN support 

laboratory. 

speciation samplers were calibrated or checked within 

the required windows of time. Samples taken when the instrument was past due on 

any calibration or recertification interval must be appropriately flagged in AQS. It is 

the responsibility of the Monitoring Organization to identify such data to the CSN

support laboratory because sampling records received by the laboratory do not 

include all the necessary information. 
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 Operational flags—All operational flags generated by the sampler electronically or 

recorded on the COC data sheet by the operator will be entered into the data base. A 

translation between sampler codes and AQS validation flags has been developed. 

Section 19.5 of this QAPP presents the AQS data flags used by the CSN support 

laboratory to qualify data. Operational flags can result in data flagging or

invalidation, depending on the severity. 

22.6 Level 1 Data Validation

Validation (level 1) is the process of evaluating the correctness and acceptability of individual 

items or groups of items within the data set using statistical methods and other screening 

techniques. This process involves evaluating the impact of verification problems, QA or QC 

problems, and statistically detected anomalies on the usability of the data for their intended 

purpose. 

Level 1 validation of field data will first involve the processing of verification results and data 

screens into AQS data flags and then providing an overall assessment of the validity of the data 

item or items. Based on the number and types of data flags and other information generated 

during the verification and validation process, some data may be designated as invalid. Invalid

concentration data are not reported to AQS, although flagged records are uploaded in place of the 

missing observation data to indicate that the data have been invalidated. The following items are 

involved with validation of the PM2.5

 Operational data screening—temperature, barometric pressure, flow, and other 

operational data are screened for compliance with acceptance limits established for 

the CSN program. 

chemical speciation field data:

 Filter inspections and other manual verification procedures performed by the site 

operator and CSN support laboratory personnel. 

 Validation flags attached and reported—A limited number of flags are provided in 

AQS to document exceptional conditions that apply to specific data items. Only valid 

data are reported to AQS. 

 Invalid data are identified—Based on the number and types of data flags and other 

information generated during the verification and validation process, some data may 

be designated as invalid. Invalid data are not reported to AQS. 

22.7 Data Screening Techniques Used by the Contracted Support 

Laboratory

The following procedures will be performed by the Contracted Support Laboratory before the 

data are made available to the monitoring agencies. 
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Preliminary Crosstab Reports by Site, Parameter Occurrence Code (POC), and Scheduled 

Dates

 

These are examined and anomalous results are investigated and corrected. The following 

crosstab tables are routinely generated:

 Chain of Custody (COC) form number for each event - include field and trip blanks, 

routine samples, unscheduled blanks. Missing cells in the table are investigated. 

 Total counts of AQS-deliverable records - each sampler type should generate a 

specific number of counts; exceptions are investigated. 

 Counts of invalid or suspicious analyte records. 

 Sampled date (i.e., the date actually sampled, as recorded on the COC form) - date 

scheduled is compared against date sampled. Any event where these do not agree is 

investigated.

Examination of Chain of Custody Forms 

COC forms are inspected for completeness by QA personnel. Flags assigned by the site operator 

or by the support laboratory’s sample handling or data entry personnel are reviewed and 

corrections are made if necessary.

Statistical Outlier Checks and Range Checks. 

Limits used for outlier checking are provided in Tables 22 - 4 below. The Quality Assurance 

Organization reviews these results and investigates problems. Outlier checks include the 

following: 

 Lower Limit on PM2.5

 Mass Balance - Routine samples only. 

Mass - Routine samples only. 

 Anion/Cation ratios - Routine samples only. 

 Sulfur/Sulfate ratios - Routine samples only. 

 Upper Limit on PM2.5 Mass - Blank samples only. 

These steps are repeated until the data base is consistent and all exceptional conditions are 

explained.
PM2.5 CSN QAPP

Section No. 22

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Entry and Verification of Data Changes from SLT Agencies and AQS Data Verification

The following step is done approximately 2 months after validation of the preliminary data set.

 Changes requested by the SLT agencies are entered into the support laboratory’s data 

base.

 The AQS text file is generated and is copied back into a QA table in the data base 

which is used for reporting and automated comparisons. 

 Crosstab tables are made from the AQS data table; these tables are compared with 

previously generated crosstab tables for the reported batch. These are inspected as 

described above. 

 After any anomalies are corrected, the AQS text file is regenerated. This is repeated 

until all problems are corrected. See Tables 22-3 through 22-6. 

Table 22-3. Statistical Validation Limits for Blanks 

Sampler/ 

Analyte(s) Percentile Tail Sample Type

Limit

μg/filter

Flagged

Analytes

Internal

Flag

MetOne/ 

PM25

5.0

Mass

Upper Field Blank 20.00(a) PM25 Mass QL1

MetOne/ 

PM25

5.0

Mass

Upper Trip Blank 14.00(a) PM25 Mass QL1

MetOne/SHA

L 

PM25

2.75

Mass

Upper SHAL Blank TBD (b) PM25 Mass QL1

URG 3000N/ 

Carbon

2.75 Upper Field Blank 6.7 Total Carbon 

Mass

QL1

URG 3000N/ 

Carbon

2.75 Upper Trip Blank 6.5 Total Carbon 

Mass

QL1

URG 3000N/ 

SHAL/Carbon

2.75 Upper SHAL Blank 1.8 Total Carbon 

Mass

QL1

(a) The orginal value for outliers was based on the MDLs for PM2.5 mass as measured by an FRM with a flow 

rate of 16.67 liters per minute. These new values are using the same regulatory MDL, 2.0 μg/m3

, multiplied 

by the flow rate of the MetOne sampler, 9.7 m3

/24 hr. event. The values are supported by data as recent as 

2009 and 2010. See Annual Data Summary Report for the Chemical Speciation of PM2.5 

(b) The MetOne SHAL blank will have to be computed from data that will be collected over the first 3 years of 

its collection, beginning in 2012.

