United States Office of Air Quality EPA-454/R-01-001

Environmental Protection Planning and Standards December 2000

Agency Research Triangle Park, NC 27711

Air

Quality Assurance 

Guidance Document

Final

Quality Assurance Project Plan:

PM2.5 Speciation Trends

Network Field Sampling
i

Foreword

This document represents the Quality Assurance Project Plan (QAPP) for the field operations involved

in the PM2.5 Speciation Trends Network (STN). 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 regulations and guidance are addressed in this QAPP.

This document has been reviewed by EPA Regional Offices responsible for implementing the STN in

their respective Regions, the QA Manager for EPA’s Office of Air Quality Planning and Standards

(OAQPS), the EPA Technical Monitors for the network, and the QA Manager for the contract

laboratory for the STN. It is considered acceptable that the Reporting Organizations (ROs) of the state

and local air pollution agencies use this document in lieu of writing their own field QAPP if the EPA

Regional Offices sign the approval page (see following approval page). 

Please note that from time to time, technical guidance documents, will be sent out to the Delivery Order

Project Officers, whom will distribute these to the State and Local Agencies. These should be added

to this QAPP in the office and field. Appendix A-7 is designed to accommodate these technical

guidance documents that will have updated information concerning quality assurance and quality control

issues that may affect how the STN is operated. 

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

or recommendation for use.

The following persons may be contacted concerning the contents of this document. All inquiries can be

made to: 

Dennis Mikel OAQPS-MQAG MD-14 Research Triangle Park, NC mikel.dennisK@epa.gov

James Homolya OAQPS-MQAG MD-14 Research Triangle Park, NC homolya.james@epa.gov
ii

Acronyms and Abbreviations

ADQ audit of data quality

AIRS aerometric information retrieval system

AMTIC Ambient Monitoring Technical Information Center

ANSI American National Standards Institute

APDLN air pollution distance learning network

APTI (EPA) Air Pollution Training Institute

ASQC American Society for Quality (Control)

CAA Clean Air Act

CAFDF custody and field data form

CAR corrective action request (form)

CASAC (EPA) Clean Air Scientific Advisory Committee

CFR Code of Federal Regulations

CMD (EPA) Contract Management Division

COC chain of custody

CV coefficient of variation

DBMS data base management system

DFR draft finding report

DGM dry gas meter

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

EMAD (EPA) Emissions, Monitoring, and Analysis Division

EPA Environmental Protection Agency

FR Federal Register

FR findings report

FRM Federal Reference Method (for PM2.5 sampling)

GALP good automated laboratory practices

GLP good laboratory practices

h hour

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

LSPM laboratory services program manager

M2.5 mass of PM2.5

m3 cubic meter 

MASS Mass Aerosol Speciation Sampler (URG, Corp.)

max./min. maximum/minimum (thermometer)
iii

min minute

mL milliliter

mmHg millimeters of mercury (pressure)

mo month

MQAG (EPA) Monitoring and Quality Assurance Group

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

NERL (EPA) National Exposure Research Laboratory 

NIST National Institute of Standards and Technology

NTN national trends network

OAQPS Office of Air Quality Planning and Standards

OAR (EPA) Office of Air and Radiation

ORIA (EPA) Office of Radiation and Indoor Air

PAMS photochemical air monitoring station

PE performance evaluation

PM2.5 particulate matter, 2.5 micrometer diameter

PO project officer

QA quality assurance

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 (Andersen Instruments, Inc.)

R&IE Radiation and Indoor Air

RO reporting organization

R&P Rupprecht and Patashnick Co. 

RSC regional speciation coordinator

RTI Research Triangle Institute (the STN support laboratory)

RTP Research Triangle Park (North Carolina)

SASS Spiral Ambient Speciation Sampler (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

STN (PM2.5) Speciation Trends Network

SVOC semivolatile organic compound

T & A testing and acceptance

TSA technical systems audit

USEPA United States Environmental Protection Agency

VOC volatile organic compound

XRF X-ray fluorescence

° C degree Celsius

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

Tables

Number Section Page

3-1 Distribution List 3 1

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

6-2 Checklist of PM2.5 STN Field Activities 6 4

6-3 Critical Filter and Denuder Holding and Use Times 6 9

6-4 Critical Documents and Records 6 11

7-1 MQOs for Total Measurement Error 7 3

9-1 STN Reporting Package Information 9 5

10-1 Schedule of Activities for State and Local PM2.5 STN Field Site Participants 10 2

10-2 Schedule of Activities for Contracting STN Laboratory 10 3

10-3 Proposed Sites for the PM2.5 STN 10 5

11-1 Summary of Information Provided by Speciation Sampler 11 2

11-2 STN Field Operations Corrective Actions 11 6

12-1 Explanation of STN Custody and Field Data Form 12 4

14-1 MQOs and Associated QC Activities for the PM2.5 STN 14 2

15-1 Testing and Acceptance Criteria Checklist for PM2.5 Speciation Samplers 15 2

15-2 Preventive Maintenance of STN 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 6

17-1 STN Field Equipment and Supplies 17 2

19-1 Laboratory Data Record Archival Summary 19 8

19-2 Validation Check Summaries 19 9

19-3 Raw Data Calculations 19 10

19-4 Data Transfer Operations 19 12

20-1 Assessment Summary 20 1

21-1 QA Reports to Management for STN 21 2

22-1 Data Verification Activities for the PM2.5 STN 22 2

22-2 Quality Control Data for STN Data Verification and Validation 22 6

22-3 Statistical Validation Limits for Blanks 22 10

22-4 Statistical Validation Limits for Routine Data 22 10

22-5 Mapping of Outlier Flags onto AIRS Codes 22 11

22-6 Automated Range Checks 22 11

22-7 Data Verification and Validation Summary 22 12
v

Figures

Number Section Page

4-1 STN Organization 4 2

4-2 Laboratory Technical Management and Staff Organization for STN 

Filter Analysis and Data Reporting 4 9

6-1 Summary of STN Project Operations 6 2

6-2 Sample Analysis Delivery Order Process 6 6

6-3 Diagram of Laboratory Filter Processing and Analysis Activities, 

by Filter Type 6 7

11-1 Quality Bulletin 11 4

12-1 Custody and Field Data Form for the PM2.5 STN 12 3

14-1 STN QA/QC Report Form 14 4

19-1 STN Data Flow Overview 19 2
PM2.5 STN QAPP

Section No. 1

Revision No.: 4

Date: 6/00

Page 1 of 2

1.0 QA Project Plan Identification and Approval

Title: Quality Assurance Project Plan for the PM2.5 Speciation Trends Network 

QAPP Category: Category 1

By signing below, the monitoring agency commits to implement the latest version of the Quality

Assurance Project Plan referenced above and the EPA approves this monitoring agency QAPP

submittal.

State/Local/Tribal Agency

Print Name:________________________ Signature:_________________________ Date:_________

 PM2.5 Monitoring Coordinator 

Print Name:________________________ Signature:_________________________ Date:_________

 Quality Assurance Officer 

Print Name:________________________ Signature:_________________________ Date:_________

 Air Program Director

EPA Regional Approval

Print Name:________________________ Signature:_________________________ Date:_________

 PM2.5 Monitoring Coordinator

Print Name:________________________ Signature:_________________________ Date:_________

 Quality Assurance Manager

Print Name:________________________ Signature:_________________________ Date:_________

 Project Officer

Print Name:________________________ Signature:_________________________ Date:_________

 Grants, Audits & Procurement 

 Program Director
PM2.5 STN QAPP

Section No.2

Revision No.: 4.1

Date: 12/00

Page 1 of 4

2.0 Table of Contents

Section Page Revision Date

Foreword i 4.1 12/00

Acknowledgments ii 4.1 12/00

Acronyms and Abbreviations iii 4.1 12/00

Tables vi 4 6/00

Figures vii 4 6/00

1.0 QA Project Plan Identification and Approval 1/1 4.1 12/00

2.0 Table of Contents 1/6 4.1 12/00

3.0 Distribution 1/4 4.1 12/00

4.0 Project/Task Organization 1/10 4.1 12/00

4.1 Trends Network Coordination Activities 2/10

4.2 Trends Network Field Site Activities Organization 6/10

4.3 Trends Network Laboratory Activities Organization 7/10

5.0 Background and Problem Definition 1/3 4.1 12/00

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 4.1 12/00

6.1 Description of Work to be Performed 1/11

6.2 Field Activities 3/11

6.3 Laboratory Activities 5/11

6.4 Schedule of Activities 8/11

6.5 Project Assessment Techniques 10/11

6.6 Project Records 10/11

7.0 Quality Objectives and Criteria For Measurement Data 1/4 4.1 12/00

7.1 Data Quality Objectives Process 1/4

7.2 Development of DQOs for the PM2.5 Chemical STN 1/4

7.3 Measurement Quality Objectives 2/4

7.4 References 4/4

8.0 Special Training Requirements/Certification 1/3 4.1 12/00

8.1 Training 1/3

8.2 Certification 3/3

8.3 Contacts for More Information 4/3

9.0 Documentation and Records 1/6 4.1 6/00

9.1 Information in the Management and Organization 

Reporting Package 1/6
2.0 Table of Contents (continued)

Section Page Revision Date

PM2.5 STN QAPP

Section No.2

Revision No.: 4.1

Date: 12/00

Page 2 of 4

9.2 Information in the Field Operations Reporting Package 1/6

9.3 Information in the Laboratory Operations Reporting Package 3/6

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 1/8 4.1 12/00

10.1 Scheduled Project Activities, Including Management Activities 1/8

10.2 Rationale for the Design 3/8

10.3 References 8/8

11.0 Sampling Methods Requirements 1/7 4.1 12/00

11.1 Sample Collection and Preparation 1/7

11.2 Sampling/Measurement System Corrective Action Process 3/7

11.3 Avoiding Sample Contamination; Temperature and 

Holding Time Requirements 5/7

12.0 Sample Handling and Custody Requirements 1/6 4.1 12/00

12.1 Introduction 1/6

12.2 Presampling Sample Handling and Custody Procedures 1/6

12.3 Postsampling Sample Handling and Custody Procedures 5/6

12.4 Filter and Sample Archival in the STN Laboratory 6/6

13.0 Analytical Methods Requirements 1/1 4.1 12/00

14.0 Quality Control Requirements 1/8 4.1 12/00

14.1 QC Checks 3/8

14.2 QC Samples 5/8

14.3 Collocated Samplers 5/8

14.4 Calculations of Accuracy, Bias, Precision, and Completeness 6/8

14.5 References 8/8

15.0 Instrument/Equipment Testing, Inspection, and Maintenance Requirements 1/4 4.1 12/00

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 4.1 12/00

16.1 Overview 1/6

16.2 Calibration and Verification of Field Instrumentation 1/6

16.3 Calibration and Verification of Laboratory Instrumentation 3/6
2.0 Table of Contents (continued)

Section Page Revision Date

PM2.5 STN QAPP

Section No.2

Revision No.: 4.1

Date: 12/00

Page 3 of 4

17.0 Inspection/Acceptance for Supplies and Consumables 1⁄2 4.1 12/00

17.1 Purpose 1⁄2

17.2 Critical Supplies and Consumables 1⁄2

17.3 Acceptance Criteria 1⁄2

17.4 Tracking and Quality Verification of Supplies and Consumables 2/2

18.0 Data Acquisition Requirements (Nondirect Measurements) 1 /2 4.1 12/00

18.1 Acquisition of Nondirect Measurement Data 1 /2

19.0 Data Management 1/12 4.1 12/00

19.1 Overview 1/12

19.2 Data Management Activities at the STN Laboratory 3/12

19.3 Data Management Activities at the RO 3/12

19.4 Recommended Data Management Practices 5/12

19.5 Data Validation 7/12

19.6 Data Transformations 10/12

19.7 Data Transmittal 11/12

19.8 Data Reduction 11/12

19.9 Data Analysis 11/12

19.10 Data Storage and Retrieval 11/12

20.0 Assessment and Response Actions 1/7 4.1 12/00

20.1 Types of Assessments 1/7

20.2 Assessment Frequency 1/7

20.3 Acceptance Criteria 2/7

20.4 Assessment Schedules 2/7

20.5 Assessment Personnel 2/7

20.6 Assessment Reports 5/7

20.7 Implementation of Response Actions 6/7

20.8 References 7/7

21.0 Reports to Management 1/5 4.1 12/00

21.1 NAMS Reporting 1/5

21.2 Additional Quality-Related Reports for the STN 4/5

22.0 Data Review, Validation, and Verification Requirements 1/12 4.1 12/00

22.1 Data Verification and Validation Responsibilities 1/12

22.2 Corrective Action Reporting Process 1/12

22.3 Use of QC Information for Verification and Validation 5/12

22.4 Use of Calibration Information for Verification and Validation 5/12

22.5 Level 0 Verification 7/12

22.6 Level 1 Data Validation 8/12

22.7 Data Screening Techniques used by RTI 9/12

22.8 Treatment of Deviations from Requirements 11/12

22.9 Verification and Validation Criteria: Field Component 12/12
2.0 Table of Contents (continued)

Section Page Revision Date

PM2.5 STN QAPP

Section No.2

Revision No.: 4.1

Date: 12/00

Page 4 of 4

23.0 Validation and Verification Methods 1/4 4.1 12/00

23.1 Interorganizational Responsibilities for Data Validation 1/4

23.2 Personnel Responsibilities within the Reporting Organization 2/4

23.3 Completion of Level 0 Data Verification and Validation 2/4

23.4 Identification of Outliers and Data Flagging Techniques 3/4

24.0 Reconciliation with Data Quality Objectives 1/7 4.1 12/00

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 Chemical STN Research Objectives 6/7

24.5 References 7/7

Appendix A

A-1 SOP5000 STN Condensed Standard Operating 

Procedure for Field Installation Of PM2.5 Speciation 

Samplers 1 9/99

A-2 SOP5100 STN Condensed Standard Operating 

Procedure For The Met One SASS 1 9/99

A-3 SOP5200 STN Condensed Standard Operating 

Procedure For The Andersen RAAS 1 9/99

A-4 SOP5300 STN Condensed Standard Operating 

Procedures For The URG MASS 400 And 

URG MASS 450 1 9/99

A-5 SOP5400 STN Packing Instructions for the Speciation Sampler 1 12/00

Modules

A-6 CY-2001 Normal and Alternate Sampling Schedule for the Speciation Trends

Network 1 12/00

A-7 Technical Guidance Document Updates 1 12/00
PM2.5 STN QAPP

Section No. 3

Revision No.: 4.1

Date: 12/00

Page 1 of 4

3.0 Distribution

A hardcopy of this QAPP has been distributed to the individuals listed in Table 3-1. The Regional Speciation

Coordinators (RSCs) will be responsible for distributing the QAPP to each field site and regional analysis laboratory

in the environmental data operations of the STN. The RSCs may also want to provide a copy of this QAPP to their

Regional QA Managers. Upon completion, the QAPP for the PM2.5 STN will be available on the EPA’s Ambient

Monitoring Technical Information Center (AMTIC) Web site.

TABLE 3-1. DISTRIBUTION LIST

Name Address Phone No. Electronic Mail

OFFICE OF AIR QUALITY PLANNING & STANDARDS

Vickie Presnell

USEPA

Office of Air Quality Planning &

Standards

MQAG (MD-14)

RTP, NC 27711

(919) 541-7620 presnell.vickie@epa.gov

James Homolya

USEPA

Office of Air Quality Planning &

Standards

MQAG (MD-14)

RTP, NC 27711

(919) 541-4039 homolya.james@epa.gov

Joann Rice

USEPA

Office of Air Quality Planning &

Standards

MQAG (MD-14)

RTP, NC 27711

(919) 541-3372 rice.joann@epa.gov

Dennis Mikel

USEPA

Office of Air Quality Planning &

Standards

MQAG (MD-14)

RTP, NC 27711

(919) 541-5511 mikel.dennisK@epa.gov

Michael Papp

USEPA

Office of Air Quality Planning &

Standards

MQAG (MD-14)

RTP, NC 27711

(919) 541-2408 papp.michael@epa.gov

CONTRACTING ANALYSIS LABORATORY

R.K.M. Jayanty

Research Triangle Institute

3040 Cornwallis Road

P.O. Box 12194

RTP, NC 27709

(919) 541-6483 rkmj@rti.org

Robert Perkins

Research Triangle Institute

3040 Cornwallis Road

P.O. Box 12194

RTP, NC 27709

(919) 541-6800 rlp@rti.org
TABLE 3-1. (continued)

PM2.5 STN QAPP

Section No. 3

Revision No.: 4.1

Date: 12/00

Page 2 of 4

Name Address Phone No. Electronic Mail

James Flanagan

Research Triangle Institute

3040 Cornwallis Road

P.O. Box 12194

RTP, NC 27709

(919) 541-7739 jamesf@rti.org

DELIVERY ORDER PROJECT OFFICERS

M. Kantz

Region 2 (East)

USEPA-Region 2

Raritan Depot / MS103

2890 Woodbridge Avenue

Edison, NJ 08837-3679

(732) 321-6690 kantz.marcus@epa.gov

P. Schraufnagel

Region 5 (Midwest)

USEPA-Region 5

77 West Jackson Blvd. / AR-18J

Chicago, IL 60604-3507

(312) 886-5955 schraufnagel.patricia@epa.gov

K. Wang

Region 8 (West)

USEPA-Region 8

999 18th Street / 8TMS-Q

Suite #500

Denver, CO 80202-2466

(303) 312-6738 wang.kenneth@epa.gov

REGIONAL SPECIATION COORDINATORS

Region 1

RSC

Mary Jane

Cuzzupe

USEPA-Region 1

New England Regional Laboratory

60 Westview Street

Lexington, MA 02421

(781) 860-4383 cuzzupe.maryjane@epa.gov

Region 2

RSC

Clinton Cusick

USEPA-Region 2

Raritan Depot / MS103

2890 Woodbridge Avenue

Edison, NJ 08837-3679

(908) 321-6881 cisocl/clinton@epa.gov

Region 3

RSC

Theodore Erdman

USEPA-Region 3

1650 Arch St

Philadelphia, PA 19103-2029

(215) 597-1193 erdman.ted@epa.gov

Region 4

RSC

Herb Barden

Richard Guilliot

USEPA-Region 4

Science and Ecosystem Support

Division

980 College Station Road

Athens, GA 30605-2720

(706) 355-8737

(404) 562-9050

barden.herbert@epa.gov

guiillot.richard@epa.gov

Region 5

RSC

Gordon Jones

USEPA-Region 5

77 West Jackson Blvd. / AR-18J

Chicago, IL 60604-3507

(312) 353-3115 jones.gordon@epa.gov
TABLE 3-1. (continued)