Filter Samples 

Project: January 1 through December 31, 2010. <http://www.epa.gov/ttn/amtic/specdat.html>. 
PM2.5 CSN QAPP

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Table 22-4. Statistical Validation Limits for Routine Data

Percentile Tail Analyte(s) Sample Type

Limit

μg/m3

Flagged

Analytes

Internal

Flag

2.0 Lower PM25 Mass Conc. Routine 2.98 PM25 Mass Conc. QL1

2.0 Lower Anion/Cation Ratio Routine 0.86 all ions QAC

2.0 Upper Anion/Cation Ratio Routine 2.82 all ions QAC

2.0 Lower Mass Ratio Routine 0.60 all analytes QMB

2.0 Upper Mass Ratio Routine 1.32 all analytes QMB

2.0 Lower Sulfur/Sulfate Ratio Routine 0.25 ions, XRF QCR

2.0 Upper Sulfur/Sulfate Ratio Routine 0.45 ions, XRF QCR

Table 22-5. Mapping of Outlier Flags Onto AQS Codes

Objective Cause Found for Level 1 Outlier

AQS codes

If NOT Invalid

(Suspicious)

If Invalid

Lab Error

Filter Damage

Module Assignment Error

Sampler Malfunction [4]

Unusual Conditions noted by operator [4]

Unknown Cause [4]

[1]

[1]

[1]

(N/A)

[2]

T

AR

AJ

AQ or AR

AN

[3]

AS

Notes:

[1] - No appropriate AQS validity status code exists in current AQS. 

[2] - Use the applicable AQS validity status code, or T.

[3] - Use the applicable AQS null value code, or AM.

[4] - Other flags may be assigned in consultation with the Monitoring Organization to more precisely define the 

cause of the problem.

(N/A) - Not Applicable

Table 22-6. Automated Range Checks 

Parameter Limits AQS Flag or Action

Exposure Duration, t 23<t exp exp<25 hrs AN - machine malfunction

AQ - collection error

AV - power failure

or other code as appropriate

Holding Time before removal 

from sampler, (FHT) 

FHT > 96 hrs IF the sampling 

schedule is not based on the 

sequential samplers, then 48 hours.

AM - miscellaneous void

(pick-up holding time is not defined in 

current AQS) 

Average Flow Rate, Favg within 10% of target flow rate AH - flow rate out of range

Temperature Reasonableness 

(all temperature channels)

-20 < T < 45 (could vary by site 

and season)

AN - machine malfunction

 or other code as appropriate

Barometric Pressure (all) 550 < BP < 800 AN - machine malfunction

 or other code as appropriate
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22.8 Treatment of Deviations From Requirements

Deviations from requirements call for a variety of response activities that are summarized below:

Flag Data in AQS—Chemical speciation data should be marked with a data validity flag only if 

the data are considered valid for most purposes and uses. 

Invalidate Data in AQS—Data of uncertain origin and data with unacceptable levels of 

uncertainty should not be included in AQS. The corresponding concentration data will be 

reported as missing with an AQS missing value code substituted. 

CAR Process—The Monitoring Organization’s CAR process or equivalent should be followed in 

cases of systematic problems or problems affecting a significant number of data points The 

CAR process is described in Section 22.2. 

Revision of SOPs and Other Project Documentation—One of the most significant of the possible 

outcomes of the CAR process is the identification of the need for revising SOPs and other project 

documentation. Procedural changes to overcome identified problems are a key element in the 

continuous improvement of the CSN program. 

Consultation to Determine Impact of Deviation—The cognizant QA supervisor in an 

organization is typically charged with the responsibility of determining the impact of a deviation 

from requirements on data quality. This process should involve consideration of the primary 

DQO of trend detection described in Section 7.0 as well as other potential uses of the data such 

as source attribution. 

Notification of EPA or Other Stakeholders

22.9 Verification and Validation Criteria: Field Component

—The investigation of a serious or systematic problem 

should consult operators, analysts, and other personnel involved with the situation being 

investigated, as well as stakeholders who might be impacted by the decision to validate or 

invalidate data. Field organizations should contact the CSN laboratory (through channels 

approved by the delivery order project office) to provide documentation of corrective actions that 

might affect the data validation status of reportable data. The state Monitoring Organizations 

should include significant QA problems in their annual QA reports to management.

Table 22-7 summarizes the verification and validation criteria applicable to the field program. 

The verification and validation (level 0 and level 1) criteria are combined into a single table 

because the criteria overlap.
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Table 22-7. Data Verification and Validation Summary

Item Criteria

Applicable 

to Comment

Flag in 

AQS if 

Violated

Invalidate

if Violated

Sampler and site identification Must be 

correct

Data forms Investigate and correct, if 

possible; invalidate data 

if identification cannot 

be established

●

(see notes)

Date and time identification Must be 

correct

Data forms ●

Filter or denuder channel 

assignment

Must be 

correct

Data forms ●

COC and Data Form records for 

filters and denuders

Must be 

present

COC forms, 

sample labels

Review and determine 

impact on data validity

○

(see 

notes)

○

Holding times and shipping and 

storage conditions:

 unexposed samples, 

holding time, and storage 

temperature

 exposed samples, 

residence time in sampler 

before retrieval

 exposed samples, on-site 

holding time plus shipping 

time, and shipping 

temperature

 holding time and storage 

temperature after receipt 

in the laboratory prior to 

analysis

See criteria 

tables in 

Section 20.0.

All filters Review and determine 

impact on data validity

● ○

Electronic data transmission No errors 

reported

Electronically 

transmitted 

data

Review and determine 

impact of the error on 

data validity

○

Sensors checked or calibrated 

within required time frame

All 

temperature, 

barometric 

pressure, and 

flow rate 

sensors

Routine 

calibration 

records

Dates of required sensor 

checks should be verified 

before data are reported

○

Transfer standards recertified 

within required time frame

All transfer 

standards 

routinely 

used by site 

operator

Audit and 

recertification 

records

Dates of recertifications 

should be verified before 

data are reported

○
PM2.5 CSN QAPP

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Item Criteria

Applicable 

to Comment

Flag in 

AQS if 

Violated

Invalidate

if Violated

Sampler-generated flags 

(electronic data):

 filter/ambient temperature 

difference

 flow rate out of 

specification

 total sampling time out of 

specification

 sampling start or stop time 

out of specification

See criteria 

table

Electronic 

data

Data should be reviewed 

and evaluated to 

determine validity for 

reporting to AQS

● ○

Operator flags and other 

information from field data 

forms:

 filter inspections

 other conditions noted by 

operator that could impact 

the sample

See field 

data form

Field data 

forms

Operator’s notes should 

be evaluated regarding 

probable impacts on data 

validity

○ ○

Statistical screening of 

operational data:

 temperature

 barometric pressure

 flow

 other operational data

See criteria 

tables

Data 

summaries

Development of 

statistical data screens 

will be coordinated with 

the laboratory

○ ○

• Flagging or invalidation is optional. Monitoring Organization should review the circumstances and the 

potential impact on the data. When both columns are marked with this symbol, there are three choices: (1) 

report to AQS without a flag if the data need not be qualified to the data user, (2) flag the data and report to 

AQS if the user might need to know that the data are qualified but may be usable for certain purposes, and 

(3) invalidate the data (invalid data are not reported to AQS).

Notes:

• Flagging or invalidation is mandatory. When this symbol is shown in the "Flagging" column and the 

"Invalidation" column is blank, the data must be flagged and must be reported to AQS. 
PM2.5 CSN QAPP

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23.0 Validation and Verification Methods

The processes for verifying and validating the measurement phases of the chemical Speciation 

Trends Network data collection operation have been discussed in the previous section. If these 

processes are followed, the quality of data should be achieved to meet the data quality objectives 

for trend detection. This section describes the organizational implementation of the validation 

procedures, the applicability of corrective actions, and the reporting requirements and schedules. 

The process of data validation and verification is a cooperative effort between the reporting 

organization responsible for field sampling and the Chemical Speciation Network (CSN) 

laboratory, which conduct the chemical analyses and reports the validated concentration values 

to the Air Quality System (AQS). This section focuses on the verification and validation methods 

applied by the reporting organizations, Monitoring Agencies, after the first stages of validation 

have been completed by the CSN laboratory. 

The Monitoring Agencies are encouraged to review and utilize similar procedures and tools for 

validating the CSN data. To this end a document EPA under wrote the book “Data Validation 

Process for the PM2.5 Chemical Speciation Network” developed by RTI under contact. See it at 

http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/05datval.pdf. RTI was also commissioned 

to develop an automated data review tool, the Speciation Data Validation and Analysis Tool 

(SDVAT < http://www.epa.gov/ttn/amtic/sdvat.html>. The CSN contract support laboratory 

provides technical support for this tool as well. The tool accepts the monthly-produced 

spreadsheets posted on the secure CSN website managed by the lab service contractor. The 

includes several of the data review methods listed below. 

 Data completeness. 

 Time series analyses. 

 Outlier tests. 

 Mass concentration reconstruction. 

 Pie chart species distributions. 

 Spatial and temporal variability analyses.

23.1 Interorganizational Responsibilities for Data Validation

The sequence of data verification and validation steps and the corresponding organizational 

responsibilities are as follows:

1. The CSN laboratory issues unexposed sample module kits to the Monitoring 

Agencies along with a partially completed Custody And Field Data Form (CAFDF). 

2. The Monitoring Agency exposes the filters, fills in the necessary data about the 

exposure on the CAFDF form, and returns them to the CSN laboratory. 

3. The CSN laboratory enters the data recorded on the CAFDF, performs the data 

analyses, and enters the results into the data system. 
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4. The CSN laboratory performs level 0 and level 1 data validation based on the data to 

which it has access. This includes validation of laboratory results and entry of any 

validation flags associated with problems noted on the CAFDF received from the 

field.

5. After all validation is completed for a data set, the CSN laboratory transmits the data 

and associated validation flags in hardcopy and electronic form to the delivery order 

project officer (DOPO) who, in turn, distributes the data to the respective Monitoring 

Agency. 

6. The Monitoring Agency completes the verification and validation process at levels 2 

and 3 based on information compiled from previous PM2.5 research programs, 

guidance from the Clean Air Scientific Advisory Committee and Expert Panel on 

PM2.5

7. The Monitoring Agency forwards the validated data back to the CSN laboratory for 

submission to AQS. 

 Speciation, its own internal records, audit results, and other information 

available from site operators and other local sources. 

8. Further statistical validation may be performed by the EPA and others as needed. 

23.2 Personnel Responsibilities Within the Reporting Organization

The Monitoring Agency should assign data validation responsibilities according to its 

organizational structure and the needs of this program. It is recommended that the following 

roles and responsibilities for CSN data validation be defined within the Monitoring Agency. 