PM2.5 STN QAPP

Section No. 3

Revision No.: 4.1

Date: 12/00

Page 3 of 4

Name Address Phone No. Electronic Mail

Region 6

RSC

Kuenja Chung

USEPA-Region 6

First Interstate Bank Tower at Fountain

Place

1445 Ross Avenue

Dallas, TX 75202-2733

(214) 665-8345 chung.kuenja@epa.gov

Region 7

RSC

Mike Davis

USEPA-Region 7

ENSV / EMWC

25 Funston Road

Kansas City, KS 66115

(913) 551-5081 davis.michael@epa.gov

Region 8

RSC

Joe Delwiche

USEPA-Region 8

999 18th Street / 8P2-A

Suite #500

Denver, CO 80202-2466

(303) 312-6448 delwiche.joseph@epa.gov

Region 9

RSC

Matthew Plate

USEPA-Region 9

75 Hawthorne St. / PMD-3

San Francisco, CA 94105

(415) 744-1493 plate.matthew@epa.gov

Region 10

RSC

Karen Marasigan

USEPA-Region 10

1200 Sixth Ave. / ES-095

Seattle, WA 98101 (206) 553-1792 marasigan.karen@epa.gov

MINITRENDS STATE CONTACTS

Tom Moore

Arizona

Arizona Department of Environ. Quality

Air Quality Division

3033 North Central Avenue, 5th Floor 

Phoenix, AZ 85012

(602) 207-2353 moore.tom@ev.state.az.us

Tom Tamanini

Florida

Hillsborough County EPC

1410 N. 21st Street

Tampa, FL 33605

(813) 272-5530 tamanini@epcjanus.epchc.org

Bob Lamorte

Illinois

Cook County Dept. of Environmental

Control

Maybrook Civic Center

1500 Maywood Drive

Maywood, IL 60609

(708) 865-6184 ccdects@wwa.com

Jerry Sheehan

Massachusetts

State of Massachusetts DEP

Air Quality Bureau

37 Shattuck Street

Lawrence, MA 01843

(978) 975-3215,

ext. 309

jerry.sheehan@state.ma.us

Bern Johnson

Missouri

State of Missouri

DNR/DEQ/APCP

P.O. Box 176

Jefferson City, MO 65102-0176

(573) 526-2027 nrjohnb@mail.dnr.state.mo.us
TABLE 3-1. (continued)

PM2.5 STN QAPP

Section No. 3

Revision No.: 4.1

Date: 12/00

Page 4 of 4

Name Address Phone No. Electronic Mail

Dirk Felton

New York

New York State Dept. of Environmental

Conservation

Division of Air Resources

Bureau of Air Quality Surveillance

80 Wolf Road, Room 403

Albany, NY 12233-3256

(518) 457-9137 hdfelton@gw.dec.state.ny.us

Daniel E. Harman

North Dakota

North Dakota Department of Health

Environmental Engineering

1200 Missouri Avenue

P.O. Box 5520

Bismarck, ND 58506-5520

(701) 328-5188 dharman@state.nd.us

Steve Aalbers

Oregon

Oregon Department of Environmental

Quality

811 SW Sixth Avenue

Portland, OR 97204

(503) 229-6798 aalbers.steven@deq.state.or.us

Norman Glazer

Pennsylvania

Technical Services Group

Air Management Services

1501 East Lycoming Street

Philadelphia, PA 19124

(215) 685-1085 norman.glazer@phila.gov

Ed Michel

Texas

TNRCC

P.O. Box 13087, Mail Code 165

Austin, TX 78711-3087

(512) 239-1384 emichel@tnrcc.state.tx.us

Robert Neal

Olson

Utah

State of Utah DEQ

Division of Air Quality

2861 Parkway Blvd.

West Valley City, UT 84119

(801) 877-0764 rolson@deq.state.ut.us

Jim Frost

Washington

Washington Department of Ecology

Air Quality Program

P.O. Box 47600

Olympia, WA 98504-7600

(425) 649-7108 JFR0461@ecy.wa.gov
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 1 of 10

4.0 Project/Task Organization

This section provides all parties involved in the Speciation Trends Network with a clear understanding

of their roles and the lines of authority, communication, and reporting for the project.

The organization of the STN involves three interacting entities: Federal and Regional EPA offices, state

and local air monitoring and reporting organizations, and one or more contracting laboratories to service

the collection 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 is

a shared responsibility 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.

Information on the STN’s organization is first presented from the perspective of all involved agencies

and contractors. Section 4.1 and Figure 4-1 provide a unified view of the network’s operating

structure and lines of communication and reporting. Block A of Figure 4-1 points out the network’s

coordination activities, led by EPA’s Office of Air Quality Planning and Standards with advice from the

Chemical Speciation Workgroup, the Clean Air Scientific Advisory Council (CASAC), the Expert

Panel on the EPA Speciation Network, and a group of advisors from EPA’s National Exposure

Research Laboratory (NERL). The Quality Assurance (QA) Manager, the network’s Project Officer

(PO), the EPA-(RSCs, and three Delivery Order Project Officers (DOPOs) are also included in the

network’s planning and coordination activities component.

Section 4.2 focuses on the roles of the EPA Regional QA Offices and the State and local agencies that

will operate the 54 sampling sites on a day-to-day basis. Block B of Figure 4-1 shows the field

activities the State and local agency STN sampling and QA/Quality Control (QC) personnel will

perform and their lines of communication to the DOPOs, the STN PO, and the contract laboratory.

Section 4.3 and Figure 4-2 discuss the contracting laboratory’s managerial and technical organization

and roles and illustrate the laboratory’s interactions with the EPA DOPOs and PO and with the State

and local agencies, which will operate the samplers and ship the samples to the laboratory. Block C of

Figure 4-1 shows the contract laboratory and the EPA Regional QA Laboratories. 
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 2 of 10

PM2.5 Chemical 

Speciation Workgroup

PM2.5 STN Coordination Activities

OAQPS Group Leader 

R. Scheffe

Project Manager

J. Homolya

 Advisors

--CASAC

--Expert Panel

--ORD/NERL

P. Solomon

Regional Offices 

Delivery Order

Project Officers

East: M. Kantz

Midwest: P. Schraufnagel

West: K. Wang

PM2.5 STN

Project Officer

V. Presnell

Speciation 

Network QA 

Coordinator

D. Mikel

Trends Network Field Activities

State and Local

Agencies 

Trends Network Laboratory Activities

Chemical Speciation

 Contract Laboratory (RTI)

Program Manager R. Jayanty

Lab QA Auditing 

and Technical 

Assistance ORIA 

-NAREL

M. Clark 

A

B C

Field QA 

Assessments

E. Braganza

Figure 4.1 STN Organization

4.1 Trends Network Coordination Activities

The STN is made up of three interactive working groups, as illustrated in Figure 4-1. Block A of this

figure includes the PM2.5 Chemical Speciation Workgroup, the OAQPS network coordination office,

three advisory groups, the QA Manager, and the PO and DOPOs. These groups assist in

coordinating, advising, planning, and managing the activities of the STN field and laboratory activities.
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 3 of 10

4.1.1 PM2.5 Chemical Speciation Workgroup

The PM2.5 Chemical Speciation Workgroup was formed to provide input and review of all aspects of

the chemical speciation program, which includes the 54 trends national air monitoring station (NAMS)

network sites and up to 250 nonroutine State and local air monitoring station (SLAMS) sampling sites. 

Members of the group include personnel from EPA OAQPS, EPA Regions, the EPA Office of

Research and Development’s (ORD’s) NERL, and State and local air monitoring organizations. This

workgroup meets monthly or more often to discuss various planning, operational, and QA issues. 

Meetings are organized and planned by OAQPS. The workgroup acts in an advisory role and has

assisted (and will continue to assist) in the development and review of the speciation network’s

implementation plan, field and laboratory standard operating procedures (SOPs). In January 2001, a

new QA workgroup will form that will oversee the development of QAPP, Quality Management Plan

(QMP) and other QA guidance documents.

4.1.2 Office of Air Quality Planning and Standards Coordination Office

OAQPS has oversight concerning the quality of the Nation’s ambient air data. OAQPS has developed

specific regulations for the development of a quality system as 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 STN. OAQPS will ensure the orderly development and

operation of this network through the following activities:

< Coordinating and overseeing the STN

< Providing a contractual vehicle for the manufacture, procurement, and distribution of PM2.5

speciation samplers and their components

< Working with the EPA Regions and State/local organizations to determine the best sampling

locations

< Providing a contract vehicle for a laboratory to support the field sites and provide filter analysis

and associated functions

< Developing documents for the STN, including the strategic plan for the quality system of trends

sites, SOPs for field sites and laboratory operations, and the QAPP

< Developing field and laboratory personnel requirements and 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 Aerometric Information

Retrieval System (AIRS) database

< 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

< Initiating and instituting a communications network and acting as a liaison to groups working on

the STN data sets
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 4 of 10

< Interacting with Regional, State, and local agency personnel and the contracted laboratory

concerning the setup and operation of the STN and its data results

< Ensuring the success of the network by coordinating various 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

Monitoring and Quality Assurance Group (MQAG) within the Emissions, Monitoring, and Analysis

Division (EMAD) is ultimately responsible for the implementation of the Speciation Trends Network. 

This includes most of the technical components (with support from ORD, Regional offices and

laboratories, and State and local agencies) and the resource estimates underlying program

implementation. The QA Coordinator (QAC) will provide guidance and oversight to the development

of the STN quality system, including this QAPP. Resource guidance necessary for the State and Tribal

Assistance Grants (STAG) distribution is coordinated through the Planning, Resources, and Regional

Management staff within OAQPS. In addition, the Information Transfer and Program Integration

Division (ITPID) is responsible for the AIRS data management system.

4.1.2.1 Speciation Trends Network Quality Assurance Coordinator

The STN-QAC, Mr. Dennis Mikel, will coordinate the implementation of the quality system of the

STN. The QAC will:

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

their approval 

< Ensure that RTI’s SOPs are reviewed and updated as required

< Coordinate with the QA workgroup, the Regional QA laboratories and others to ensure that

periodic systems reviews and performance reviews of the field and laboratory activities are

accomplished.

< periodic of the field and laboratory activities 

4.1.2.2 Speciation Trends Network Project Manager 

 Mr. James Homolya is the delegated OAQPS program manager of the STN. He is responsible for the 

OAQPS activities that are implemented as part of normal data collection activities. His responsibilities

include:

Ccommunication with EPA Project Officers and EPA QA personnel on issues related to routine

sampling and QA activities;

Cunderstanding EPA monitoring and QA regulations and guidance, and ensuring all key personnel

understand and follow these regulations and guidance; 

Creviewing acquisition packages (contracts, grants, cooperative agreements, inter-agency

agreements) to determine the necessary QA requirements.

Cdeveloping budgets and providing program costs necessary for EPA allocation activities
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 5 of 10

Censuring that all personnel involved in environmental data collection have access to any training or

QA information needed to be knowledgeable in QA requirements, protocols, and technology;

Crecommending required management-level corrective actions.

4.1.3 Advisory Panels

Three advisory panels will consult with OAQPS on technical matters related to the STN. These panels

are the Clean Air Scientific Advisory Committee, the Speciation Expert Panel, and a panel of

ORD/NERL technical experts.

Clean Air Scientific Advisory Committee—This committee is a subcommittee of the Science

Advisory Board (SAB) and reports directly to the SAB administrator. It will serve as the principal

review body for the PM2.5 monitoring program and will emphasize review of the speciation network. 

This committee will interact with the OAQPS coordination office.

Expert Panel on Speciation—The Expert Panel on Speciation was formed to advise OAQPS on

structural and technical matters related to the PM2.5 speciation network. It is composed of recognized

technical experts in the fields of network monitoring strategy, sampling and monitoring methods for

PM2.5, physical and chemical characterization of fine particles, and data analysis and interpretation. 

Members of the Speciation Expert Panel are Drs. Petros Koutrakis (chair), Tom Cahill, Phil Hopke,

Lara Gundel, and John Ondov, and Mr. Robert Stevens. This panel has focused on review of the

guidance documents for the speciation network and instrumentation. It will report to and interact with

the OAQPS STN coordinating office.

ORD/NERL Expert Panel—This panel is composed of scientists and engineers in EPA’s ORD, in

particular the NERL. Members of this panel (including Drs. Russel Weiner and Paul Solomon) led

efforts to design, test, and approve PM2.5 mass samplers as Federal Reference Methods (FRMs). 

They have also bench- and field-tested most of the available PM2.5 speciation samplers. This panel will

be called upon for expert advice on technical and operational aspects of the speciation samplers,

handling samples, and laboratory analyses of PM2.5. They will communicate with the OAQPS

coordinating office. 

4.1.4 Speciation Trends Network Project Officer

The STN Project Officer (PO), Ms. Vickie Presnell, is with EPA/OAQPS. She will be the liaison

between the EPA Contracts Management Division and the various contractors and vendors. The PO

will interact with others in OAQPS, EPA Contracts Management Division personnel, the DOPOs, and

the contract laboratory’s Services Program Manager to ensure contract details are followed, including

the submittal and review of required draft and final semi-annual data summary reports from the

contracted laboratory. 
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 6 of 10

4.1.5 Regional Speciation Coordinator

The Regional Speciation Coordinator (RSC) will receive PM2.5 speciation analytical needs requests

from State or local agencies. The RSC then consolidates all requests received from States within his or

her region and submits them to the DOPO for that region. The RSC interacts with the State and local

agencies and provides assistance on field related QA issues.. Any special equipment or nonroutine

analytical needs requested by the monitoring agencies are relayed to the STN Project Office for action. 

The names of the RSCs are listed in Section 3.0, Table 3-1.

4.1.6 Delivery Order Project Officer

The Delivery Order Project Officer (DOPO) will consolidate the requests for sampling media and

sample analysis received from the RSCs. A DOPO will be assigned to the East (Regions 1-4 and

Puerto Rico), Midwest (Regions 5-7), and West (Regions 8-10) of the United States. Once the STN

is in full operation, the delivery order process is expected to become fairly routine because all sites in

this network will request analyses of specific analytes on samples collected every third day for a number

of years. The DOPO will communicate with the STN Project Officer and with the laboratory

contracted for analysis of filters and other sampling media. The DOPO will also review the monthly

analytical data packages from the contracting laboratory, ensure they are complete, and, after approval,

make arrangements for payment of the invoice for the various delivery orders.

EPA Contracts Management Division—The Contract Management Division (CMD) is located within

the Office of Acquisition Management (OAM). CMD is responsible for all communications with

vendors and extramural contract organizations. For the STN, it will:

< Provide a Contract Officer to represent the government.

< Develop national contracts for speciation sampler purchases, some filter purchases, sample

shipping, and laboratory support and analyses of speciation sampler filters.

< Communicate with OAQPS to provide the above services.

4.2 Trends Network Field Site Activities Organization

Personnel from State and local agencies will install speciation samplers at NAMS sites, operate the

sites, and promptly ship samples to the contract laboratory to ensure schedules are met. State or local

personnel will also implement QC procedures as given in the SOPs for sampler operation and sample

shipping. Another line of communication from the States will be to the DOPO and the RSC. Dialogues

concerning sampling equipment and laboratory supply or sample analysis problems occur here. 

Interested State and local personnel may also participate in Chemical Speciation Workgroup

discussions. 

State or local site operators and supervisors should communicate directly with the contracted sample

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

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 7 of 10

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

Regional QA laboratories for technical assistance and QA services. The State or local site operations

and records will be subject to systems and performance reviews, which will be coordinated through the

EPA’s Speciation Trends Network QA Manager. 

4.2.1 Organization for Routine Field Sampling Operations

The State and local air monitoring agencies are responsible for day-to-day operation of STN 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

< Purchase, receipt, acceptance testing, and installation of sampler, calibration equipment, and

meteorological equipment

< 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 

< Interactions with STN network management personnel. Participation in external QA activities. 

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

Quality assurance activities supporting the STN sites will be arranged through the QA Manager at each

State or local agency. QA personnel will be identified prior to field data collection and will be assigned

and organized to accomplish the following tasks, among others:

< Implementation of the quality system for the STN

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

< Site inspections and review of procedures to ensure specified QA/QC checks are being made

and measurements systems are in control. Issuance of corrective action memoranda and

monitoring of follow-up actions.

< Participation in monthly validation of draft data sets received from the contract laboratory

< Arrangement for and participation in QA activities called for by EPA Regional offices.

4.3 Trends Network Laboratory Activities Organization

Block C of Figure 4-1 illustrates the organization of the trends network laboratory activities sector. 

Laboratory activities will include QA related work by the EPA Office of Radiation and Indoor Air

(ORIA) and the EPA Region 1 Laboratory, and routine laboratory work by Research Triangle

Institute (RTI), the contracted field site supply and filter analysis laboratory. 
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 8 of 10

4.3.1 EPA QA Laboratories

EPA’s Office of Radiation and Indoor Air (ORIA) laboratories in Montgomery, Alabama and Las

Vegas, Nevada will be working in concert with the EPA Region 1 Laboratory, and OAQPS. 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

analysis laboratory

< Provide QA auditing and technical assistance to the field sites and to the contracting analysis

laboratory.

The EPA QA laboratories will be establish lines of communication with the following:

< Access to the STN PO to send and receive information concerning the performance of the

contracted laboratory and the status and quality of operations at the field site/contract

laboratory interface

< Contact with OAQPS coordinators and technical monitors, their advisory panels, and the QA

office

< Interactions with the contracted laboratory to conduct systems and performance reviews.

4.3.2 Contracted Filter Analysis Laboratory Organization

Figure 4-2 illustrates the organization of management, QA, and technical staff for the PM2.5 analysis

laboratory.

Management Organization—The PM2.5 speciation analysis laboratory is headed by a Laboratory

Services Program Manager (LSPM) and a Deputy Manager. The LSPM receives site servicing

delivery orders from the EPA DOPOs and is the official contact person for sending or receiving

sampling media and for release of analytical and other data sets. The management office will oversee

activities of the technical laboratories and the data management office. The LSPM will also receive and

respond to quality systems findings provided by the laboratory QA Manager and staff as well as to

external audit reports. 

Quality Assurance Organization—The laboratory’s QA Office is staffed by a QA Manager (QAM),

a Deputy QA Manager, and support staff. The QA Manager interacts with each of 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 LSPM for review and action. This office

summarizes QA activities for inclusion in the monthly reports to EPA. The QA Office also prepares

and updates the laboratory QAPP and associated SOPs. 
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 9 of 10

Technical Organization—The laboratory is composed of seven entities that will provide the following

analytical services and data report packages to STN sites:
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 11 of 10

< Sample Handling and Archival Laboratory (SHAL). Supply each Speciation Trends

Network site with all necessary sampling supplies to include coated denuders, sampling filter

media, assembled sampling modules, shipping containers, and documentation paperwork. (The 

laboratory will use hardware purchased by the State or local organization; the contractor will

supply only the filters.)

< Gravimetric and Microscopy Laboratories. PM2.5 mass by microbalance determination. 

Scanning electron and optical microscopy studies of particles.

< Elemental Analysis Laboratory. Elements by energy-dispersive X-ray fluorescence

(EDXRF) determination.

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

< Carbon Species and Semivolatile Organic Carbon Compounds Laboratory. Carbon

species by elemental carbon/organic carbon (EC/OC) analysis. Determination of semivolatile

organic compounds (SVOC’s) as needed.

< Denuder Refurbishment Laboratory. Denuder refurbishment. 

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

includes issuance of monthly and quarterly data sets to State/local agencies and to the EPA

DOPO and entry of validated data to the AIRS database system.

Details on these activities can be found in the companion laboratory QAPP for this program. 
PM2.5 STN QAPP

Section No. 4

Revision No.: 4.1

Date: 12/00

Page 10 of 10

EPA Project Officer

and

Delivery Order Project Officers

Subcontractor

C. Lytle, Chester LabNet

Technical Advisor

R. W. VanderpoolXRF Consultants

J. Cooper

Cooper Environmental Services

RTI Services Program

 Manager

R. K. M. Jayanty

RTI Deputy Services Program

 Manager

R. L. Perkins

Quality Assurance Manager

J. B. Flanagan

Deputy Quality Assurance Manager

C. E. Tatsch

Support Staff

Sample

Handling and

Archiving Lab

(SHAL)

Manager

J. A. O’Rourke

Support Staff

Gravimetric and

Microscopy

Labs

 Technical

Supervisor

R. L. Perkins

Support Staff

Elemental

Analysis Lab

 Technical

Supervisor

W. F.

Gutknecht

Support Staff

J. J. Giglio

Subcontractor:

Chester

LabNet

Cations/Anions

Lab

 Technical

Supervisor

E. D. HardisonSupport Staff

Carbon

Species and

SVOC Lab

 Technical

Supervisors

M. R. Peterson

J. H. Raymer

Support Staff

Denuder

Refurbishment

Lab

 Technical

Supervisor

W. C. Eaton

Support Staff

Data

Management

Office

Technical

Supervisor

E. E. RickmanSupport Staff

Services

Program

Manager

Services

Program

Manager

Send/Receive

Sampling

Media

• State• Local• EPA Regions

Data Set

Releases

• State/Local • EPA DOPO• AIRS

Figure 4-2. Laboratory technical management and staff organization for STN filter analysis and data reporting.
PM2.5 STN QAPP

Section No. 5

Revision No.: 4.1

Date: 12/00

Page 1 of 3

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 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 CAA also 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 recently reviewed the air quality criteria

and National Ambient Air Quality Standards (NAAQS) for PM and epidemiological evidence that

shows 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 :m, referred to

as PM2.5) and the regulatory requirements for monitoring the chemical composition of these particles. 

In meeting the requirements to monitor and gather data on the chemical makeup of these particles, EPA

is establishing a chemical speciation network consisting of approximately 300 monitoring sites. These

sites will be placed at various NAMS and SLAMS across the Nation. It is currently anticipated that

54 of these chemical speciation sites will be used to determine, over a period of several years, trends in

concentration levels of selected ions, metals, carbon species, and organic compounds in PM2.5. Further

breakdown on the location or placement of the trends sites requires that approximately 20 of the

monitoring sites be placed at existing Photochemical Assessment Monitoring Stations (PAMS). The

placement of the remaining trends sites will be coordinated by EPA, the Regional offices, and the State

and local agencies. Locations will be primarily in or near larger Metropolitan Statistical Areas (MSAs). 

The remaining chemical speciation sites will be used to enhance the required trends network and to

provide information for developing effective State implementation plans (SIPs). This QAPP focuses on

required measures for ensuring that data of adequate quality are provided by the 54 trends network

sites.

5.2 Problem Definition

The STN is a component of the National PM2.5 Monitoring Network. Although the STN is intended to

complement the activities of the much larger gravimetric PM2.5 measurements network component

(whose goal is to establish if NAAQS standards are being attained), STN data will not be used for

attainment or nonattainment decisions. The programmatic objectives of the STN network are:

< Annual and seasonal spatial characterization of aerosols;

< Air quality trends analysis and tracking the progress of control programs;

< Compare the chemical speciation data set to the data collected from the IMPROVE

network; and 

< Development of emission control strategies.
PM2.5 STN QAPP

Section No. 5

Revision No.: 4.1

Date: 12/00

Page 2 of 3

Stakeholders in the STN will be those at EPA seeking to determine concentration trends of PM2.5

chemical species over a period of 3 or more years and decision-makers at State and local levels who

will use the data as input to models and for development of emission control strategies and

determination of their long-term effectiveness. Other users will be public health officials and

epidemiological researchers. However, expectations for data sets from the STN must be put in

context. A number of limitations are recognized, (for instance, the 24-h integrated sample approach,

taken every 3rd day, is not suitable for determination of diurnal patterns and may have limited use to

those who study acute health effects). EPA recognizes these data use limitations and limitations on the

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

requirements, and methods for speciation sampling may need to be adjusted in the future.

5.3 PM2.5 Speciation Sampling Techniques and Ongoing Research

The samplers will have the capability of collecting 24-h integrated samples. The three commercial

sampler designs currently available under the EPA sampler contract for use in the STN are the

Reference Ambient Air Sampler (RAASTM), the Mass Aerosol Speciation Sampler (MASS), and the

Spiral Ambient Speciation Sampler (SASSTM). Another sampler that has been in use for several years,

the Interagency Monitoring of Protected Visual Environments (IMPROVE) sampler, is also available

for use. In the near future, Rupprecht and Patashnick Co. (R&P) Model 2300 will soon be available

to the ROs. However, this sampler must pass the EPA’s acceptance procedures before it can be

considered for the STN. In addition to the R&P sampler, there are several sequential samplers that

will be commercially available in the near future. EPA is currently conducting tests on these instruments

and assuming that the sequential samplers pass these tests, the EPA will make these instrument available

to the ROs. 

All filter-based STN samplers use TeflonTM, nylon, and quartz filter media for the collection of target

analytes. The TeflonTM filter will be used to collect particles for the analysis of mass and metals

composition, samples to be analyzed for carbon components of particles will be collected on the quartz

filters, and samples for ion analysis will be collected on nylon and/or Teflon filters. Each sampler’s

operating manual and the corresponding field SOP (refer to Appendix A-1 through A-4) should be

consulted for further details. 

At the recommendation of the Speciation Expert Panel, the operation and acceptable performance of

the commercial samplers have been tested (and continue to be tested) in a series of field and laboratory

research and intercomparison studies. The samplers are being tested against each other and against the

Federal Reference Method (FRM) sampler and historically accepted speciation samplers such as the

IMPROVE sampler and the Versatile Air Pollution Sampler (VAPS) in a four-phase study. In Phase I,

which occurred in the winter and spring of 1998/1999, tests were conducted in four cities (Philadelphia,

PA; Research Triangle Park, NC; Phoenix, AZ; and Rubidoux, CA) during the period to determine

response to differing aerosol compositions. Phase II took place in Seattle, WA; from March to July

1999. Phase III was carried out in Atlanta, GA, during the summer of 1999 as part of a Supersite

study. Phase IV is a 12-city mini-trends and operational evaluation study, to be operated by the States,
PM2.5 STN QAPP

Section No. 5

Revision No.: 4.1

Date: 12/00

Page 3 of 3

in which each site will have at least two speciation samplers for comparison. The Mini-Trends Study

will begin in November 1999 and continue for 6 months. The Mini-Trends Study is a part of the STN. 

Therefore, this QAPP will be used for the Mini-Trends Study and will be revised, based upon needed

improvements for the full STN.

Each phase of the testing program seeks to refine the samplers’ designs and operation and to better

understand topics such as the following:

< A sampler’s ability to collect, size-selective, fine particle mass, sulfate, and elements;

< A sampler’s ability to collect carbonaceous aerosols and nitrate; and

< The ease and reliability of a sampler’s operation, including its ability to hold steady

calibrations of temperature, pressure, and flow.

5. 4 Monitoring Network Design Considerations

The design of the STN 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. General requirements for chemical

speciation specify that approximately 20 sites must be located at existing type 2 PAMS sites. PAMS

network design and monitoring objectives are explained in Appendix D of Part 58, Code of Federal

Regulations (CFR). 

Selection of the remaining STN sites was based on EPA recommendations, with review and advice

from State and local agencies. Most of the remaining sites will be located in MSAs. Their specific

locations will be based on factors such as:

< Location of existing PAMS and IMPROVE network sites

< Geographic locations of MSAs using 1996 population statistics

< Ozone nonattainment areas

< PM10 nonattainment areas.

STN sites will be placed at the one MSA community-oriented PM2.5 mass site that is experiencing the

maximum concentration in the area. 

Sites will also be placed at population centers in the central, midwest, and southeast portions of the

country to bring the total number of STN sites to 54. Where feasible, sites will be equipped with 10-m

height meteorological towers and instrumentation to collect data on wind speed and direction,

temperature, and humidity. 

Refer to Table 10-3 and Figure 10-1 for further information on the locations of sites in the PM2.5 STN.
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 1 of 11

6.0 Project/Task Description

This section provides trends network partcipants with a background understanding of the STN project

and the types of activities to be conducted, including acquiring the samples; performing chemical

analysis; carrying out quality assurance/quality control goals and procedures; and meeting the schedules

for network implementation, operation and data reporting. 

6.1 Description of th Work to be Performed

6.1.1 Overview of the STN Operations

The operation of the STN can be diagrammed as a series of interlocking field and laboratory activities. 

Figure 6-1 depicts 10 steps involved in implementing and operating the network and the delineation of

responsibilities for required tasks. Each step is briefly described below:

1. The PM2.5 STN 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; sampling schedule; and the requirements

for number and type of sample filters, denuders, and sample analyses is sent to the Regional

Speciation Coordinator by the site contact person or other State coordinator.

2. The RSC conveys the site’s needs to the 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 DOPO authorizes the contract laboratory to begin

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

keeps the STN Project Officer informed about these requests.

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 (e.g., examine anemometer and wind vane for damage; check realtime data display for wind speed, wind direction, temperature, and relative humidity versus

independent observations), collect the PM2.5 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 a computer disk. 

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

and quality assurance samples are sent to the designated QA laboratory. The RSC informs

the site when there are nonroutine or QA samples and how and where to send them.

6. The support laboratory analyzes filter samples and conducts level 0 and level 1 data

validation. The data is sent to the State and locals who review and accept the level 0 and 1

validated data or provide edits. The information is sent back to RTI who corrects data.

RTI makes final AIRS database entry.
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 2 of 11

PM2.5 STN Site

Contact Person

- Sampler QA checks

- Install sampling media

- Collect samples

- Pack and ship samples and field data

- RSC

- DOO

- PM2.5 STN PO

Contracted Support 

and Sample 

Analysis Laboratory

EPA QA Labs

- Sample analysis

- Conduct level 0, 1 data validations

- Data review by State/local

- Airs database entry

Assemble 

monthly data and 

QA/QA reports

Perform analysis and 

report to States

PM2.5 STN 

DOPO

Filter and filter 

extract archival

- Conduct level 2, 3 data validations

- Data summarization and interpretation

1 4

3

2

5A

5B

9A 6

8 9B

7

10

Figure 6.1 Summary of STN project operations

7. The support laboratory archives filter extracts for 6 months. Upon request, the laboratory

can send filters back to the ROs who would like to store filters for a longer period of time. 

RTI will archived the filters for three years. 

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

9. The support laboratory submits the monthly analysis report to STN site personnel for

review, further validation, and verification. This report is also submitted to the DOPO.

10. State and local personnel conduct level 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.

6.1.2 Field Site and Laboratory Measurements for the PM2.5 STN

Table 6-1 lists critical field and laboratory measurements for the PM2.5 STN and gives the methods to

be used to acquire the data. 
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 3 of 11

TABLE 6-1. CRITICAL MEASUREMENTS IN THE PM2.5 STN

Measurement 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

Wind direction (degrees of compass)** Wind vane

Free-form notes on sampling difficulties and unusual

conditions at the site

Analytical Support Laboratory

Temperature, shipment cooler (Celsius) Digital thermometer

Mass, PM2.5 (TeflonTM filter) (:g/filter and :g/m3 of air) Balance, microgram

Elements (Teflon filter) (:g/m3) Energy-dispersive X-ray fluorescence (EDXRF) (Na

through Pb)

Cations (various filters) (:g/m3) Ion chromatography (IC) (NH4

+

, Na+, K+)

Anions (various filters) (:g/m3) IC (nitrate, sulfate)

Carbon species (:g/m3) Thermal/optical analysis (total, organic, elemental,

and carbonate carbon)

** - Optional at site

6.2 Field Activities 

6.2.1 Checklist of Field Activities

The field site operator and the sampling site he or she operates are considered the most important

components of the STN and its scientific output. 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 STN. The table also gives the

frequency at which the activity should be performed.
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 4 of 11

TABLE 6-2. CHECKLIST OF PM2.5 STN FIELD ACTIVITIES

Activity Frequency

Comment or

Reference

Attend training sessions. Once, prior to site operation. 

Updated training as required.

Assist with equipment selection, contact with RSC,

and ordering of laboratory analytical services. 

Once, prior to site operation.

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.

Document 2.12,

Section 4

Install sampler(s) at site. Once, at beginning of STN

participation.

Refer to

Appendix A-1

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

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. 

Every 3rd day with dates and

start/end times specified by

EPA. 

Cleaning process

must be thorough

and avoid

contamination of

sample pathways

Retrieval and packaging of samples, field blanks, and

denuders into cooler. Completion of custody and

field data forms, and shipment of samples to

laboratory via Federal Express. 

Every 3rd day for regular STN

operation.

Refer to 

Appendix A-1

Data download from instrument As soon as practicable

Participate in data validation training session. 

Review initial data from laboratory; conduct levels 2

and 3 data validation. Inform DOPO of data

acceptability.

Initial training. Follow-up

sessions. Monthly review of

data sets.

Refer to PM2.5

Speciation Guidance

Document, Section

2.0, “Data Analysis”

Communicate with State or local management, STN

management, and contract laboratory (through

DOPO).

As required and appropriate.

Participate in scheduled STN 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 EPA Office of

Air Quality Planning and

Standards (OAQPS) or EPA

Regional QA Officers.
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 5 of 11

6.3 Laboratory Activities

The STN will require extensive laboratory activities. A single contract laboratory will be employed for

analysis of routine samples from the network. Research Triangle Institute has been chosen to fulfill

these duties. The following subsection summarizes the laboratory activities that will occur to support

the STN.

6.3.1 Presampling Activities

1. Teflon, nylon, and quartz filters will be received from various vendors and examined for

integrity and background analyte concentrations.

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

accurate data entry.

3. Filters will be tested, equilibrated, and weighed as required and stored awaiting use.

4. Filters will be prepared or packaged for field activities. 

5. The laboratory will maintain shipping/receiving supplies to include cooler containers, ice

substitute packs, and custody and field data forms.

6.3.2 Postsampling Activities

1. Shipments of filters bearing PM2.5 deposits will be received in the laboratory, checked for

integrity (damage, shipment temperature, and so on), and logged in. Information on the

custody and field data form will be reviewed.

2. Filters will be stored (refrigerated or frozen) until ready for analysis.

3. Filters will be 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 will be entered into the laboratory database.

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

concentrations of species in terms of a mass per unit volume of air sampled (:g/m3).

6. Filters and filter extracts will be archived (frozen or refrigerated) for 6 months.

7. Data will be transferred to the AIRS database, to the DOPO, and to the designated person

in the State operating the trends network site for review and approval.

8. All paperwork, including custody and field data forms, chromatographs, analyzer data

reports, results of QA/QC studies, and free-form notes, will be filed for ready retrieval and

inspection as required for at least a 3-yr period.

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

laboratory’s QAPP. 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 with the exception

that the URG sampler also collects samples for ions on PTFE (Teflon).
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 7 of 11

RTI Submits to 

AIRS

 Approved for 

AIRS? 

RTI performs 

Level 0/1 Data 

Validation

Data to

 State

Data to 

DOPO

 Approved 

for 

Payment?

Notify Region 

and DOPO

DOPO Contacts 

RTI

DOPO Signs 

Invoice

Suspend or 

Reject 

Payment

EPA Finance

Copy 

Project 

Officer

Yes Yes

No No

30 Days

60 Days 60 Days

State identifies need for 

analysis and forwards 

request to RSC

RSC sends 

consolidated 

request to DOPO

DOPO consolidates 

and forwards 

request to contract 

lab SPM

Sites collect 

samples and

return filters to 

contract lab

Contract lab 

prepares and ships 

filters and supplies 

to sites.

Routine Sample type? Field QA/nonroutine

Contract lab 

performs analysis

EPA and regional 

QA labs perform 

analysis

Data forwarded

Technical Assistance

Figure 6-2 Sample analysis delivery order process
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 8 of 11

Figure 6-3. Diagram of laboratory field processing and analysis activities, by 

 filter type
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 9 of 11

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

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

particle components) in micrograms (:g) that, when combined with the field sampler air volume 

in cubic meters (m3), provides a final concentration in micrograms per cubic meter (:g/m3). Table 6-1

lists all the analytes to be quantified for the STN samples. 

6.4 Schedule of Activities

In order to ensure that the implementation of the additional trends sites is accomplished, many aspects

of the program must be completed in a timely, efficient fashion.

6.4.1 Planning Time Lines

Table 10-1 in Section 10.0 provides the key planning aspects of the program.

6.4.2 Implementation Time Lines

Other important dates must be met during implementation activities. 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 6-3 and

stipulated in the Code of Federal Regulations (CFR), Teflon filters must be used at the field site

within 30 days (d) of presampling weighing or they must be reconditioned and reweighed. 

Furthermore, the contracting laboratory must submit validated speciation concentration data to EPA

within 20 business d following receipt of any sample from the field. Therefore, it is critical that the

contract laboratory and the field sites develop, agree on, and consistently follow a schedule that will

satisfy the requirement that the mass of PM2.5 on Teflon filters be determined within 10 d after the

sampling period ends and that determination of all analytes be completed, validated, and submitted to

the DOPO for review and acceptance within 20 business d. 