Program Manager—The Monitoring Agency's manager for the PM2.5 chemical CSN is 

ultimately responsible for meeting schedules, for ensuring that qualified staff perform data 

management and validation functions, and for delivering valid data to AQS. The Monitoring 

Agency's CSN Manager should ensure that data validation and data management responsibilities 

have been assigned to individuals with the appropriate educational background, training, and 

knowledge of the CSN program. 

Data Validation Specialist—The Data Validation Specialist is the person who conducts the actual 

examination of data received from the CSN laboratory via the DOPO. This person should be 

knowledgeable about quality assurance principles, particulate measurement methods, and basic 

statistics and chemistry and should be familiar with network operations including sampler 

operation and shipping and receiving of sample modules. Often, the quality assurance supervisor 

responsible for the CSN program will be assigned to validate the data. The Data Validation 

Specialist should be supported by data management personnel, chemists, environmental 

scientists, and statisticians to deal with questions that arise during the validation process. It is 

critically important that field personnel, particularly the operator responsible for CSN sampling 

and his/her supervisor, be available to answer questions. The Data Validation Specialist should 

also have ready access to project files and relevant data sets.
PM2.5 CSN QAPP

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The following sections describe the verification and validation procedures that should be applied 

by Monitoring Agencies to the partially validated data received from the CSN laboratory. 

23.3 Completion of Level 0 Data Verification and Validation

The first step in the Monitoring Agency's data verification and validation process should be to 

confirm that the data are correctly accounted for according to the Monitoring Agency's own 

records. The CSN laboratory will have checked the data according to its shipping and receiving 

records and the chain of custody data form and will have flagged any discrepancies in data 

attribution. The Data Validation Specialist should examine each discrepancy that the CSN

laboratory has flagged as suspicious due to uncertain attribution or problems with chain of 

custody. The Monitoring Agency should examine its copy of the CAFDF, shipping and receiving 

records, operator logbooks, and any other relevant records to address the problem. (The CSN

support laboratory may have already contacted the Monitoring Agency, via the DOPO, regarding 

problems of data attribution, so a repeated check of a previously investigated problem may not 

be necessary.) The Monitoring Agency can deal with this type of flagged data in a number of 

different ways, as follows: 

 If the level 0 flag can be explained and the data are correct, the flag may be removed 

or changed to a more appropriate flag. 

 If the CSN laboratory has flagged data as misassigned (i.e., assigned to the wrong 

sampling date, site, analyzer, or channel), the Monitoring Agency may edit the data 

so that monitoring data are correctly assigned. This may only be done if verifiable 

information can be found in the Monitoring Agency's operating records that allow the 

correct data assignments to be made. 

 If concentration values that have been flagged can be corrected numerically (e.g., by 

correcting an incorrect sample volume recorded on the CAFDF sheet), the Monitoring 

Agency can make this correction directly, but it is recommended that this information

be passed back to the CSN laboratory, via the DOPO, so that the calculation can be 

verified.

 If the Monitoring Agency cannot find an explanation for a flagged discrepancy, the 

data flag should be allowed to stand. 

23.4 Identification of Outliers and Data Flagging Techniques

23.4.1 Manual Methods

To fully complete the validation process, the Monitoring Agency must examine the data set, both 

flagged and unflagged data, for validation criteria based on information sources available within 

the organization. The validation tables in Section 22.0 of this document should be consulted for 

specific validation criteria. Some validation criteria that are not easily automated are listed 

below: 
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 Manual Data Inspection



—The purpose of manual data inspection is to spot unusually 

high (or low) values that might indicate a gross error in the data collection system. It 

is often helpful to plot data in a time series. 

Systems Audit Report Results



—Audits occasionally turn up serious deficiencies that 

could affect the validity of the data. For example, if it is found that a field operator is 

mounting sample modules incorrectly, it would be necessary to flag or invalidate all 

the data corresponding to that sample module when that operator was working. 

Performance Audit Results



—Large deviations from acceptance or advisory limits for 

critical measurements such as sample volume accuracy could result in data 

invalidation or flagging back to the last previous acceptable audit or control check 

result. Poor performance audit results should be investigated further, and if a specific, 

identifiable problem is uncovered that affects reportable data, that data should be 

flagged or invalidated. In general, reportable data should not be invalidated unless a 

specific, identifiable cause for the discrepancy can be found. 

Collocated Sample Results—Performance on collocated duplicates should be 

evaluated if information is available. Collocated sampling equipment may include 

FRM samplers operated for the PM2.5



 mass network. Poor collocated sample results 

should be investigated further, and if a specific, identifiable problem is uncovered that 

affects reportable data, that data should be flagged or invalidated. In general, 

reportable data should not be invalidated unless a specific, identifiable cause for the 

discrepancy can be found; however differences greater than a factor of 2 can be 

invalidated at the discretion of the Monitoring Agency using a flag such as AM – 

Miscellaneous Void. 

Operator's Notes and Site-Specific Information



—Operator's notes can contain 

information that would call for data invalidation due to lack of sampling 

representativeness. Examples include meteorological events such as sand storms, 

temporary violations of siting criteria such as nearby construction, or operational 

difficulties with the sampling equipment. The Monitoring Agency should use its best 

judgment about the impact of site conditions on the acceptability of the data and may 

consult with EPA via the DOPO or the Regional Office if there are questions.

Shipping Records—Shipping records can be compared with CAFDF records to 

identify exposed sample sets that were held too long before shipping. Unexposed 

sampling media should not be used if more than 30 days have elapsed since the initial 

weighing of the TeflonTM filters. Sample module sets should be used at a designated 

site in the order they were received from the CSN support laboratory. 
PM2.5 CSN QAPP

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 Corrective Action Requests that Affect Data Quality

23.4.2 Automated Methods

—The Data Validation Specialist 

should review any corrective action requests in effect when the samples were 

acquired. Any corrective action requestions that could affect the data should be 

evaluated and appropriate actions taken with regard to flagging or invalidating the 

data. 