6.4.3 Field Time Lines

Table 6-3 indicates that filters should be collected and be prepared and ready for shipment to the

laboratory within 48 hours (h) of the end of the sample period to prepare for the next 1-in-3 d sampling

period. Please see Appendix A-6 on the CY2001 calendar, which indicates the sample run days for

the STN. In some circumstances, this may not be practical or possible. If the agency cannot collect

the samples on weekend, then an alternate schedule must be adopted. Please see Appendix A-6 for

the Monday and Friday dates that must be collected. It is noted that if a Friday run is operated and

collected on Monday, as noted in the alternate schedule, then the hold time will be greater than 48
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 10 of 11

hours. This should be noted on the COC form. Any other instance where a sample is not shipped

within 48 hours should also be noted. 

Data should be downloaded from the speciation samplers on the day of filter sample retrieval and

stored on two media (computer hard drive and diskette). Data may also be transmitted using a modem. 

In addition, the most critical data values will also be recorded from each sampler’s liquid-crystal display

(LCD) screens onto a custody and field data form and sent to the laboratory with the samples. 

Figure 12-1 is an example of such a data form. 

6.4.4 Data Assessment Time Line

Data Availability—In order to compare the speciation and routine samplers’ mass data, data from the

routine sampler must also be available in AIRS. State/local requirements for data upload to AIRS is 90

d after the quarter in which the data were collected. However, the time frame for pre- and postsampling

weighing, as indicated in Table 6-3, is also a requirement for the routine samplers. Therefore, data for

the routine sampler evaluated could be available within 30 d of the sample end date. This requirement

is written into the laboratory contract with OAQPS. Submittal of routine sampler data as soon as

possible is encouraged if data assessment is to occur in a timely manner.

Assessments—After both routine (mass only) data and speciation data for a site are in the AIRS

database, OAQPS, Regions, and State and local agencies can use the AIRS data evaluation programs,

based on data quality assessment (DQA) techniques, to assess this information. This assessment will be

part of the level 2 and level 3 data validation process. 

TABLE 6-3. CRITICAL FILTER AND DENUDER HOLDING AND USE TIMES

Filter or Denuder Type Field Deadlines Laboratory Deadlines

Teflon (*) Use within 30 days of preweighing;

retrieve and must ship within 48 h

of sample completion.

Condition and reweigh within 10

business d of receipt from field site.

Quartz (*) Retrieve and ship within 48 h of

sample completion.

Analyze filter catch within 20

business d of receipt of sample.

Nylon (*) Retrieve and ship within 48 h of

sample completion.

Analyze filter catch within 20

business d of receipt of sample.

Nitric acid denuder (sodium

carbonate) (**)

Replace after 3 months’ use. Refurbish as required.

Nitric acid denuder (magnesium

oxide) (**)

Replace after 3 months’ use. Refurbish or replace as required.

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

(**) Limitations on denuder lifetime are tentative.
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 11 of 11

6.4.5 OAQPS Reporting Time Lines

QA Reports—As mentioned in Section 3.0, OAQPS plans to develop a yearly QA Final Report

(QAFR) and an interpretive QA report every 3 yr. The yearly report will be based on a calendar year

and will be completed 6 months from the last valid entry of routine data by the State and local agencies.

The 3-yr QA report will be generated 9 months after the last valid entry of routine data by the State

and local agencies for the final year.

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 (MSRs), network reviews, technical system audits (TSAs), performance

evaluations (PEs) and, audits of data quality (ADQs). Table 20-1 specifies the agencies responsible for

these assessments.

6.6 Project Records

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

review, approval, issuance, use, control, revision, and maintenance of documents and records. Table

6-4 represents the categories and types of records and documents applicable to document control for

PM2.5 information. Information on key documents in each category is explained in more detail in

Section 9.0.
PM2.5 STN QAPP

Section No. 6

Revision No.: 4.1

Date: 12/00

Page 12 of 11

TABLE 6-4. CRITICAL DOCUMENTS AND RECORDS

Categories Record or Document Types

Management and organization Organizational structure

Quality system strategic plan

Implementation plan

Reporting agency information

Personnel qualifications, training records, certifications

Quality management plan

Document control plan

EPA and State directives

Support contract documentation

Site information Network description

Site characterization file

Site maps (paper or digital)

Site photographs

Environmental data

operations

QAPP

Standard operating procedures (SOPs), including operating manuals

Guidance document (laboratory)

Guidance document (sampling sites)

Field site and laboratory notebooks

Sample handling and custody records

Inspection/maintenance/safety records

Raw data Any original data (routine and QC data), including data entry forms and

diskette/hard drive data

Data reporting Data, summary and progress reports

Trends evaluation reports and other data summaries

Reports to management

Journal articles, papers, presentations

QA Reports

Data management Data algorithms

Data management plans and flow charts

PM2.5 speciation data

Data management systems

Field and Laboratory Quality

Assurance

Calibration and QC check records

Good laboratory practices (GLP) documentation, including good automated

laboratory practices (GALPs)

Network reviews

Control charts

Data quality assessments (DQAs)

QA reports

System and performance review reports

Response or corrective action documentation

Site visits and audits (technical system audits)
PM2.5 STN QAPP

Section No. 7

Revision No.: 4.1

Date: 12/00

Page 1 of 4

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 for the

Data Quality Objectives Process (U.S. Environmental Protection Agency , 1994):

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

chemical Speciation Trends Network (STN). The DQO process that the workgroup employed is fully

documented in its report (U.S. EPA, 1998), which is available online at the AMTIC Web page for

speciation:

http://www.epa.gov/ttn/amtic/pmspec.html

7.2 Development of DQOs for the PM2.5 Chemical STN

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

EPA workgroup, who acted as stakeholders for the program:

... to be able to detect a 3 to 5 percent annual trend 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 although the DQO statement says "3 to 5 percent" and "3 to 5 years," the

default assumptions in this QAPP will be detection of a 5 percent trend after 5 yr.]

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
PM2.5 STN QAPP

Section No. 7

Revision No.: 4.1

Date: 12/00

Page 2 of 4

statement means that there must be an 80 percent probability of detecting a trend of 5 percent after 5 yr

at any particular site, for any single analyte.

Several secondary objectives for data collected at the STN sites and other chemical speciation sites

were identified, but these were not evaluated quantitatively by the workgroup. Four important

secondary data uses are as follows:

< Model evaluation, verification, and/or validation

< Emission inventory

< Source attribution

< Spatial and seasonal characterization of aerosol distributions.

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

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

objective for trend detection.

The DQO study also concluded that by sampling every 3rd d for 5 yr, trends greater than 5 percent (or

less than -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 3rd d provides little

improvement in the ability to detect trends; however, the model showed that cutting the sampling rate to

every 6th d begins to impair the ability to detect concentrations trends within 5 yr.

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 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 prescribed by the DQOs. The MQOs can

be defined in terms of the following data quality indicators:

Precision - a measure of mutual agreement among individual measurements of the same property usually under

prescribed similar conditions. This is the random component of error. 

Bias - the systematic or persistent distortion of a measurement process which causes error in one direction.

Bias will be determined by estimating the positive and negative deviation from the true value as a percentage of

the true value.

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 method specific

procedure can reliably discern.
PM2.5 STN QAPP

Section No. 7

Revision No.: 4.1

Date: 12/00

Page 3 of 4

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 Pt. 50).

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

Accuracy has been a term frequently used to represent closeness to “truth” and includes a combination

of precision and bias error components. 

For the field activities Section 14 presents the MQOs and the calculations for accuracy, precision, bias,

and completeness. Representativeness is determined through the original STN DQO and sampling

design process and detectability is discussed in the Quality Assurance Project Plan: Chemical

Speciation of PM2.5 Filter Samples. Comparability is achieved in the STN by use of appropriate

(performanced based) sampling instruments, and adherence to standard SOPS, and QAPPS and the

use of a single laboratory for analysis and data reporting.

The STN strategic plan (U.S. EPA, 1999b) quotes measurement quality objectives (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 Table 7-1. 

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 QC 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. 

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.
PM2.5 STN QAPP

Section No. 7

Revision No.: 4.1

Date: 12/00

Page 4 of 4

7.4 References

U.S. EPA (Environmental Protection Agency). 1994. Guidance for the Data Quality Objectives

Process: EPA QA/G-4, Report No. EPA/600/R-96/055, U.S. EPA, Washington, DC.

U.S. EPA (Environmental Protection Agency). 1998. 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). 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). 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 STN QAPP

Section No. 8

Revision No.: 4.1

Date: 12/00

Page 1 of 3

8.0 Special Training Requirements/Certification

8.1 Training

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

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

positions. Each State or local monitoring agency is ultimately responsible for adequately training the

personnel performing supervisory, QA/QC, data handling, and other duties related to the PM2.5

chemical speciation network. Monitoring agency management must ensure that these personnel have

access to the relevant guidance documents, SOPs, 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 adequately documented. 

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

State and local personnel who may be unfamiliar with the operation of PM2.5 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 Speciation Trends Network. 

8.1.1 State and Local Agency PM2.5 Training

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

are as follows:

< Review of 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 Quality System for the

Chemical Speciation Monitoring Trend Sites (April 1999).

Suggestions for State and local management personnel for training site operators in STN site operations

are as follows:

< Supply an overview of the NAMS PM2.5 STN through a video presentation. A video is

available online through the OAQPS’ Education and Outreach Group at

http://www.epa.gov/oar/oaqps/eog.

< Schedule meetings and/or teleconferences with personnel from the State and local agencies,

OAQPS, the Regional Speciation Coordinator, the support laboratory, and the Delivery

Order Project Officer prior to beginning trends network sampling operations.

< 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.
PM2.5 STN QAPP

Section No. 8

Revision No.: 4.1

Date: 12/00

Page 2 of 3

< Field personnel who are unfamiliar with operating and quality assuring data from

meteorological monitoring systems should review the system’s operating manual and consult

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 Web site is

available at http://www.epa.gov/ttn/amtic/amticpm.html.

8.1.2 Targeted Training for PM2.5 Sampling and Laboratory Operations

Videos—The video, “Filter Handling and Analysis for PM2.5 Chemical Speciation Monitoring,” is

available from the EPA OAQPS contact person listed in Section 8.3.

Telecourses—The Air Pollution Distance Learning Network (APDLN) is a digital state-of-the-art

educational satellite-broadcasting network of more than 100 governmental and university broadcast

affiliates located across the United States. The APDLN is the result of a collaborative partnership

between the EPA, State and local air pollution control agencies, and North Carolina State University

(NCSU). During seminars and telecourses, participants are able to interact with the Nation’s leading

authorities on the latest air pollution control findings, monitoring devices, and systems. Participants can

ask questions of regulators and litigators and interact with the implementers on the APDLN.

The official listing of telecourses available from the EPA’s APTI is announced on a 3-month rolling

schedule that is updated on the APDLN Web site and available from APDLN site coordinators. The

Web site is available at http://www.epa.gov/oar/oaqps/cog.

Workshops—The workshop titled "PM2.5 Monitoring Training: Chemical Speciation" was presented in 

February 1999. Contact APTI and OAQPS to be placed on notification lists for future workshops.

Internet Resources—The following Internet resources are specifically applicable to the PM2.5

speciation monitoring program:

Ambient Monitoring Technical Information Center

http://www.epa.gov/ttn/amtic/amticpm.html—PM2.5 monitoring information: Contains links to other

areas including chemical speciation documents.

http://www.epa.gov/ttn/amtic/pmspec.html—Current chemical speciation documents.
PM2.5 STN QAPP

Section No. 8

Revision No.: 4.1

Date: 12/00

Page 3 of 3

EPA/OAQPS

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 sites.

National Park Service

http://www.nature.nps.gov/ard/vis/vishp.html—National Park Service's visibility monitoring

information, including the Interagency Monitoring of Protected Visual Environments (IMPROVE)

network.

http://www.nature.nps.gov/ard/vis/sop/index.html—IMPROVE standard operation procedures

(SOPs).

http://www.nature.nps.gov/ard/impr/index.htm—IMPROVE newsletters.

PM2.5 Speciation Sampler Manufacturers' Information and Contacts

http://www.graseby.com/fpm.htm—Andersen Instruments Inc., manufacturer of RAAS 2.5-400

sampler.

URGCorp@compuserve.com—URG Corp., manufacturer of MASS 400 and 450 samplers.

metone@metone.com—Met One, manufacturer of SASS sampler.

8.2 Certification

There are no special certification requirements applicable to operation of the chemical speciation trends

monitors.

8.3 Contacts for More Information

OAQPS Contact for PM2.5-Related Training

Ms. Jan Cortelyou-Lee

Office of Air Quality Planning and Standards (MD-14)

Research Triangle Park, NC 27711

(919) 541-5393

Internet: cortelyoulee.jan@epa.gov
PM2.5 STN QAPP

Section No. 9

Revision No.: 4.1

Date: 12/00

Page 1 of 6

9.0 Documentation and Records

This section defines the records critical to the Speciation Trends Network, 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.

The STN will structure its records management system in a manner similar to the EPA records

management system and follow the same coding scheme in order to facilitate easy retrieval of

information during internal and external systems audits and reviews. Table 6-4 in Section 6 identifies

the documents and records that will be filed according to the statute of limitations discussed in Section

9.7. The field and laboratory 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 QA reporting

packages for management, field operations, laboratory operations, data management, and quality

assurance functions of the STN. The term reporting package is defined as all the information required

to support the chemical speciation concentration data (and ancillary data) reported to EPA, which

includes all data required to be collected as well as other data deemed to be important by the STN. 

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. 

Table 6-4 in Section 6 identifies these documents and records. 

9.1 Information in the Management and Organization Reporting Package

There are three distinct management organizations associated with the STN: (1) the EPA Office of Air

Quality Planning and Standards and Regional EPA offices, (2) the State and local monitoring offices,

and (3) the contract site supply and sample analysis laboratory. The management reporting package

for these organizations will vary but would normally consist of at least 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 STN.

9.2 Information in the Field Operations Reporting Package

9.2.1 Site Information

A file containing site documentation will be maintained in the State or local agency’s central or field

office for each STN 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
PM2.5 STN QAPP

Section No. 9

Revision No.: 4.1

Date: 12/00

Page 2 of 6

speciation sampler(s). The STN coordination office or the Regional Speciation Coordinator may ask

for copies of this material for a central file.

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 STN 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 sample

content and concentration (wind or electrical damage to equipment, construction or mowing activities in

the area, welding, traffic). Such information should 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 (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.

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.

Field Binders—A 3-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—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

STN work. It will include examples of standard shipping/receiving forms and areas for free- form notes

about shipment difficulties or concerns such as equipment that arrives damaged or has missing parts. 

9.2.3 Electronic Data Collection at Field Sites

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 containing information from each of the

every-third-day sampling events will be created. It will be retained in the field operator’s files 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.
PM2.5 STN QAPP

Section No. 9

Revision No.: 4.1

Date: 12/00

Page 3 of 6

9.2.4 Hand-Entered Data at Field Sites

A number of field forms will require hand entry of data. These forms are primarily associated with the

field sites. An example of the combined custody and field data form can be found in the SOPs of

Appendix A to this QAPP and in Section 12.0. The forms should be in 3-part carbonless paper

format. A quality assurance/quality control report form, shown in Section 14.0 and in the SOPs in

Appendix A to this QAPP, 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

diskette data become corrupted or lost. Difficulties with or suggestions for improved operation of the

samplers should be recorded here and in the field notebook. Such comments will be very valuable

during the initial months of the network operation. 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 STN contract laboratory. 

9.4 Information in the QA Reporting Package

Four distinct QA organizations are associated with the PM2.5 STN.
PM2.5 STN QAPP

Section No. 9

Revision No.: 4.1

Date: 12/00

Page 4 of 6

9.4.1 Network QA Manager

The OAQPS management organization has a QA Manager. This Manager and staff members will

produce and update the quality system and will review QA documents from the STN’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 STN QAPP and any subsequent changes

made to it.

9.4.2 State and Local Field Site QA Offices

The various State and local agencies whose personnel will operate the STN 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.

9.4.3 Contract Laboratory QA Manager’s Office

The contract 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 EPA.

9.4.4 EPA QA Laboratory Offices

EPA and Regional laboratories will provide QA services to the field and laboratory components of the

STN. Their documented procedures will be kept on file and updated as necessary using document

control methods. EPA Region 1, NAREL and R&IE laboratories will provide QA services for STN

field and laboratory activities.

9.5 Reports to Management

The State and local field site operators will follow their customary procedures for reporting information

to their local or State managers. 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 RSC as

appropriate. Field site operators will also report information on PM2.5 sample and meteorological data

capture rates and problems with sampling equipment and check devices for the speciation samplers. 
PM2.5 STN QAPP

Section No. 9

Revision No.: 4.1

Date: 12/00

Page 5 of 6

Table 9-1 STN 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 Pictures

Field and

Laboratory

Environmental

Data Operations

QA Project Plans 

Standard operating procedures (SOPs)

Field and laboratory notebooks communications

Sample handling/custody records

Inspection/Maintenance records

Raw Data Any original data (routine and 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

Data Management Systems

Quality Assurance Good Laboratory Practice 

Control charts

Data quality assessments

QA reports 

System audits

Response/Corrective action reports

Site Audits

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.

The contracted 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 DOPO and to the State or local

contact who submitted the delivery order within 20 business from receipt of the sample. Level 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 Aerometric Information Retrieval System (AIRS) electronic database. Draft and final

composite semiannual data summary reports will be issued from the laboratory to the State or local
PM2.5 STN QAPP

Section No. 9

Revision No.: 4.1

Date: 12/00

Page 6 of 6

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 STN 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 contract laboratory, Regional and EPA QA offices,

and validated electronic AIRS data sets must be retrievable for inspection and review during regular

business hours by OAQPS management or other U.S. Government authorities.

Limits on the time of data (and sample filter) retention will be 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 yr following sample analysis is presently 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 STN QAPP

Section No. 10

Revision No.: 4.1

Date: 12/00

Page 1 of 7

10.0 Sampling Process Design

This section describes all components associated with on-site field operations of the nationwide PM2.5

STN. The network will be operated by State and local agencies in 39 States, the District of Columbia,

and Puerto Rico. This section describes the key parameters to be estimated, the locations of primary

speciation samplers and collocated quality assurance speciation samplers, the frequency of sampling

using the primary and QA samplers, and the location and frequency of on-site systems and

performance evaluations PEs. The network design components comply with the regulations specified in

40 Code of Federal Regulations Part 58, Section 58.13, Appendices A and D, which are further

described in the document Guidance for Network Design and Optimum Site Exposure for PM2.5

and PM10 (U.S. EPA 1997).

10.1Scheduled Project Activities, Including Management Activities

The STN will be sampling for chemical components of PM2.5 at 54 locations. Fifty-four primary

speciation samplers and 7 collocated QA speciation samplers will be employed. Of the 54 sites, 20

will be located at existing Type 2 PAMS, which are part of the NAMS network. The remaining 34

sites will be located at existing sites, or sites to be established, in selected (MSAs or CMSAs. All 54

sites will have a collocated Federal Reference Method monitor present to collect samples for

determination of particle mass concentration.

Installation of the speciation samplers and operator training occurred during the third quarter of 1999

and the first quarter of 2000. Twelve sampling sites in 12 States were installed in October 1999 as a

Mini-Trends Study and an initial operational evaluation component of the network. The installation

sequence then proceeded to each of the existing PAMS sites and then to NAMS sites in the chosen

MSAs. Those sampling locations that did not have an existing site available will come online as the

locations are approved and readied for use. The goal is to have all 54 samplers installed and tested,

operators trained, and laboratory support arrangements and schedules in place by December 2000. A

time line schedule of activities that apply to sites in the STN is given in Table 10-1.

Attaining a complete understanding of the interactions and scheduling of field and support laboratory

activities is a very important consideration during the design, installation, and startup phases of the STN. 

A schedule of activities for the supporting contract laboratory for the NAMS trends network is

presented in Table 10-2. 
PM2.5 STN QAPP

Section No. 10

Revision No.: 4.1

Date: 12/00

Page 2 of 7

TABLE 10-1. SCHEDULE OF ACTIVITIES FOR STATE AND LOCAL PM2.5 STN 

FIELD SITE PARTICIPANTS

Anticipated Date Notes

Select sites. Arrange for space, electrical

power, personnel.

July 1999 through March

2000

Network participants meet (12-site MiniTrends Study initially).July 1999 and continuing

Order speciation sampler(s) and accessories

under national contract (12-site Mini-Trends

Study initially).

August 1999 and

continuing

Confer with U.S. Environmental

Protection Agency (EPA) prior to

ordering to confirm sampler

selection and need for collocated

sampler.

Acquire 10-m meteorological tower and sensor

package, if appropriate

August 1999 and

continuing

Confer with EPA prior to ordering.

Order only if needed at site(s).

Review, conditionally approve STN quality

assurance project plan (QAPP) and pertinent

standard operating procedures (SOPs).

August and September

1999

Receive and install sampler(s). September 1999 through

March 2000

Contingent on vendor schedule.

Confer with Regional Speciation Coordinator

(RSC) and others.

September 1999 and

continuing as sites come

on line.

Finalize mechanism and schedule

for delivery order process for

routine, nonroutine, and QA

samples.

Attend training sessions and/or review video. October 1999 and

continuing

Consult EPA’s Office of Air Quality

Planning and Standards (OAQPS)

and EPA Regional Offices for plans.

Complete site preparation and sampler

installation. (a) 12-site Mini-Trends Study (b)

42 additional sites.

(a) By October 1999

(b) By Decemberl 2000

Obtain site documentation and

photographs/slides for site file.

Begin Mini-Trends sampling at 12 sites. November 1, 1999

Incorporate lessons learned and comments

from 12-site Mini-Trends network into draft

STN field QAPP.

July 2000-Dec. 2000

Final Approval Jan. 2001

Resolve sampling problems experienced by

the 12-site Mini-Trends Study. Revise

procedures accordingly and obtain networkwide approval.

Prior to April 2000

sampling date

Involve field staff, RSC, laboratory,

OAQPS as required.

Begin routine, every 3rd-d speciation sampling

at all STN sites.

February 1, 2001 Refer to every 3rd-d sampling

schedules for 2000 and beyond.

Participate in routine and nonroutine trends

sampling and field QA programs.

December 2000 and

continuing

Interact with RSC.

Review and level 2 ,3 validation of monthly

data reports received from laboratory.

Each month. Complete

review within 30 d

Interact with RSC and OAQPS to

resolve problems.

Report problems and suggestions for

improvement to State/local management and

so on.

As required Interact with RSC and OAQPS.

Consolidate STN QAPPs for field, laboratory,

audit program.
PM2.5 STN QAPP

Section No. 10

Revision No.: 4.1

Date: 12/00

Page 3 of 7

TABLE 10-2. SCHEDULE OF ACTIVITIES FOR CONTRACTING STN LABORATORY

Activity Date Notes

Prepare and obtain approval of QAPP and

SOPs for laboratory activities and field site

support.

Draft: August 1999

Final: September 1999

Includes laboratory SOPs, tested

and approved for use.

Meet with OAQPS project scientists, RSCs,

and Delivery Order Project Officers (DOPOs).

September 1999 Receive details on initial STN site

contacts and sampler requirements. 

Finalize mechanism and schedule

for delivery order process for

routine samples.

Receive and analyze routine speciation

samples.

November 1999 and

continuing

Assemble, validate, and report data. Review

field and laboratory interactions; review and

resolve problems.

November 1999 and

continuing

Complete analyses within 20 business d of

sample receipt. Prepare and submit monthly

draft summary data reports to DOPO and State

agencies for review and validation.

Submit summary data

report by 15th d of month

following month of

analyses

Conduct level 0 and level 1

validation of data. 

Submit final data packages following

State/local and DOPO approval of draft data.

Quarterly Enter data into Aerometric

Information Retrieval System

(AIRS).

QA auditing and inspections. Various times; quarterly QA Manager for contract

laboratory conducts audits.

Systems audit and review of data archives. Annually Coordinated by EPA.

10.2 Rationale for the Design

10.2.1 Network Design

The rationale for the design of the STN is in part found in the requirements and principles set forth in the

Federal Register (62 FR 38763), promulgated as part of the PM2.5 National Ambient Air Quality

Standards review completed in 1997. This rule specifies that a 50-site chemical speciation trends

network be established as a component of the overall PM2.5 criteria pollutant study effort. These sites

should include approximately 20 PM2.5 core sites to be collocated at PAMS sites. 

The remaining speciation trends sites are located to include major population areas in the central,

Midwestern, and southeastern United States, which, in many cases, also include areas with the region’s

higher PM10 and PM2.5 precursor emissions. In locating speciation sites within each of the suggested
PM2.5 STN QAPP

Section No. 10

Revision No.: 4.1

Date: 12/00

Page 4 of 7

MSAs, it is recommended that the speciation trends site be a community-oriented PM2.5 core site,

which is expected to receive the maximum PM2.5 concentrations for the MSA. Where feasible, each

MSA speciation trends site should be outfitted with a 10-m eter meteorological tower to collect data on

wind speed and direction, temperature, and humidity. Please note that for modeling purposes, wind

speed and direction vector, the standard deviation of wind direction (sigma theta), ambient temperature

and relative humidity should be collected. Most modern data acquisition systems have the capability to

collect the vector and sigma theta data. If a meteorological tower is not feasible, then the RO should

attempt to collect the nearest meteorological data from the National Weather Service or nearby

airports. However, the weather station should be within 10 miles of the station for the weather data to

useable. If this is not feasible, the meteorological data used must represent the airshed. If, after

collection and review of data from several samples, a site is judged to be biased by emissions from a

nearby source or by poor ambient air exposure, the data will be examined, recommendations will be

made by the local agency for relocating the site, and a decision will be made by the networks

coordinating office based on the findings. Examples of causes of sampling bias could be detection of

unusually high concentrations of a metal or filter loadings much higher than other sites in the airshed. 

OAQPS scientists and peer review members of the Subcommittee on Fine Particle Monitoring (a

subcommittee of the Clean Air Scientific Advisory Committee, have participated in numerous meetings

to discuss the STN’s design and how it should begin operations. It was decided that the network

should first begin as a 12-site, 12-State Mini-Trends Study. The Mini-Trends Study’s purposes are to

provide State personnel with hands-on experience in the operation and selection of speciation samplers

and to gain knowledge about PM2.5 chemical composition and sampler operations during cold weather

and in woodsmoke emissions areas.

10.2.2 Speciation Sampler Design and Selection

Sampler design requirements stated in 40 CFR Part 53 require that speciation samplers incorporate

particle inlets and size fractionators having comparable particle size discrimination curves as the

reference method for PM2.5, employ denuder technology to remove acidic and organic 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 on performance in order to meet the STN data quality objectives. Desirable

features of speciation samplers are discussed in the PM2.5 speciation guidance document (U.S. EPA

1999).

Speciation sampler(s) will also be collocated at 7 of the 54 sites in the network. These sites are

identified in Table 10-3. The collocated samplers provide a set of PM2.5 speciation data, originating

from a separate but otherwise identical sampler, in order to estimate the precision of the total sample

collection, handling, and analysis/data reporting process. The collocated QA sampler will also be

operated every 3rd d to coincide with the start and end run times of the site’s primary monitor. Samples

and data from the QA sampler will be handled in exactly the same way as those from the primary

sampler. Section 14.0 discusses this precision check in more detail.
PM2.5 STN QAPP

Section No. 10

Revision No.: 4.1

Date: 12/00

Page 5 of 7

TABLE 10-3. PROPOSED SITES FOR THE PM2.5 STN

EPA

Region

State or

Commonwealth

MSA or PAMS 

City Site Name AIRS Number Local Sampling and QA/QC Contacts

1 Connecticut East Hartford (M) 09-003-1003

Maine Kittery (P) 23-031-3002

Massachusetts Boston, U. (P, 1) 25-025-0042 Jerry Sheehan, 978-975-3215

(jerry.sheehan@state.ma.us)

Massachusetts Chicopee (P) 25-013-0008 Jerry Sheehan, 978-975-3215

(jerry.sheehan@state.ma.us)

Rhode Island East Providence (P) 44-007-1010

Vermont Burlington (M)

2 New York Queens (P)

Rochester (M)

36-081-0097

36-005-6001

Dirk Felton, 518-457-9137

(hdfelton@gw.dec.state.ny.us)

New Jersey New Brunswick (1

,P)

34-023-0011

Puerto Rico San Juan (M)

3 Washington, DC McMillan Reservoir

(P)

11-001-0043

Maryland Essex (P) 24-005-3001

Pennsylvania E. Lycoming (P)

Pittsburgh (M)

42-101-0004 Norman Glazer, 215-685-1085

(norman.glazer@phila.gov)

Virginia Norfolk (M)

4 Alabama Birmingham (M)

Florida Miami (M)

Tampa (M)

Tom Tamanini 813-272-5530

(tamanini@epcjanus.epchc.org)

Georgia S. Dekalb (P) 13-089-0002

Mississippi Biloxi (M)

North Carolina Charlotte (M)

South Carolina Charleston (M)

Tennessee Memphis (M)

5 Illinois Northbrook (1, P) 17-031-4201 Terry Sweitzer, 217-782-7438

(epa2204@epa.state.il.us)

Bob Lamorte, 708-865-6184

(ccdects@wwa.com)

Indiana Indianapolis (M)

Michigan Detroit (M)

Minnesota Minneapolis (M)

Ohio Cleveland (M)

Wisconsin Milwaukee (P)

6 Louisiana Capitol (P) 55-079-0041

Oklahoma Tulsa (M) 22-033-0009

Texas Deer Park. (1, P)

Hinton (P)

Chamizal (P)

48-201-1035

48-113-0069

48-141-0044

Ed Michael, 512-239-1384

(emichel@tnrcc.state.tx.us)
TABLE 10-3 (continued)

PM2.5 STN QAPP

Section No. 10

Revision No.: 4.1

Date: 12/00

Page 6 of 7

EPA

Region

State or

Commonwealth

MSA or PAMS 

City Site Name AIRS Number Local Sampling and QA/QC Contacts

7 Kansas Kansas City (M)

Missouri St. Louis (M) Bern Johnson, 573-526-2027

(nrjohnb@mail.dnr.state.mo.us)

James Brunnert, 573-751-2706

(nrbrunj@dnr.state.mo.us)

Nebraska Omaha (M)

8 Colorado Denver (1, M) 

Montana Missoula (M)

North Dakota Bismark (M) Daniel E. Harman, 701-325-5200

(dharman@state.nd.us)

Utah Salt Lake City (M) Robert Neal Olson, 801-877-0764

(rolson@deq.state.ut.us)

9 Arizona Phoenix (M) Tom Moore, 602-207-2353

(moore.tom@ev.state.az.us)

California Riverside

(Rubidioux) (1,M)

El Cajon (P)

Simi Valley (P)

Sacramento (P)

Bakersfield (M)

Fresno (M)

San Jose (M)

06-065-8001

06-073-0003

06-111-2002

06-067-0006

06-029-0014

06-019-0008

06-085-0004

Nevada Reno (M)

10 Idaho Boise (M)

Oregon Portland (M) Steve Aalbers, 503-229-6798

(aalbers.steven@deq.state.or.us)

Washington Seattle (1, M)

Network

Totals

30 States 34 MSAs/Sites; 19

PAMS

Sites; 53 Total 

1 Selected as collocated speciation sampling sites.

2 MSA is Metropolitan Statistical Area, coded by (M) following the site name. PAMS is photochemical air

monitoring station, coded by (P) 

following the site name.
PM2.5 STN QAPP

Section No. 10

Revision No.: 4.1

Date: 126/00

Page 7 of 7

10.2.3 Sampling Frequency

The entire STN will sample consistently every 3rd d. Routine samples will be collected for a 24-h

period beginning and ending at midnight on the assigned day. The every 3rd-d sampling schedules for

CY2001 is available in Appendix A-6. This should be distributed to all site supervisors and operators. 

Sites in the STN will not acquire samples on any other days unless specifically directed to do so by

network authorities. Should nonroutine sampling be requested, such samples must be taken on days

other than those set by the every-3rd-d schedule and must be handled separately when submitted to the

laboratory for analysis.

10.2.4 Deviations from the Sampling Plan

Because the STN’s major goal is to determine trends in PM2.5 chemical speciation concentrations over

time and within geographical areas, deviations from the sampling plan are not allowed. Should an

occasional deviation occur at a site, the site operator must note this in his or her field site notebook and

on the field data form that is returned to the laboratory with the sample filters so the resulting data can

be flagged. Continued deviations from the sampling plan at one or more sites will give rise to a review

of the site’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

may be sequestered and not used in trends analysis studies.

 10.3 Reference

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.

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

Document. Third Draft. January 1999.
PM2.5 STN QAPP

Section No. 11

Revison No.: 4.1

Date: 12/00

Page 1 of 7

11.0 Sampling Methods Requirements

The Speciation Trends Network 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

PM2.5 in ambient air over a 24-h period. Three different brands of PM2.5 speciation monitors will be

used to collect PM2.5 samples. These three samplers have been subjected to bench testing and to

comprehensive multicity field test intercomparisons against each other and against the FRM and the

IMPROVE samplers and have met the requirements stated in the EPA requisition for speciation

samplers. Standard operating procedures for setup, operation, and quality control of the samplers are

given in Appendix A to this quality assurance project plan. 

11.1 Sample Collection and Preparation

11.1.1 Preparation

Before a site visit, the operator must gather sampling modules, data forms, and sampler verification

equipment to check flow, temperature, and pressure (if a 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 coolers. 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, if desired.

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. 

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 and the samplers will run every 3rd day, 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.

11.1.3 Sampler Recorded Measurements

Table 11-1 lists the information that is expected to be 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.
PM2.5 STN QAPP

Section No. 11

Revison No.: 4.1

Date: 12/00

Page 2 of 7

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 h in duration; however, in some cases, a shorter sample period may be necessary, but it should

not be less than 23 h or more than 25 h. Because capture of the 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 h or greater than 25 h, 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

TABLE 11-1. SUMMARY OF INFORMATION PROVIDED BY SPECIATION SAMPLER

Information to be Provided Units

Availability

Provided to

Anytime End of Period Visual Display AIRS Database

Flow rate, average, for the sample

period

L/min r (optional) U (required) r

Flow rate, CV, for the sample period L/min r U r Ž

Flow rate, 5-min average out of

specification (FLAG)

U U U Ž

Sample volume, total m

3 r U U Ž

Temperature, ambient, min., max.,

average, for the sample period

°C r U U Ž

Barometric pressure, ambient, min.,

max., average, for the sample period

mmHg r U U Ž

Filter temperature, differential, 30-

min interval, out of specification

(FLAG)

r U U Ž

Date and time yr/mo/d/h/mi

n

U — U —

Sample start and stop time settings yr/mo/d/h/mi

n

U U U

Sample period start time yr/mo/d/h/mi

n

— U U Ž

Elapsed sample time h min r U U Ž

Elapsed sample time out of

specification (FLAG)

— U U Ž

Power interruptions >1 min, start

time of first ten interruptions

h min r U r

User-entered information, such as

sampler and site identification

U U U Ž
PM2.5 STN QAPP

Section No. 11

Revison No.: 4.1

Date: 12/00

Page 3 of 7

express within 48 h following the end of a sample run. If an agency must deviate from sending the

sample out within 48 hours, please see the discussion in Section 6.4.3 and Appendix A-6. 

11.1.5Field Maintenance and Calibration

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 region personnel will notify the QA

Manager in the Office of Air Quality Planning and Standards (OAQPS) Coordination Office. The QA

Manager will review the information and convey the issue to the Chemical Speciation Workgroup. 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 National Trends

Network (NTN) 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.

Class 3—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.

Upon agreement by the speciation workgroup to institute a change, hard copies of Class 1 and 2

changes will be distributed using the quality bulletin illustrated in Figure 11-1. The STN laboratory, each

site, and the management of each site will be notified. New versions of SOPs will be mailed to STN

participants with instructions to discard the old version. 
PM2.5 STN QAPP

Section No. 11

Revison No.: 4.1

Date: 12/00

Page 4 of 7

Quality Bulletin

Number 

Date 

Page of 

Supersedes No. 

Dated 

Replace and Discard Original

Add Material to Document

Notes:

 

 PM2.5 QA Coordinator

Retain this bulletin until further notice 9

Discard this bulletin after noting contents 9

This bulletin will be invalid after (Date) _____ 9

This bulletin will be incorporated into quality

Procedure No. _________ by (Date) ________ 9

Subject:

Figure 11-1 Quality bulletin
PM2.5 STN QAPP

Section No. 11

Revison No.: 4.1

Date: 12/00

Page 5 of 7

11.2.2 Data Operations

Corrective action measures in field operations of the STN 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 is an attempt to forecast the expected problems and corrective actions

needed for a well-run speciation trends 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 STN 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. Filter cassettes (used with the Andersen RAAS sampler) will be stored in

protective containers. Other sampling modules (used with the URG MASS or the Met One SASS)

will be capped and protected in plastic wrap or polyurethane foam 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 is suggested that they are cleaned

immediately before the sample handling step. It is recommended that plastic gloves be used.

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-h period), the filters will be

subject to ambient temperatures and should not exceed the ambient temperature by more than 5 °C for

more than 30 min continuously. Sampling modules should be removed from the sampler within 48

hours after the sampling period ends. The temperature of sampling modules must be brought to 4 °C as

soon as possible and the shipment package, cooled to 4 °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).
PM2.5 STN QAPP

Section No. 11

Revison No.: 4.1

Date: 12/00

Page 6 of 7

TABLE 11-2. STN FIELD OPERATIONS CORRECTIVE ACTIONS 

Item Problem(s) Action Notification

Sampling media inspection

(presample)

Note: This inspection will

apply only to the

Andersen RAAS sampler.