Because the data will be downloaded from the CSN laboratory’s website to the Monitoring 

Agencies in Excel spreadsheet format, automated checking methods have been implemented. 

Some automated screening methods of most use for assessing the CSN datasets include the 

following: 

 Interparameter Checks—These include ion ratio and mass balance checks that use 

data from a number of different channels. Note that each sampling site will have a 

pattern or cycle of relationships that are set up by seasonal patterns, local sources of 

PM2.5



, and geography. Samples with atypical results could be examined more closely 

as part of the validation process. 

Time Series Analysis



—This analysis is typically the examination of a set of data for a 

single observable (e.g., a particular chemical species at a certain site) acquired over a 

period of time. Time series data are often best examined graphically, and it is often 

helpful to chart related variables together on the same graph. 

Outlier Checks—Statistical outlier checks for screening PM2.5

.Once potential outliers or other suspicious data points are identified, a more in-depth 

investigation may be performed to determine it they are invalid.

chemical speciation 

concentration measurements (the actual environmental measurements, rather than 

quality assurance/quality control data) are another means of identifying potential 

problems. An environmental observation should never be invalidated simply 

because it is identified as a possible outlier by statistical techniques. Observed 

environmental concentration distributions tend to be somewhat skewed, so that a 

small number of concentrations significantly higher than the long-term average 

should be expected. Selecting the top 2 to 5 percent of values in a data set for 

investigation; however, is often a good rule of thumb for data assessment because 

high data values are sometimes the result of analytical, procedural, or calculation 

errors. 
PM2.5 CSN QAPP

Section No. 24

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24.0 Reconciliation with Data Quality Objectives (DQOs)

Results obtained must be reconciled with the requirements defined by the data user or decisionmaker, as specified by the DQOs for the project (U.S. EPA, 1994). The methods initially 

envisioned to analyze the data were based on the statistical model described fully in Data 

Quality Objectives for the Trends Component of the PM2.5

24.1 DQO for Chemical Speciation Trends

 Speciation Network (U.S. EPA, 

1999a. See http://www.epa.gov/ttn/amtic/specgen.html). This section discusses measurements of 

the MQOs and components of uncertainty that were made from 2000-2010 and compare them to 

the values that were used as preliminary assumptions to develop the original DQOs. Several 

analyses of speciation data will be summarized to illustrate if the original DQOs have been met. 

The tools that were used will be briefly discussed and references supplied so that future analyses 

can be constructed and DQOs retained or modified to suit the needs of environmental decisionmakers.

The primary DQO for the Chemical Speciation Network (CSN) was stated to be the ability to 

detect a +5 percent trend within 5 years with statistical power of 0.80. To assess whether this 

DQO has been met, it is necessary to determine if a significant time trend can be detected (or 

rejected, when there is no trend) with the requisite statistical power after 5 years of data have 

been collected. Note that by satisfying the DQO it is not necessary to show that a trend 

definitely exists or does not exist; a legitimate finding is that a trend cannot be either diagnosed 

or rejected with the required certainty. In fact, this is a likely outcome when a trend of 

intermediate size (e.g., +2 to 3 percent per year) exists or when a trend is present but highly 

variable over time. On the other hand, if all sources of error and uncertainty are particularly wellcontrolled, it may be possible to diagnose a trend smaller than +5 percent over the designated 5-

year period. To satisfy the primary DQO, it is only necessary to demonstrate that the 5-year data 

set is capable of detecting a 5 percent trend (or failing to find a trend when none exists) with the 

requisite level of confidence. This is done on a species-by-species basis. All the species used in 

the study, however, were present at a relatively high level; it is not likely that the trend detection 

DQO will be met for all chemical species. Reasons for failing to meet the trend detection DQO 

for a particular species include the following:

 Low concentration (typical of certain uncommon elements reported by energydispersive X-ray fluorescence [EDXRF]). 

 Large background variability near the analytical method’s detection limit. 

 Large proportion of “non-detects”, thus weakening the statistical power of the 

analysis. 

 High variability in concentration of the species in the environment. 

 Seasonal variability. 

 The presence of local sources (ocean, nearby construction, industrial or residential 

sources).
PM2.5 CSN QAPP

Section No. 24

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 Method or equipment changes that prematurely interrupt any five year sequences may 

introduce enough bias or other uncertainty to essentially reset the baseline year. 

 Moving a site prior to 5 years of operation probably precludes the determination of a 

trend at the initial site. The baseline year for a new trend determination is established 

by the restart of the sampler at the new location.

24.2 Interim Evaluations of Data Quality

The CSN and its constituent monitoring agencies should perform interim evaluations of data 

quality annually to assess whether the goal of meeting the DQO for trend detection can be met 

within 5 years. Here are two primary ways of performing interim evaluations of data quality: 

comparison of the project's quality control (QC) statistics against measurement quality objectives 

(MQOs) and direct modeling using the method used by EPA in the DQO study. The following 

sections describe these two approaches and suggest corrective actions that can be taken if interim 

analysis indicates that the DQO may not be met after 5 years. 

24.2.1 Evaluations Based on MQOs

Estimating the measurement error being achieved based on available QC data is perhaps the 

quickest interim measure of assessing progress toward meeting the DQO for trend detection. 

Objectives for total measurement error based on the DQO study are provided in Section 7.0 of 

this document. This quick but inexact method of data quality assessment is appropriate after 

1 year of sampling; however, analysis that is more exhaustive should be done after 2 or 3 years 

of data have been collected, as described in the next section. 