Filter with pinhole(s) or

tears. Missing component

of sampling module. 

Mismatched module and

chain-of-custody (COC)

form.

1. If additional sampling

module available, use

it; void filters with

pinholes or tears

1. Document on field data

form

2. Use new field blank

module as sample filter

2. Document on field data

form

3. Obtain a new sampling

module from laboratory

3. Notify Delivery Order

Project Officer (DOPO)

and laboratory

Sampling media filter

inspection (postsample)

Note: This inspection will

apply only to the

Andersen RAAS sampler.

Torn or suspect filter

catch

1. Inspect filter holder and

connections

1. Document on field data

form 

2. Check sampler

pneumatics

2. Document in site

notebook; notify field

manager

Sample flow rate

verification(s)

Out of specification

(+10 percent of transfer

standard)

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. Check flow rate at three

points to determine if

flow rate problem is

with zero bias or slope

3. Document on QA/QC 

field data form and

notify supervisor and

sampler vendor

4. Recalibrate flow rate 4. 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 Orings; 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

3. Document in field

notebook and on

QA/QC field data form
TABLE 11-2. (continued)

PM2.5 STN QAPP

Section No. 11

Revison No.: 4.1

Date: 12/00

Page 7 of 7

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

2. Check flow with a flow

rate verification filter

and determine if actual

flow is low

2. Document in field

notebook

Ambient temperature

verification and filter

temperature verification

Out of specification (+2°C

of standard)

1. Recalibrate sensor;

replace sensor

1. Document in field

notebook and on

QA/QC field data form

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 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-crstal 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

1. Document key

information on sample

data sheet. Make

certain problems are

resolved before data

are written over in

sampler microprocessor
PM2.5 STN QAPP

Section No. 12

Revison No.: 4.1

Date: 12/00

Page 1 of 6

12.0 Sample Handling and Custody Requirements

12.1 Introduction

This section describes sample handling and custody procedures that are necessary to ensure that

< Speciation Trends Network 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 STN laboratory.

< Field site use COC and 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 Presampling Sample Handling and Custody Procedures

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 and presented more fully in the PM2.5 sampler SOPs which are

included in Appendix A to this quality assurance project plan.

12.2.1 Procedures in the STN Laboratory

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 STN

laboratory’s QAPP.

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 three-page, carbonless PM2.5 custody and field data form

(CAFDF). 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

CAFDF is illustrated in Figure 12-1 and its contents are explained in Table 12-1. The laboratory will

fill in much of the information required in parts A, B, and C of the form and will retain the third copy. 
PM2.5 STN QAPP

Section No. 12

Revison No.: 4.1

Date: 12/00

Page 2 of 6

The information on the CAFDF will ultimately be entered into a sample tracking system, where an

electronic record will be kept.

12.2.2 Procedures at the Field Office

Upon receipt at the field office of a set of sampling components for a particular speciation sampler, the

STN 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. 

< Inspect the exterior of the shipping cooler, note any evident damage, and record

observations in the operator's field notebook.

< Open the shipping container and ensure that a CAFDF 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 min./max. thermometer (if required) are present. Ensure each

identifying number printed on the CAFDF corresponds to an enclosed sampling channel

component. Do not use any sampling component whose identifying bar code number is not

listed on the CAFDF. Notify the STN laboratory about any discrepancies. Remove the

gel packs and freeze them.

< Sign and date the custody record portion of the CAFDF. 

< 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 STN laboratory has labeled each

sampler channel component for use at a particular site. Should an interchange occur, the STN site

operator must fully document the variance and inform the laboratory so the analytical results can be

associated with the correct sampler and site. 

It has been noted by RTI, that the temperature of some of the coolers that have been received by the

SHAL have been above 4oC. RTI staff believe the problem may be due to the gel packs not being

frozen long enough or at a cold enough temperature. This QAPP recommends that gel packs be frozen

for at least 3 days at a temperature of -32oC. This will insure that the filters do arrive at the RTI

laboratory at or under 4oC.
PM2.5 STN QAPP

Section No. 12

Revison No.: 4.1

Date: 12/00

Page 3 of 6

BAR CODE GOES HERE PM2.5 STN CUSTODY AND

FIELD DATA FORM

White – return to lab

Yellow – site retains

Pink – lab retains Custody/Data Form No.

A. CUSTODY RECORD (Name, Date)

1. Laboratory, Out ______________ 

Date_________

3. Site, Out Date 

2. Site, In Date 4. Lab, In Date 

B. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name 

2. Sampler S/N 6. Intended date of use 

3. Sampler Type 7. Date of sampler set-up 

4. Sampler POC 8. Operator’s name 

C. SAMPLER CHANNEL COMPONENTS

Channel

Number

Component ID

No.

Component Description

1 kept at site SASS cyclone

1 I1234568 SASS cassette (Teflon filter) (GREEN)

2 kept at site SASS cyclone

2 I1234570 SASS cassette (MgO denuder, nylon filter) (RED)

3 kept at site SASS cyclone

3 I1234572 SASS cassette (quartz filter) (ORANGE)

D. START, END, AND RETRIEVAL TIMES

Channel No. Start date Start time End date End time Retrieval

date

Retrieval

time

1

2

3

E. SAMPLER CHANNEL INFORMATION (Post-Sampling)

Channel

No.

Run

Time

Run

 Time, Flag

Sample

Volume

(m3)

Avg.

flow

(L/min)

Avg.

flow CV

(L/min)

Avg.

ambient

T (°C)

Max.

 ambient

T (°C)

Min.

ambient

T (°C)

1

2

3

Channel

No.

aT

Flag

Avg. Filter

T (°C)

Max. Filter

T (°C)

Min. Filter

T (°C)

Avg. BP

(mm Hg)

Max. BP

(mm Hg)

Min. BP

(mm Hg)

1

2

3

Figure 12-1. Custody and field data form (CAFDF) for the PM2.5 STN.
PM2.5 STN QAPP

Section No. 12

Revison No.: 4.1

Date: 12/00

Page 4 of 6

TABLE 12-1. EXPLANATION OF STN 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 analytical 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 multichannel

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, and trip blank 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 laboratory to compute analyte

concentrations. The State and local agencies will use these data in level 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.

12.2.3 Procedures at the Field Collection Site

Sampling components/modules must be used at the field collection site on the sampling date specified

on the CAFDF. 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 STN site operator should follow the SOP written

for the particular sampler. Refer to Appendix A for instructions for the installation of sampling modules

and denuders and programming of the sampler. 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 CAFDF.
PM2.5 STN QAPP

Section No. 12

Revison No.: 4.1

Date: 12/00

Page 5 of 6

12.3 Postsampling Sample Handling and Custody Procedures

The following procedures represent brief descriptions of more detailed 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 cooler

for shipment, refer to the specific sampler's SOPs in Appendix A to this QAPP, to SOPs concerning

sample packaging and shipment in the STN laboratory’s QAPP, and to the sampler’s operating manual

12.3.1 Procedures at the Field Collection Site

The following is a brief description of the post sampling procedures at the field site.. Within 48 h after

the end of a sampling period, the STN site operator should remove the sampling modules from the

sampler. 

At the site, the operator must complete the following: 

< 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 page of the carbonless

form. Refer to the custody and field data form example in Figure 12-1 and to Table 12-1

for details. 

< 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. 

< 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 via a laptop computer to a labeled diskette. Alternatively,

download to a data transfer device for later entry to a diskette.

< Return to the field office.

12.3.2 Procedures at the Field Office

Within 48 h following the end of the sampling period, the STN site operator will: return the modules to

the field office; complete all paperwork; seal the CAFDF in a plastic bag and tape the bag on the inside

of the cooler and package the modules and denuders in the cooler for pickup by the shipping agency

(Federal Express). It is strongly recommended that the site operator not freeze the samples

before they are shipped to RTI. The freezing of the filters may cause some of the ionic constituents

to change chemically. The sample filters should be stored between 0o and 4o Centigrade until

they are placed in the coolers to be shipped to RTI. Illustrated packing instructions for the

modules can be found in Appendix A-5. Please see that appendix for details on packing the modules

for shipment to RTI. At the field office, the operator must complete the following:
PM2.5 STN QAPP

Section No. 12

Revison No.: 4.1

Date: 12/00

Page 6 of 6

< Retain the second page of the 3-page CAFDF and package the top copy in the shipping

container. Package the sampling modules, insert the ice packs in the shipping container,

and take the cooler or package to a drop point or arrange for pickup by the contracted

overnight air shipping company (Federal Express). 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.

12.3.3 Procedures in the STN Laboratory

The STN 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 STN laboratory’s QAPP.

12.4 Filter and Sample Archival in the STN Laboratory

The laboratory database 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 document Quality Assurance Project Plan: Chemical Speciation of PM2.5

Filter Samples. Please contact Research Triangle Institute (see address in Table 3-1) for a copy of

this QAPP. 
PM2.5 STN QAPP

Section No. 13

Revison No.: 4.1

Date: 12/00

Page 1 of 1

13.0 Analytical Methods Requirements

Analytical methods requirements are given in the QAPP for the contract laboratory, Research Triangle

Institute, which will serve the Speciation Trends Network and other State and local agency speciation

sampling programs. Refer to that QAPP, Quality Assurance Plan for Chemical Speciation of PM2.5

Filters for more information.

The analytes sought in PM2.5 for the STN include ions, metals, and various carbon-containing species. 

Refer to Table 6-1 for specific analytes and the analytical methods for their determination. Figure 6-2

is a schematic of the sample analysis delivery order process to be followed by STN participants. The

flow diagram of Figure 6-3 shows how the filters will be processed and analyzed.

The STN laboratory’s technical management and staff organization are presented in Section 4.0 of this

QAPP. Refer to Figure 4-2 for more information. 
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 1 of 8

14.0 Quality Control Requirements

Quality control is the overall system of technical activities that measures the performance of a 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 STN, QC activities are used to ensure and

document that 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 STN QC program requires of State

and local field site participants, as follows:

1. The State or local 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 samples, field blanks, and trip blanks with supporting

hand-entered and computer-downloaded data to the STN laboratory on schedule.

2. The site operator must control the sampler’s collection process through activities including

handling cassettes and sampling modules, properly calibrating samplers, and conducting

both scheduled and as-needed 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 STN laboratory to the

State and local contacts and then reporting the data quality statistics that describe how

effective the QC system has been in achieving accuracy, bias, precision, and completeness

goals.

Table 14-1 contains a complete listing of field QC procedures, their frequency of performance, and the

acceptance criteria, i.e.; measurement quality objectives. Laboratory QC procedures are included in

the companion Quality Assurance Plan for Chemical Speciation of PM2.5 Filters.

 The MQOs have been established in two ways. Some of the MQOs have been derived to help ensure

that the DQO for identifying a trend of 5 percent (in either direction) can be made after 5 yr of

sampling. Other MQOs are based on requirements 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). The

strategic plan for the STN (U.S. EPA, 1999) summarizes the QC requirements for field and laboratory

activities.

Table 14-1 also lists the action to be taken if a QC check shows a parameter to be out of specifications

and how the effectiveness of the corrective action is demonstrated and documented. Specific

procedures for implementing field QC activities are described in the sampler-specific SOPs given in

Appendix A to this quality assurance project plan
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 2 of 8

TABLE 14-1. MQOs AND ASSOCIATED QC ACTIVITIES FOR THE PM2.5 STN

Measurement Frequency

Acceptance Criteria

(MQO)a

Corrective Action if Out

of Specification

Samples or

Channels

Filter visual checks before and after

each exposure

free of visible defects record in lab database

and/or field data form;

filter may be discarded

prior to use; flagged or

invalidated after use

all filter types

Collocation with

another chemical

speciation monitor

each sampling

day for 12 minitrends sites. 

Then 7 or 55 sites,

each sampling

day thereafter.

see Table 7-3 for

maximum total error

of various chemical

species 

result used to calculate 

replicate precision of

measurement system

all sampling

media

Temperature:

check monthly +/-2 °C of a certified 

transfer standard

note on QC data form;

troubleshoot; recalibrate

sensor and conduct

recheck; note on QC data

form

all temperature

sensors

audit quarterly +/-2 °C of

independent standard

note on data form;

recalibrate sensor and

conduct recheck

all temperature

sensors

Pressure:

check monthly +/-10 mmHg vs.

certified transfer

standard

note on data form;

recalibrate sensor and

conduct recheck

barometric

pressure

sensor

audit quarterly +/-10 mmHg vs.

independent certified

transfer standard

note on data form;

recalibrate sensor and

conduct recheck

barometric

pressure

sensor

Flow rate:

one-point

operational

check

monthly +/-10 percent of

working standard

troubleshoot (e.g., perform

leak check)

all flow

channels

one-point audit quarterly +/-10 percent vs.

independent transfer

standard

same as above all flow

channels

Blanks:

trip blanks one set every 30 d unspecified at this

time 

N/A one per

channel

field blanks one set every 10

sampling d

30 μg (gravimetric);

other limits to be

developed for

chemical species

concentrations

retroactive

troubleshooting and/or

data validation after

notification by laboratory

one per

channel

aSource: U.S. EPA, 1999.
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 3 of 8

The remainder of this section describes the types of QC checks called for in the PM2.5 STN and the

procedures used to calculate values for the principal QC indicators. QC results should be recorded on

a form or in a field notebook dedicated to this purpose. Figure 14-1 illustrates the QA/QC data report

form proposed for use in the STN program. 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 or repair of a speciation sampler. Detailed

information on multipoint calibrations and repairs should be recorded in the field notebook.

14.1 Quality Control Checks

14.1.1 Checks

A check, for this QAPP, is described as a verification by use of a transfer standard that the sampling

instrument is operating within acceptance limits. Usually, if the check fails to meet specification

troubleshooting would occur that might lead to recalibrating the instrument. Calibration is discussed in

Section 16.

14.1.2 Audits and Independent Checks

The chemical speciation samplers will be audited with an independent transfer standard on a quarterly

basis. Flow rate, temperature, and barometric pressure will be checked. For samplers with multiple

flow channels, each channel and the associated sensors will be audited. The transfer standards are to be

recertified or recalibrated annually. 

14.1.3 Performance Evaluations

EPA has conducted several intercomparison studies of chemical speciation samplers. Intercomparisons

will continue with the 12-site mini-trends network, which will operate annually starting in December

2000.

The STN laboratory must also assess the accuracy of its analytical measurements. This will include

assessment of field blanks and other samples supplied by the EPA QA laboratory. Refer to the STN

laboratory QAPP for more information.
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 4 of 8

QA/QC Form No. PM2.5 STN QA/QC REPORT FORM c. 1 (site retains)

c. 2 (Agency QAM)

c. 3 (Send to Lab)

A. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name

2. Sampler S/N 6. Interval: Month _______ Quarter ______ Special

______

3. Sampler Type 7. Date(s) of QA/QC Checks 

4. Sampler POC 8. Operator’s Name 

B. DATE AND TIME CHECKS (Transfer Standard Name ____________ Transfer Standard ID Number ____________)

Sample display date/time Transfer standard date/time Date and time agree ±5 min? Action takena

C. LEAK CHECKS (Transfer Standard Name ___________________ Transfer Standard ID Number ______________)

Channel number Manufacturer’s specifications met? Action taken and recheck resultsa

1

2

3, etc.

D. TEMPERATURE CHECKS (Transfer Standard Name _____________ Transfer Standard ID Number __________)

Sensor location Sampler display (°C) Transfer standard

(°C) 

Agreement ± 2 °C ? Action taken and

recheck resultsa

Ambient

Filter

Dry gas meter

Manifold

E. PRESSURE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ____________)

Sensor location Sampler display,

(mmHg)

Transfer standard,

(mmHg)

Agreement within

±10 mmHg?

Action taken and

recheck resultsa

Ambient

Manifold

F. FLOW RATE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ___________)

Channel number Sampler display,

(L/min)

Transfer

standard display,

(L/min)

Design flow rate,

(L/min)

Agreement within

± 10 percent?b

Action taken and

recheck resultsa

1

2

3, etc.

Figure 14-1. STN QA/QC report form.
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 5 of 8

14.2 QC Samples

Several types of standard QC samples are defined. The field program will mainly be concerned with

blanks sent by the STN laboratory to assess the effects of field operations and shipping and handling.

14.2.1 Blanks

Field Blanks—These provide an estimate of total measurement system contamination. By comparing

information from laboratory 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 STN laboratory will also determine blank concentrations of analytes for each lot of TeflonTM,

nylon, or quartz fiber filters received. The STN 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 occurring during transport. Trip blanks would be sent to the

field as a normal sample but would remain unopened. They would processed as a normal field sample

and sent back to the laboratory and treated as a routine sample from the point of sample receipt and

beyond.

14.3 Collocated Samplers

Collocated sampling will occur at 7 of the 55 sites in the full STN 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. Workup and interpretation of collocated sampler data

sets are discussed in Section 22.0 of this QAPP.

14.4 Calculations of Accuracy, Bias, Precision, and Completeness

Accuracy is defined as the degree of agreement between an observed value and an accepted reference

value and includes a combination of random error (precision) and systematic error (bias). The
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 6 of 8

Bias

N

Yi Xi Y X

i

N

= − = −

=

∑

1

1

( ) (14-3)

di = Xi − Yi(14-1)

d

X Y

X

i x

i i

i

' =

−

100 (14-2)

following four accuracy checks are implemented in the chemical speciation program:

< Flow rate, temperature, barometric pressure, and other checks against a known standard

< Collocation with an Federal Reference Method (FRM) sampler (gravimetric only)

< Collocation with another PM2.5 speciation sampler (all analytes)

< Balance checks and other laboratory performance audits.

14.4.1 Accuracy of a Single Measurement

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 accuracy of a single measurement, di, can be calculated as

the difference between the measured value and a standard value and is expressed in the same units as

the original measurement.

In addition, accuracy is often calculated as a percent difference from a standard of known value. 

Calculate the percentage difference (d'i) for a single calibration check i is calculated using the following

equation:

where

d’i = percentage difference for a single calibration check

Xi = standard value

Yi = indicated (measured) value

14.4.2 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. The following equation is

used to calculate bias:
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 7 of 8

$

( )

s =

− ∑ −X X

n

i

2

1

(14-4)

where

Xi = standard value

Yi = indicated (measured value)

N = total number of observations in a set of observations

and = averages of all the Yi and Xi values, respectively.

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. 

14.4.3 Calculation of Precision

Precision defines the random variability of a set of measurements and excludes systematic bias. 

Precision is given either in the units of measurement (e.g., standard deviation) or in relative units (relative

standard deviation or coefficient of variation [CV]). Like the calculation of bias, precision calculations

require a set of data collected over a period of time or over multiple observations. 

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 out of the scope of this QAPP but should be considered when performing advanced statistical

analysis of the data.

14.4.4Calculation of Completeness

The goal for completeness is 75%. 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 d sampling was sufficient to meet the DQO for assessing a data trend after

5 yr provided other uncertainties described above are controlled. Significant data loss, however, could

compromise the ability to assess the DQO. 
PM2.5 STN QAPP

Section No. 14

Revison No.: 4.1

Date: 12/00

Page 8 of 8

%C

N N

N

t invalid

t

=

−

× 100 (14-5)

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 yr 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

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.
PM2.5 STN QAPP

Section No. 15

Revision No.:4.1

Date: 12/00

Page 1 of 4

 15.0 Instrument/Equipment, Testing, Inspection and Maintenance

Requirements

This section discusses procedures to test, inspect, and maintain instruments and equipment to be used at

Speciation Trends Network field sites.

15.1 Testing and Acceptance Criteria

The STN will employ a set of testing and acceptance (T & A) criteria that were used to accept FRM

samplers. Table 15-1 lists the 13-step procedure by which final acceptance of each speciation sampler

will occur. If any deficiencies are discovered, the vendor should be called to report the deficiency and

begin the process of resolving the deficiency. Receiving papers, warranty information, and the 13-step

checklist noting the deficiency should be kept on file for reference and to document problem resolution. 

A copy of the completed checklist is sent to the STN Project Officers .

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 room thermometer, ice bath, or other

known 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 STN laboratory are discussed in the QAPP prepared by the

STN laboratory.

15.2 Maintenance

Many items may require maintenance in the STN. Preventive maintenance should be practiced in

accordance with the manufacturer’s instructions given in the operator’s manual and as experience is

gained. This section describes maintenance items for STN field equipment. The STN laboratory

QAPP discusses laboratory equipment maintenance. Maintenance of speciation samplers will become

increasingly important as the equipment ages over this multi-year study. STN site operators and

managers 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. Others may be added to this list as experience is gained.
PM2.5 STN QAPP

Section No. 15

Revision No.:4.1

Date: 12/00

Page 2 of 4

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 a diskette.

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 h as would be done for routine sampling.

Certifying Official’s Signature __________________Date______ Circle one 66 Accept? Reject?

Note: Send copy of completed checklist to STN PO.
PM2.5 STN QAPP

Section No. 15

Revision No.:4.1

Date: 12/00

Page 3 of 4

TABLE 15-2. PREVENTIVE MAINTENANCE OF STN FIELD EQUIPMENT

Maintenance Item Recommended Frequency

PM2.5 Speciation Samplers

1. Inspect and empty water collection bottle (f applicable).

2. Clean or change out impactor well (if applicable).

3. Check sampling intake lines/hoses (if applicable).

Each visit to site

Every 5th sampling day

1. Clean sampler inlet surfaces.

2. Clean impactor housing and jet surfaces (if applicable). Examine O-rings.

3. Clean interior of sampler case (if applicable).

4. Clean impactor downtube (if applicable).

5. Inspect denuder for breakage (RASS and MASS only). Replace denuders with

freshly coated ones and return used denuder to laboratory for refurbishment.

6. 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 and impactor assembly (if applicable). Apply 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.

4. Clean cyclones and manifolds upstream of sampler module.

5. Inspect and service O-rings of impactor assembly.

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

Flow rate transfer standard

1. Recertify vs. NIST standards.

2. Replace batteries (if applicable).

3. Visually check orifices for dust or breakage.

Temperature transfer standards (digital thermometer and TEOM)

1. Recertify vs. NIST standards.

2. Replace batteries.

3. Inspect probe tip and connecting cord.

Pressure transfer standard

1. Recertify vs. NIST standards.

2. Replace batteries.

Annually

As needed

Each use

Annually

As needed

Each use

Annually

As needed

15.2 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 STN 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 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 laboratory and field site).
PM2.5 STN QAPP

Section No. 15

Revision No.:4.1

Date: 12/00

Page 4 of 4

< Speciation sampler

• O-rings for downtube connections (if applicable)

• Connecting pressure tubing and compression or other types of fittings

• Filter packs or cassettes (to be forwarded to STN laboratory)

• Denuders (to be forwarded to STN laboratory)

• Sampling lines/tubing (as applicable)

• Fuses

< Digital thermometer, pressure device and orifice-based flow transfer standard

• Spare batteries

• Spare temperature probe

. • Spare tubing
PM2.5 STN QAPP

Section No. 16

Revision No.: 4.1

Date: 12/00

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 standard or

instrument to report, or eliminate by adjustment, any variation (deviation) in the accuracy of the

item being compared. The purpose of calibration is to minimize bias. For PM2.5 chemical speciation

instruments, calibration activities follow a two step process:

1. Certifying the calibration standard and/or transfer standard against an authoritative standard

(usually the National Institute of Standards and Technology).

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

STN 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. 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 gravimetric monitoring program. The speciation samplers are identical to the gravimetric

samplers with respect to ambient temperature, barometric pressure, date/time, and elapsed time. They

may differ from the gravimetric 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. 

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
PM2.5 STN QAPP

Section No. 16

Revision No.: 4.1

Date: 12/00

Page 2 of 6

performed. After installation, regular checks and maintenance are carried out by the STN 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.

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 barometric pressure against the working pressure

standard,

< Verification/calibration of volumetric flow rate meter in the samplers against the working

flow rate standard, and

< Verification of the sampler’s internal clock against a timepiece.

Temperature Probes—The STN chemical speciation sampler has both ambient and internal

temperature probes. The STN 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 NIST-traceable 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 (operators watch) can be set against an atomic clock that can be found on the Internet

(available online at http://www.fyi.net/~tharvey/time.html) 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.

Calibration Standards—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.
PM2.5 STN QAPP

Section No. 16

Revision No.: 4.1

Date: 12/00

Page 3 of 6

Temperature, barometric pressure, and flow rate transfer standards that are used to perform routine

verifications of STN chemical speciation samplers should be recertified at the same intervals as the

transfer standards for the PM2.5 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 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—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. The records

will normally be controlled by the STN 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).

16. 3 Calibration and Verification of Laboratory Instrumentation

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

STN contract laboratory.
PM2.5 STN QAPP

Section No. 16

Revision No.: 4.1

Date: 12/00

Page 4 of 6

TABLE 16-1. ACCEPTANCE CRITERIA AND CALIBRATION AND

MAINTENANCE FREQUENCIES FOR PM2.5 CHEMICAL SPECIATION SAMPLERS

Criteria Acceptance

Criterion

Frequency SOP Comments

Field Calibrations and Routine Checks

One-point flow rate

check

±10 percent of

transfer standard

Monthly A-2, A-3,

A-4

Same as for gravimetric

samplers. Applies to all flow

channels.

External leak check <80 mL/min Every five sampling

events or when

impactor serviced

A-2, A-3,

A-4

Same as for gravimetric

samplers. Applies to all flow

channels.

Internal leak check <80 mL/min If external leak

check fails

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 A-2, A-3,

A-4

Same as for gravimetric

samplers. Applies to all

temperature sensors.

Pressure

verification

±10 mmHg Monthly A-2, A-3,

A-4

Same as for gravimetric

samplers.

Clock/timer

verification

1 min/mo Monthly A-2, A-3,

A-4

Same as for gravimetric

samplers.

Other calibrations

as specified by

manufacturer

per manufacturer’s

SOP

Per manufacturer’s

SOP

Quarterly Checks and Audits

External leak check <80 mL/min Quarterly Same as for gravimetric

samplers. Applies to all flow

channels.

Internal leak check <80 mL/min If external leak

check fails

Same as for gravimetric

samplers. Performed as a

troubleshooting procedure

only. May not be applicable

to all sampler designs.

Temperature audit ±2 °C Quarterly Same as for gravimetric

samplers.

Pressure audit ±10 mmHg Quarterly Same as for gravimetric

samplers.

Flow rate audit ±10 percent of audit

standard 

±10 percent of

design flow rate

Quarterly Same as for gravimetric

samplers. Applies to all flow

channels.
TABLE 16-1. (continued)

PM2.5 STN QAPP

Section No. 16

Revision No.: 4.1

Date: 12/00

Page 5 of 6

Criteria Acceptance

Criterion

Frequency SOP Comments

 Initial Installation Calibration

Temperature

calibration

±2 °C of standard On installation,

annually, or if

verification is failed

Applies to ambient

temperature and all internal

filter temperature sensors.

Pressure calibration ±10 mmHg On installation, then

annually or if

verification is failed

Same as for gravimetric

samplers.

 Multipoint flow

rate calibration

±10 percent of

transfer standard at

each flow rate

On installation,

annually ,or if

verification is failed

Applies to all flow channels

individually.

Design flow rate

adjustment

±2 percent of

design flow rate

As needed Applies to all flow channels

individually.

Sampler Maintenance

Impactor cleaned/changed Every five sampling

events

If applicable to sampler

design. External leak check

should be performed

immediately after impactor

maintenance.

Inlet/downtube

cleaning

cleaned Every 15 sampling

events

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. 

To be determined.

Consult operator’s manual

Circulating fan filter

cleaning

cleaned/changed Monthly Same as for gravimetric

samplers.

Manufacturerrecommended

maintenance

per manufacturer’s

SOP

Per manufacturer’s

SOP

Recertification of Standards (audit and calibration)*

Flow rate transfer

standard

±2 percent of NISTtraceable standardAnnually Same as for gravimetric

samplers.

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.

* Recertifications may be done in-house, by the manufacturer of the device, or by a third party. 
PM2.5 STN QAPP

Section No. 16

Revision No.: 4.1

Date: 12/00

Page 6 of 6

TABLE 16-2. CALIBRATION STANDARDS FOR PM2.5 CHEMICAL SPECIATION

SAMPLERS

Description of Calibration

Standard

QA Objective

Acceptance

Criteriona

Listed Uncertainty

for Calibration

Standard

Manufacturer

of Calibration

Standard

Model Number

of Calibration

Standard

Digital thermometer ±0.5 °C

Digital pressure gauge ±0.7 percent b

Flow meters ±2 percent

a Acceptance criteria taken from page 1 of Element 16 in the Quality Assurance Project Plan for the PM2.5

Performance Evaluation Program (U.S. EPA, OAQPS. February 1999).

b The pressure criterion (±5 mmHg) is equivalent to ±0.7 percent of atmospheric pressure (760 mmHg).
PM2.5 STN QAPP

Section No. 17

Revision No.: 4.1

Date: 12/00

Page 1 of 2

17.0 Inspection/Acceptance for Supplies and Consumables

17.1 Purpose

This section establishes and documents a system for inspecting and accepting all collection site supplies

and consumables that may directly or indirectly affect the quality of the STN data. Documented

inspection and acceptance criteria will ensure the consistency of sampling media and associated

supplies and thus minimize their effect on analyte concentrations. The inspection and acceptance

process is of utmost importance to data sets that will be compiled for years to detect concentration

trends. The quality of the supplies and consumables used in the STN laboratory is of utmost

importance to the quality of the data set. Sampling media and chemicals used to calibrate the analytical

instruments are major concerns. The STN laboratory quality assurance project plan should be

consulted for details.

17.2 Critical Supplies and Consumables

17.2.1 Field Sites

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 STN. The State or local 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 STN are also operating routine samplers for the mass PM2.5 Program, the calibration

and check standards may be used for the STN since they should meet the performance standards. 

The contract laboratory will care for and track the cassettes and modules used in servicing the sampling

and analysis needs of the sites but will not carry them on its own inventory list.

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 State or

local 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-yr period
PM2.5 STN QAPP

Section No. 17

Revision No.: 4.1

Date: 12/00

Page 2 of 2

TABLE 17-1. STN FIELD EQUIPMENT AND SUPPLIES

Quantity

per Site

Operator Equipment and Supply Description

Vendor/

Catalog No. Make/Model No.

Speciation Sampling Equipment and Supplies

1 Transport cases for loose equipment, supplies

1 Speciation sampler

1 Speciation sampler operating manual

6 sets Filter cassettes or sampling modules for speciation

sampler 

To be

determined

Denuders for acid gases

Custody and field data form for each sample run

Sample shipping containers/ice packs (from lab)

Max./min. thermometer (if required)

Mounting Equipment and Tools

1 Tool kit

Calibration/Check Standards and Related Equipment

1 Flow rate adapter (size depends on sampler brand)

1 or more Flow transfer standard (Chinook, BIOS, dry gas meter)

1 Pressure transfer standard (portable barometer)

1 Digital thermometer (or thermocouple calibrator)

Spare Parts

O-rings, tubing, fuses, impactor oil (if applicable),

impactor filters (if applicable), compression fittings

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 NIST-traceable that is

subject to wear and tear during use (for example, temperature, pressure, and flow rate check devices)

should be returned annually to the vendor or an appropriate metrology laboratory for cleaning,

servicing, and recertification vs. NIST standards.

State and local 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. Section 15.0 of this QAPP contains the STN testing and

acceptance checklist, which State agencies may find useful to accept or reject a new sampler based on

the operational evaluation steps given in the T&A checklist. 
PM2.5 STN QAPP

Section No. 18

Revision No.: 4.1

Date: 12/00

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 STN. These data are obtained from nonmeasurement sources and historic or concurrently

acquired databases not under the direct control of the STN.

18.1 Acquisition of Nondirect Measurement Data

The STN 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

Physical and chemical 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) and Lange’s Handbook.

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 STN 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 trend exist. Characterization of PM2.5

constituents in rural or regional environments (especially when data sets are combined with IMPROVE

data) is also possible if some sites are in transport and/or background locations. To select the best

locations for trends 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
PM2.5 STN QAPP

Section No. 18

Revision No.: 4.1

Date: 12/00

Page 2 of 2

of urban areas. Information about local emissions sources will be needed, for example, to avoid

locating a sampler too close to a particle source such as a chimney or an industrial vent. Information in

State or local agency databases 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. 
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 1 of 12

19.0 Data Management

19.1 Overview

This section presents information on how field and analytical data for the STN 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. This section addresses these data management

topics: recording, transformation, transmittal, reduction, validation, analysis, management, storage, and

retrieval. For the latest detailed information, refer to the STN Laboratory QAPP for chemical

speciation of PM2.5 filter samples. 

Data for the STN come from several sources at both the STN Laboratory and the reporting

organizations that perform the field operations. The general flow of data between organizations is

illustrated in Figure 19-1. This figure emphasizes the organizational responsibilities, database systems,

and major operations. The STN laboratory, shown at the top of Figure 19-1, is responsible for

integrating data from the various laboratories with the shipping/receiving and chain-of-custody

information for the sample module sets provided to the ROs. After level 0 and level 1 validation, the

data are sent monthly through the Delivery Order Project Officer to the respective ROs for completion

of data validation. The accepted data sets are then sent by the ROs to RTI for upload to the

Aerometric Information Retrieval System (AIRS) database.

The following list describes the data management activities in more detail. This list is presented in

chronological order:

1. Presampling Laboratory Activities. This stage is conducted by the STN laboratory and

includes inputting weight values for the TeflonTM filters, filter lot acceptance test results, quality

control (QC) information such as the background concentrations of analytes on blank filters,

and records of laboratory temperature and humidity conditions during weighing sessions. 

Secondly, information about shipping and COC are entered so that shipments of modules to

and from the various ROs can be tracked.

2. Field Activities. These data are initially written on the CAFDF and input by the STN

laboratory to its database management system (DBMS). Items include data on operation of the

speciation sampler (sample identification numbers, volume collected, ambient 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 field SOPs

contained in the appendices to this QAPP.
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 2 of 12

Filter Lot

Acceptance 

Records

STN

Laboratory 

DBMS

Distribution to

 the RO's to

final validation

Internal QA/QC Data:

-COCD Forms 

-Logbooks 

-Shipping Records

-Audit Results 

-Ca. Data, etc. 

Data 

Validation

Level 0 & 1

STN Laboratory

Monthly Data 

Reports in

hardcopy and

electronic 

format

DOPO

Filter

pre-Exposure

Weights

Analytical 

Results

Chain of

Custody Data

Records

SHAL

Shipping 

Records

Fully 

Validated

Data Set

Final Data

Validation

(all levels)

RO's Data

System

AIRS Upload

Reporting Organization

Figure 19.1 STN data flow overview

3. Postsampling Laboratory

Activities. The STN

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.

4. Data Validation at the

STN Laboratory. Data

validation will be carried

out at both the STN

laboratory and at the ROs.

The STN laboratory will

base its validation on

CAFDF forms, shipping

records, and analytical

QA/QC information. 

These activities are

explained in Section 22.0

of this QAPP.

5. Data Reporting to the DOPO. The STN laboratory will transmit its validated data monthly to

the DOPO, who will pass the hardcopy and electronic data sets to the appropriate ROs. Data

from the laboratory and field are combined at this stage of operations and expressed in terms of

concentration units such as micrograms per cubic meter (:g/m3) of air. The electronic data set

will be in the AIRS format and accompanied by a QC report that further describes the flagging

of the data.

6. Data Validation Activities at the ROs. The ROs 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.
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 3 of 12

19.2 Data Management Activities at the STN Laboratory

Data management activities in the STN laboratory are described in the QAPP for laboratory analysis of

PM2.5 filters.

19.3 Data Management Activities at the RO

This section describes in more detail the data management activities and responsibilities of the ROs. 

These data management activities should be conducted in accordance with the recommended practices

for data management described in Section 19.4. 

19.3.1 Shipping and Receiving Records

The first stage of data management activities at the RO begins with receipt of a sampling module set

containing a partially completed CAFDF. The RO should record whenever a set of sampling modules

is received or shipped. Recording the following information in the RO's shipping/receiving area is

recommended:

Before Sampling:

< Date an unexposed set of sampling modules is received

< Site and sampling date that the module set is to be used

< Condition of the shipping container (if the container was damaged in shipment, the STN

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 drop the modules at the site)

After Sampling:

< Person bringing the exposed set of sampling modules back to the shipping area

< Site and sampling date that the sampling module set was exposed

< Condition of the modules and the external shipping container

< Whether the ice substitute was precooled as required

< Federal Express air bill number and destination (the STN laboratory's address should be

pre-printed on air bills supplied in each module set)

< Date and time that the cooler package was sent

< One copy of the multipart CAFDF should be retained by the RO 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 RO should develop its own system for maintaining shipping and receiving

records. 
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 4 of 12

19.3.2 Custody and Field Data Form

The CAFDF is shown in the sampler-specific SOPs in Appendix A and in Section 12.0 to this QAPP. 