The CSN program has various measures of bias and precision available as a result of the QC data 

being taken. Measurement error must be assessed as the total end-to-end error. Some QC 

samples assess only part of the total system and thus underestimate the total error. Some of the 

QC samples that are useful in assessing total measurement error are as follows:

Flow Rate Checks—these checks are carried out at various intervals using different independent 

flow standards. Total volume is directly proportional to flow rate, and calculated concentration is 

inversely related to flow rate. Thus, a 5 percent bias error in flow rate will result in a 5 percent 

error in calculated concentration (approximately, not accounting for the effect of such an error on 

the particle size range distribution, that is, a change in the cut-point of the inlet due to a change 

in flow rate)

1

Another statistical check on flow rate uncertainty is its coefficient of variation (CV) during a 

sampling event. There are several forms of the metric; however, they generally involve 

averaging the differences in polled flow rates at specified intervals; calculating a standard 

deviation of the differences and dividing the standard deviation by the average. The CV metric is 

always stated in absolute value; consequently, the data analyst should examine the polled flow 

rates if a CV of greater than 4% is reported. If it is directional in nature in flow rate could result 

in a calculation error in concentration. If a direction is not discernable then the calculated

. 

 

1 Error due to particle size distribution will only occur if there is a distribution. If for example all the PM is PM2.5, 

the separator will have no effect on the mass that is removed—there will be none. 
PM2.5 CSN QAPP

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volume over the duration of the sampling event may be considered as an accurate estimate. If 

CV >5% and there is a significant PMcoarse (PM10-2.5) concentration in the ambient air sampled 

by that monitor, then the effect of the variable flow should be estimated. The amount of time that 

the flow is less than 10% of the design rate will be biasing the apparent PM2.5 mass on the high 

side. But the chemical constitution of the ambient air will affect other values. For example, if 

geo-crustal components dominate the PMcoarse fraction, the PM.25 mass and the XRF results 

may be the only values biased by the aberrant flow rate. Finally flow rate is only one factor in 

the estimate of total measurement error because it does not include sampling representativeness 

and analytical errors.

Analytical QC Samples Including Analysis of Standards, Duplicates, and Matrix Spikes—These 

samples provide information about the analytical component of accuracy and precision. 

Theoretical estimates of uncertainty are also available for the EDXRF data (elemental analysis). 

These estimates do not completely characterize the total measurement system because they omit 

field errors, including flow rate and sampling representativeness. 

Field Blank Results—Field blanks provide information on contamination due to handling 

operations within the laboratory and in the field, plus any of the species of interest that might 

have been present in the clean filter, for example. Normally, field blank levels should be kept 

quite small by early corrective actions and should never be allowed to become a significant 

component of total measurement error. 

Laboratory Blank Results— Laboratory blanks provide information on contamination due to 

handling operations within the laboratory plus any of the species of interest that might have been 

present in the clean filter, for example. This allows for separation of the sources of error 

associated with the laboratory versus the field portion of the process. Normally, laboratory blank 

levels should be kept quite small by early corrective actions and should never be allowed to 

become a significant component of total measurement error. Filters high in the analyte of interest 

also should never be allowed to become a significant component of total measurement error, if 

appropriate QC is being conducted. 

Collocated Sampling Results

If the network employs several makes and models of samplers that are designed to generate the 

same data, a measurement of relative bias of each make of sampler must be ascertained. It may 

be done once as was the case for the CSN samplers that were originally approved for use in the 

network. By having all the samplers together each sampler’s value would be compared to the 

— Collocated sampling may be utilized for assessing two different 

types of measurement variability. One type is when a replicate sampler is placed side-by-side 

with the primary network sampler and operated by the same technician using the same 

procedures. Data from several sampling events using this tactic provides a estimate of precision 

for a given site and sampler. If data from several sites that use the replicate pairs of the same 

sampler is compiled, it provides an estimate of general precision using that particular sampler 

along with the analytical measurements associated with the sampling. 
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average of the entire group’s values on each day they sample. 2

Another way to determine bias is with a longer term program that periodically collocates every

sampler in the network with the single make and model of sampler, which is believed to achieve 

excellent precision and to most accurately represent the parameter being measured. The so-called 

reference sampler would be operated by an independent technician and the sample would be 

analyzed by an independent laboratory, which has demonstrated rigorous quality control and 

quality assurance procedures. The results provide a measure of relative bias and if the results are 

widely disparate other issues may be revealed. This strategy was not employed by the CSN 

because the costs of running the independently samplers and the chemical speciation analyses 

that would be necessarily performed on the acquired filter samples of each sampling event. 

EPA determined that the 

originally approved samplers would meet the needs of the CSN’s monitoring and quality 

objectives. 

When starting up a new chemical speciation sampler at a site, it is a good idea to collect a 

number of duplicate samples with a replicate collocated sampler. Approximately ten valid 

duplicate samples should be considered the minimum for estimating the total error. These should 

be collected over a given season. 

Continued collocations should be done on a regular schedule so that data can be developed over 

all seasons of the year. Although the collocated sampling results provide a relatively complete 

picture of end-to-end measurement error, two components of measurement are not included. 

The first is related to the fact that collocated samples are generally analyzed in the same 

laboratory on the same day. The collocated sampling error will underestimate the true total 

measurement error by an amount related to the laboratory's day-to-day variability. This error can 

be controlled, or at least estimated, by tracking the results of daily analyses of laboratory 

standards. The variability in repeat analyses of laboratory standards should be kept small with 

respect to the targeted MQO. The CSN laboratory will provide the EPA with regular quality 

assurance (QA) summary reports that will include the necessary information for assessing this 

and other components of analytical error. This error is expected to be small, compared to the 

total measurement error.

The second error that collocated sampling omits is due to field sampling representativeness 

caused when the paired samplers are not equivalently sited. This factor can be controlled by 

careful observance of the siting requirements (for example, separation of sampler inlets by at 

least 1 meter but no more than 4 meters) as well as by using common sense in making the two 

sampler locations as equivalent as possible. Problems with siting might also be detected by 

assessing the duplicate precision for total mass. Consistent relative differences in total mass of 

more than about 10 percent may indicate a siting problem or a problem with one or both of the 

samplers exists. Low-level chemical species are likely to show larger relative variability than 

mass measurements—this is to be expected and may not indicate a problem. If siting and sampler 

 

2 Evaluation of PM2.5 Chemical Speciation Samplers for Use in the EPA National PM2.5 Chemical Speciation 

Network; EPA-454/R-01-005, July15, 2000. http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/fourcty.pdf. 
PM2.5 CSN QAPP

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operation are carried out correctly, this “error” should not be an issue with regard to total 

measurement uncertainty. 

Finally to get a better characterization of precision across the network the collocations should 

occur at multiple sites. Through the first 12 years of the CSN only 6 sites were designated for 

collocated measurements. By 2013 collocated sampling at half of these sites will be suspended 

and the replicate samplers will be rotated among other CSN sites for 1 year collocations. 

The recommended interim method for estimating total measurement error is to calculate the total 

error based on ten or more collocated measurements for each chemical species and mass. The 

following method of calculation is adapted from the method given in 40 Code of Federal 

Regulations (CFR) Part 58, Appendix A, Section 5.5.2.1: 

1. Calculate the duplicate difference for each observation, as follows: 

( ) 100

2/

×

+

− =

ii

ii

i XY

XY d

where

di

Y

 = percent difference for observation i

i

X

 = primary (station) sampler concentration value 

i = duplicate (reference) sampler concentration value. 

Note: Omit data for which the average concentration in the denominator is less than 3 times the 

method detection limit. This may result in inadequate data for evaluating some trace species.

2. Calculate the CV for a single check. The following equation for calculating the CV is 

provided in 40 CFR Part 58, Appendix A, Section 5.5.2.2: 

2

i

i

d

CV =

where

CVi

d

 = CV for observation i

i = duplicate percentage difference for observation i. 

3. Calculate the single sampler precision. The following equation is adapted from 40 

CFR Part 58, Appendix A, Section 5.5.2.3, which calculates precision for collocated 

samplers of identical type CVj represents an average error value over all observations 
PM2.5 CSN QAPP

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within a given time period for a particular chemical species (or total mass) designated 

by the subscript j: 

j

ij

j

j n

CV

i

n

CV

2

=1

∑

=

where

CVj

CV

 = pooled CV for species j over the specified time period 

i,j

n

 = CV for species j, observation i

j = number of paired observations made for species j over the time period. 

4. Compare the CVj results against the MQO. If the CV does not meet established 

criteria for a species of interest, corrective actions such as those discussed in 

Section 24.2.3 should be considered. Corrective actions should be taken promptly 

after identification of a problem; do not allow a problem to linger, otherwise 

significant amounts of data may be invalidated. 

24.2.2 Evaluations Based on Direct Assessment of the Monitoring Data 

Using the statistical model described in the DQO (U.S. EPA, 1999a), an assessment of progress 

toward meeting the DQO can be made with less than 5 years' worth of data but with reduced 

statistical power. The statistical power of the tests should be extrapolated to 5 years, based on the 

error levels computed for the preliminary data. If this extrapolation indicates that the DQO for 

detecting a trend will not be satisfied for a critical species of interest, corrective actions should 

be taken as described in the next section. It is important to do a careful assessment of the actual 

monitoring data as early in the program as possible, typically after the second or third full year of 

sampling, because the assumptions used in the DQO study may not hold at any particular CSN

site.

24.2 3 Interim Corrective Actions

If an interim assessment indicates that the DQO for trend detection is not being met, 

modification to the experimental design should be considered after any obvious measurement 

quality problems have been resolved to. Experimental design factors include site selection, 

frequency of sampling, frequency and precision of QC measurements, and frequency of 

equipment maintenance. The experimental design changes most likely to improve data quality 

are listed below in decreasing order of effectiveness: 
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 Increase the Frequency of Sampling



—The DQO study (U.S. EPA, 1999a) showed 

that 1-in-3 day sampling was adequate to meet the DQO based on the IMPROVE data 

set, while daily sampling was unnecessary and 1-in-6 day sampling was not adequate 

to meet the DQO. Increasing the sampling frequency may be helpful when 

measurement error and unexplained variability are larger than expected. Increasing 

the frequency of sampling is unlikely to affect variability attributable to seasonality. 

Add Additional Samplers



—Locating one or more additional samplers in the same 

impact area may help decrease the statistical uncertainty in the same way that 

increased sampling frequency does. In addition, locating samplers at some distance 

from one another may be effective in reducing unexplained variability due to local 

sources and siting variables.

Remedy Siting Problems



—Factors such as proximity of local sources or shielding by 

nearby buildings and other objects should be eliminated as potential sources of 

excessive variability. 

Improve QC and Maintenance

24.3 Assessing and Reporting Chemical Speciation Trends

—Measurement errors can, in principle, be reduced by 

increasing the frequency of QC checks, audits, and maintenance. Increasing the 

intensity of the QC program, however, may not be the most effective approach for 

reducing total uncertainty for two reasons: the relative contribution of measurement 

error to the total uncertainty is small, and a point of diminishing returns may be 

reached after which little improvement in measurement quality can be achieved. 

Purchasing more precise or accurate standards is unlikely to make a meaningful 

difference in overall data uncertainty. On the other hand, increasing the frequency of 

QC and maintenance can sometimes be effective at sites where a excessive numbers 

of operational problems and malfunctions are being seen and will certainly be 

effective in the latter years of network operation as the equipment ages and major 

maintenance is required. 

At the end of the first 5 years of monitoring, every monitoring agency should assess whether or 

not the DQOs and MQOs for trend detection has been met and will apply suitable statistical tests 

to test for a trend in the concentration data for all chemical species of interest. Detailed 

description of the trend assessment method is outside the scope of this QAPP. Network and 

reporting agency personnel should use methods similar to those in the DQO document (U.S. 

EPA, 1999a) as a point of departure for their analysis of concentration trends, but they are 

encouraged to use the most appropriate statistical model for their individual situations. Specific 

assistance can be obtained from OAQPS in Research Triangle Park, North Carolina. 

The interim DQO analyses should address the following questions for each analyte: 

 Was an annual trend of +5 percent or greater indicated by the analysis?

 Was an annual trend of as much as +5 percent excluded by the analysis?

 Was the statistical test inconclusive about the existence of a trend?
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 If the test was inconclusive, was the data of sufficient quality to make the assessment 

with the requisite power if a trend had been present?

24.4 Reconciling Other CSN Research Objectives

There are several important research objectives for the CSN data other than trend identification 

(U.S. EPA, 1999b). These include model development and validation, source attribution, spatial 

and seasonal characterization of aerosol distributions, state implementation plan attainment and 

strategy development, and emissions inventory. The ultimate users of the data include 

environmental researchers, regulators, and state and federal policymakers. The DQO for trend 

detection focuses on changes in concentrations of individual species over time. Other data uses, 

however, may rely on different characteristics, such as concentration ratios between species, 

seasonal variations in concentrations or concentration ratios, or the absolute concentration of 

certain chemical species at a particular point in time. Meeting the DQO for trend detection does 

not guarantee suitability of the data for another purpose. To be useful for objectives other than 

trend detection, the primary data set must be accompanied by a complete set of supporting data 

so that the user can derive information that might be applicable to other research objectives. 

24.5 References

U.S. EPA (Environmental Protection Agency). February 2006. Guidance on Systematic 

Planning Using the Data Quality Objectives Process: EPA QA/G-4, Report No. EPA/240/B06/001, U.S. EPA, Washington, DC. 

U.S. EPA (Environmental Protection Agency). February 2006. Data Quality Assessment: A 

Reviewer’s Guide, EPA QA/G-9S, Report No. EPA/240/B-06/002,

U.S. EPA (Environmental Protection Agency). 1999a. Data Quality Objectives for the Trends 

Component of the PM2.5

U.S. EPA (Environmental Protection Agency). 1999b. Particulate Matter (PM

 Speciation Network, U.S. EPA, Research Triangle Park, NC, 1999. 

(Available online on the Ambient Monitoring Technical Information Center [AMTIC] at 

http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/dqo3.pdf)

2.5

U.S. EPA (Environmental Protection Agency). July15, 2000. Evaluation of PM2.5 Chemical 

Speciation Samplers for Use in the EPA National PM2.5 Chemical Speciation Network; EPA454/R-01-005. (Available at: 

) Speciation 

Guidance Document (Final Draft), U.S. EPA, Research Triangle Park, NC. October 7, 1999. 

(Available at: http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/specfinl.pdf ) 

http://www.epa.gov/ttn/amtic/files/ambient/pm25/spec/fourcty.pdf) 
PM2.5 CSN QAPP

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Appendices 

The original appendices A-1 through A-7 have been either deleted or incorporated into the following 

appendices A-1through A-4 as appropriate due to the consolidation of the network to Metone SASS or 

SuperSASS and the URG 3000N carbon samplers. They are incorporated in this QAPP by reference to 

reduce redundancy of electronic files as well as the size of this file. Each may be reviewed and 

downloaded from EPAs Ambient Monitoring Technical Information Center on the Technology Transfer 

Network. The web address is http://www.epa.gov/ttn/amtic/spectraining.html. 

Appendix A-1: Met One SASS Field Operation Manual (PDF) (79pp, 648 kb) - 12/27/2001 

Appendix A-2: Met One SASS Standard Operating Procedure (SOP) (PDF) (12pp, 89 kb) - 7/27/2011 

Appendix A-3: Standard Operating Procedure (SOP) for the URG 3000N Sequential Particulate 

Speciation System (Sampler) (PDF) (82pp, 2.4 MB) - 8/11/2011 

Appendix A-4: The URG3000N Operator's Manual, Version 5.6 (PDF) (75pp, 5.8 MB) - 7/17/2009 

The current QAPP for the national contract service laboratory is also located at

http://www.epa.gov/ttn/amtic/specguid.html. 

National Contract Service Laboratory Quality Assurance Project Plan: Chemical Speciation of PM2.5 

Filter Samples (PDF) (95 pp, 1.1 MB) 05/11/2012 

The SOPs associated with all activities covered by the national service contract are integral to the 

operation of the Chemical Speciation Network. These SOPs are identified below and may be accessed for 

review and download at http://www.epa.gov/ttn/amtic/specsop.html. 

Note the national contract service laboratory’s QAPP and associated SOPs could change upon award of 

the next service contract. 
PM2.5 CSN QAPP

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PM2.5 CSN QAPP

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United States

Environmental Protection

Agency

Office of Air Quality Planning and Standards

Air Quality Assessment Division

Research Triangle Park, NC

EPA-454/B-12-003

June 2012