The field operator is responsible for filling the form in fully, completely, and accurately. The handwritten

notations on the form are the only source that the STN 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 so on during the sampling

period

< 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 CAFDF will be formatted so that there is a specific space for each item above and will be

customized for the different speciation samplers to be used in the STN program. The operator will

repack the exposed modules and return the top copy of the CAFDF in the cooler package. The

operator is responsible for keeping the middle copy of the CAFDF and returning it to the designated

person at the RO for filing and later use in data validation.

19.3.3 Data Management Activities during Data Validation by the RO

Approximately 30 to 60 d after sampling has occurred, the DOPO will give each RO a data summary

and QC report prepared by the STN laboratory. The data summary will include an electronic file of

partially validated AIRS-formatted data that will require further validation by the RO. The STN

laboratory will have performed the following level 0 and level 1 validations on the delivered data:

< Data attribution and COC verification

< Validation of laboratory analytical data

< Screening for data input/output problems.

Refer to Section 22 of this QAPP or the STN laboratory QAPP and its accompanying data

management SOPs for a full description of the data validation procedures that it will apply and the

checklist that is used.

The QC report delivered with the data file will include the following information that the RO will need in

order to complete the data validation:
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 5 of 12

< Data records with missing or uncertain attribution or COC information (principally the

site/date of exposure or defective 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 STN

laboratory.

The RO will use its in-house records 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 flagged due to a laboratory problem. Questions about flags applied by the STN

laboratory should be sent through the DOPO.

After reviewing the STN laboratory's QC information, the RO 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

handling methods and means for ensuring correct inputs/outputs during data handling are described in

Section 19.4.

19.3.4 Reporting Data to AIRS

After the data set has been finalized, each RO is responsible for returning the data set to the STN

laboratory for reporting to AIRS. The DOPO should be notified whenever a finalized data set is

transmitted to the STN laboratory for AIRS reporting.

19.4.Recommended Data Management Practices

This section describes recommended data handling practices that are applicable to the STN laboratory

and to the ROs. It is expected that all organizations participating in the STN program will follow EPA

guidelines such as good automated laboratory practices (GALPs).

19.4.1 Manual Data Entry

Manually entered data will include entries from the CAFDFs 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 database. 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 custody and field data
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 6 of 12

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. 

This is one of the most cost-effective methods for entering large amounts of data with

extremely high accuracy.

< Range Checking—Many parameters lend themselves to checking for reasonable range

during or after data input. 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.

19.4.2 Electronic Data Entry

The data sets sent from the STN laboratory to the ROs in electronic format will be delivered in AIRS

format. The data set will be visually reviewed before the file is closed and transmitted to the DOPO. 

No further checking of data integrity will be done for electronic file transfers because these are internally

validated by the transmission medium.

The site operator will download a full set of information retained in the memory of the speciation

sampler by use of a download program and a laptop computer or data transfer device connected to the

sampler’s RS232 port. The diskette 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. However, any information entered by the site operator (AIRs code, filter

numbers etc.) should be checked. 

19.4.3 Sample and Data Tracking

Within the STN laboratory, a laboratory information management system will track 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 CO form. Module sets sent from the

STN laboratory to the ROs will be tracked in the laboratory's database system. These processes will

be described further in the STN laboratory QAPP and the data management SOP. 

Each RO must also develop methods for tracking, shipping, and receiving data and for filing custody

and field data forms, audit reports, and other STN-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 NAMS is encouraged. Recommendations for file

retention of documents and records are given in Section 9.0 of this QAPP.

19.4.4 Data Recording, Security, and Archiving

ROs and the STN laboratory should address data security in their data management processes for STN

and other reportable environmental data. ROs should implement practices such as the following (or

equivalent):
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 7 of 12

< Organizations must perform regular backups of the STN database.

< As insurance against fires and other problems affecting an entire building, backup sets

should be kept off-site.

< Weekly full backups of the database, 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 STN data. 

< Dial-in modem access to computers or networks containing unreleased STN data should

be password-restricted, if possible, to authorized users.

< Access to unreleased STN data should be restricted to personnel working on the STN

program.

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 STN laboratory

or RO for the life of the contract or for a term of 5 yr, unless otherwise specified by EPA. The

Location or Responsibility column 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 AIRS. 
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 8 of 12

< Data validation must include 100 percent manual review of both flagged and unflagged

data. A qualified reviewer, such as a qualified analyst or the QA Officer, should examine

each entry for reasonableness before it is reported out of the organization.

< Completeness checks of the data set must be included in the validation system. This can

sometimes be automated, particularly for within-record checks. The RO should verify the

completeness of the data set created by the STN laboratory by checking that all exposures

have been accounted for by comparison with its custody 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 19-1. LABORATORY DATA RECORD ARCHIVAL SUMMARY

Type of Record

LaboratoryRO

Data Archival Location or Responsibility

Completed custody and field data forms T T Lab: sample handling and archival 

laboratory; RO: STN Manager's files

Shipping records T T Shipping department files

Internal custody forms T Sample handling and archival laboratory

Analytical and weighing raw data and instrument

traces

T Weighing 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 files

QA records, including audit checklists and audit

reports

T T QA files

Copies of all partially validated data sets sent from

the STN laboratory to the DOPO

T STN Laboratory Program Manager's files

Copies of all fully validated data sets sent from

the ROs to AIRS

T RO STN Manager's files

Purchasing records related to the STN program T STN Laboratory Program Manager's files

Correspondence with the DOPO, including

consolidated sample requests

T T RO: STN Manager's files

Lab: Program Manager's files

Correspondence and business records with

subcontractors involved with the STN

T Program Manager's files

Training records T T Program Manger's files
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 9 of 12

Table 19-2 summarizes the validation checks applicable to the STN data sets.

Refer to Sections 22.0 and 23.0 of this QAPP for specific data validation procedures to be applied. 

Validation procedures applicable to the STN laboratory are described in the laboratory QAPP.

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

AIRS. The STN laboratory database may contain a superset of the AIRS flags for internal use to

facilitate QC reporting; however, these flags will be mapped onto the set of approved AIRS flags

before they are released from the laboratory. 

This section will be updated to include a summary of AIRS data flags after the parameter codes

for PM2.5 chemical speciation data have been issued by EPA.

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 STN 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

TABLE 19-2. VALIDATION CHECK SUMMARIES

Type of Data Check

Electronic

Transmission and

Storage Manual Checks

Automated

Checks

Data parity and transmission protocol checks U

Data review U

Date and time consistency U U

Completeness of required fields U U

Range checking U

Statistical outlier checking U

Manual inspection of charts and reports U

Sample batch data validation U
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 10 of 12

TABLE 19-3. RAW DATA CALCULATIONS

Parameter Units Conversion type Equation

Volume of air

sampled through

filter

m

3 Calculated from average flow rate (Qavg) in L/min and

total elapsed sampling time, t, multiplied by the unit

conversion (m3/L)

Va = Qavg × t × 10-3

Total mass on filter

(M2.5)

:g Calculated from filter postsampling weight (Mf) and

filter presampling weight (Mi) in mg, multiplied by the

unit conversion (:g/mg)

M2.5 = (Mf - Mi) × 103

PM2.5

concentration

(CPM2.5)

:g/m3 Calculated from laboratory data and sampled air

volume

CPM2.5 = M2.5/Va

< 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 (this is an

instance when the audit trail entry is not record-specific).

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 19-3 summarizes transformations

applied to analytical data to produce volume, mass, and concentration data. 

NOTE: Table 19-3 is applicable to the general categories of analytes to be produced by the

STN 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 speciation sampler.

19.7 Data Transmittal

Transmittal of data occurs when one person or location transfers data to another or when data are

copied from one form to another. Examples of data transmittal include copying entries from a notebook

to a data entry form, keying information from a handwritten data entry form to a computer file, and
PM2.5 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 11 of 12

transferring data electronically via telephone or computer network connections. 

Table 19-4 summarizes data transfer operations and the QA measures applied to ensure accurate and

complete transfers into the organization's database management system. 

19.8 Data Reduction

Data reduction is the process of aggregating and summarizing results so they can be understood and

interpreted. Examples of data reduction products are

< Average PM2.5 mass or species concentration

< Accuracy, bias, and precision statistics based on accumulated FRM and speciation sampler

data

< 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.

19.9 Data Analysis

Management of data analysis techniques and products is beyond the scope of the STN field or

laboratory QAPP. Management procedures will be developed by data analysis participants.

19.10 Data Storage and Retrieval

STN laboratory data storage and retrieval techniques are described in the laboratory QAPP and

SOPs.

Data storage and retrieval techniques for the ROs should be described in their system documentation or

through in-house SOPs developed for the STN 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 STN QAPP

Section No. 19

Revision No.: 4.1

Date: 12/00

Page 12 of 12

TABLE 19-4. DATA TRANSFER OPERATIONS

Description of Data

Transfer Originator Recipient QA Measures Applied

Keying weighing data

and chemical analysis

results into the STN

laboratory's database

Laboratory analyst

(handwritten data forms)

Laboratory analyst

(enters data into the

database 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 data

C Field site sampler

C Laboratory instruments

Field auditor; field site

operator

laboratory auditor;

laboratory analysts

Laboratory data clerk Field data entries are

checked by field operator.

Laboratory data checked

by laboratory supervisor

and spot-checked by QA

staff

AIRS data summaries Laboratory data clerk and

data supervisor

AIRS (EPA) (via the

DOPO)

Entries checked by

laboratory data clerk and

data supervisor; OAQPS

QA Officer

Finalized AIRS data

summaries

STN laboratory AIRS Checked by the

laboratory’s Program

Manager or QA Officer

The contract laboratory will reduce data consistently to an agreed upon format in order to

upload it to AIRS. Each RO may choose to develop additional data reduction procedures for

data interpretation to assist with data validation and reporting of its own data. Development of

unified procedures to be applied across the STN is encouraged. EPA’s Office of Air Quality,

Planning and Standards will assist in coordinating the development of such procedures. Simple

reports are easily generated using a PC equipped with a modern spreadsheet program such as

Microsoft Excel® or Lotus® or with a more specialized statistical package such as SAS®.
PM2.5 STN QAPP

Section No. 20

Revision No.: 4.1

Date: 12/00

Page 1 of 6

20.0 Assessment and Response Actions

20.1 Types of Assessments

The following types of assessments will be performed by the STN:

< 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/G3). 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 follow the specifications and guidance given in the American Society for

Quality Publication ANSI/ASQC E4-1994.
PM2.5 STN QAPP

Section No. 20

Revision No.: 4.1

Date: 12/00

Page 2 of 6

20.2 Assessment Frequency

Assessments will be performed at the frequency described in Table 20-1. 

Table 20-1 Types of Assessments for the STN

Agency Type of Assessment Agency Assessed Frequency

NAREL TSA, DQAs, MSRs and PEs RTI Annually

R&IE TSAs State and local

agencies

Annually* 

R&IE Performance Audits State and local

agencies

Annually*

OAQPS-EMAD TSAs RTI, NAREL, State

and Local agencies,

Regional offices and

R&IE

As needed by

EMAD

determination

OAQPS-EMAD MSRs RTI, NAREL, State

and Local agencies,

Regional offices and

R&IE

As needed by

EMAD

determination

Regional Offices Network Reviews State and local

agencies

Once every 3

years

 * Not all STN samplers will be audited. Perhaps up to 25 % of the network annually. 
PM2.5 STN QAPP

Section No. 20

Revision No.: 4.1

Date: 12/00

Page 3 of 6

20.3 Acceptance Criteria

Assessments will be based on the acceptance criteria to be developed based on the DQOs and findings

from the 12-site mini-trends network. Figure 20-1 outlines the TSA acceptance criteria for field and

laboratory operations for the gravimetric portion of the STN.

20.4 Assessment Schedules

TSAs for the 12-site mini-trends network will be conducted between 3 to 6 months of the start of

sampling. TSAs for the remaining sites in the full PM2.5 STN will be conducted within 1 year of the

start of sampling.

20.5 Assessment Personnel

Assessors should have a minimum of 4 years' 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 assessment, technical, 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 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 STN. In general,

they need to be able to evaluate the PM2.5 STN's scope of work, its management system structure, and

its operating procedures and to judge the PM2.5 STN's adequacy compared to this QAPP.

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 PM2.5 STN. Depending on the scope of the technical assessment,

assessors may need to meet additional qualifications, including health and safety requirements.

Technical specialists, who have specialized knowledge of PM2.5 STN 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 STN.
PM2.5 STN QAPP

Section No. 20

Revision No.: 4.1

Date: 12/00

Page 4 of 6

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.

< The assessors should be free from personal and external barriers to independence,

organizationally independent, 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. 

< 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 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 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. 

20.6 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 EPA and the assessed organization. The

report must include
PM2.5 STN QAPP

Section No. 20

Revision No.: 4.1

Date: 12/00

Page 5 of 6

< 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 STN activity being assessed, the purpose and

date(s) of the assessment, the particular parameter evaluated, and a brief description of

the assessment process;

< Summary and conclusions of the assessment and proposed response actions; and

< Attachments and appendices that include all evaluation and finding information.

Typically, two reports are produced: the draft findings report (DFR) and the quality assurance final

report (QAFR). The lead assessor is responsible for producing the DFR 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 DFR might simply be a listing of the positive findings as well as the findings that call for some

corrective action. A full DFR should be written with 15 working days of the audit.

The DFR will be submitted for review by the EPA Speciation QA Coordinator and the EPA project

official. The EPA Lead Assessor will send the DFR, through the EPA project official, to the assessed

organization for its comments. The assessed organization should be given the maximum opportunity to

respond to the DFR. 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, if a follow-up assessment is required, and when it is appropriate to close out the

assessment.

After the assessed organization's comments have been addressed, the FR should be prepared. The FR

should be similar in format to the DFR and should be based on the DFR. 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 FR

should be submitted to the EPA Speciation QAC and copies should be sent to the EPA project official

and to the assessed organization.

Documentation for TSAs and network reviews will be archived at the EPA Regional Offices and

tracked using the AIRS. The results of MSRs will be on file in EPA’s Monitoring and Quality

Assurance Group, which is ultimately responsible for implementing the PM2.5 monitoring network.

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 and threats to personnel health and safety. Verbal approval from responsible

parties suffices under these conditions.
PM2.5 STN QAPP

Section No. 20

Revision No.: 4.1

Date: 12/00

Page 6 of 6

 OAQPS uses a response action form to document any nonconformances that require actions and the

resolution of them. This form includes the signatures of the individual identifying the need for response

action, the EPA project official, the EPA Speciation QAM, and the individual responsible for

implementing the response action. The problem requiring response action, the proposed response

action, and the approach for evaluating the response action should be described.

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 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 STN QAPP

Section No. 20

Revision No.: 4.1

Date: 12/00

Page 7 of 6

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.

U.S. Environmental Protection Agency. 1994. Guidance for Preparing, Conducting, and Reporting

the Results of Management Systems Reviews. Draft EPA Publication No. EPA QA/G-3.

Washington, DC.

U.S. Environmental Protection Agency. 1998a. 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. 1998c. Guidance for Data Quality Assessment: Practical

Methods for Data Analysis. EPA Publication No. EPA QA/G-9. Washington, DC.

U.S. Environmental Protection Agency. 1999. Guidance on Technical Audits and Related

Assessments for Environmental Data Operations. EPA Publication No. EPA QA/G-7. Washington,

DC.

U.S. Government Accounting Office. 1994. Government Auditing Standards. Washington, DC.
PM2.5 STN QAPP

Section No. 21

Revison No.: 4.1

Date: 12/00

Page 1 of 5

21. 0 Reports to Management

This section describes the type, content, distribution, and frequency of submission of QA reports for the

PM2.5 Speciation Trends Network. Regular QA reporting to management serves the following needs:

< Documentation of adherence to schedules for delivery of equipment, data, and reports

< Documentation of deviations from approved QA and SOPs, and the impact of these

deviations on data quality

< Analysis of the potential uncertainties in decisions based on the data.

Section 21.1 discusses how QA information for the new STN sampling sites, as part of the NAMS

network, will be reported along with other NAMS QA data by the reporting organization. Section

21.2 describes additional QA reporting and information sources that are applicable to the STN

sampling sites during the implementation phase of the program.

21.0 NAMS Reporting

As part of the NAMS network, the STN must adhere to basic reporting schedules, as described in the

Quality Assurance Handbook for Air Pollution Measurement Systems, Volume II, Part 1, Section

16 (EPA 454/R-98-004, August 1998). The handbook should be consulted for recommendations and

suggestions regarding report preparation and formats. Table 21-1 lists standard QA reports to

management that are applicable to the STN. A reporting organization may have other reports to add to

the list or may create reports that are combinations of those listed in the table.

Corrective Action Reports—Corrective Action Reports (CARs) for the STN should be modeled on a

reporting organization's existing CAR system, if possible. The CARs themselves are typically retained

by the organization, but summaries and narratives based on CARs should be included in the annual QA

report to management. The CAR file is also subject to system audit to ensure that the file is being

maintained and that CARs are being turned in and acted upon as needed.

Control Charts—The control chart is primarily a tool used internally to maintain control of an

organization’s quality systems. Each reporting organization should define a control charting program

that meets its needs. Some considerations are as follows:

< What parameters should be charted? For the STN field program, regular flow checks

against a standard reference device and temperature sensor or transducer output in

response to a standard input should be considered for charting. 

< How frequently to chart? Each measurement of the same standard or reference should be

charted. Avoid mixing results obtained from different standards on a single control chart.

< How to calculate control limits? Parameters may be assessed against fixed limits rather

than by statistically derived limits. Variations are frequently encountered (for example,

certain parameters may have only one control limit).
PM2.5 STN QAPP

Section No. 21

Revison No.: 4.1

Date: 12/00

Page 2 of 5

Table 21-1 Types of Assessment Reports 

Type of Report Contents Report Author

Suggested Reporting Frequency

As

Required Monthly Quarterly Yearly

Corrective

Action

Request

Description of problem;

recommended action;

feedback on resolution

EPA Regional

Office Ž

Control Chart Repetitive activity; plot

of control limits vs.

time. Update whenever

a new check or

calibration is

performed.

STN site

operator or

State/local

Agency Ž Ž

SelfAssessment

Results

Summary of internal

technical systems

audit, audits of data

quality, and

performance evaluation

results;

recommendations for

action, as needed

State and

Local

Agencies

Ž Ž

Independent

Assessment

Results

Summary of external

technical systems

audits, audits of data

quality, and

performance

evaluations; corrective

actions if

unsatisfactory results

(out of limits)

EPA Regional

Office, NAREL

and R&IE 

Ž

Data Set

Review

Notes on Level 2 and

Level 3 data validation;

actions taken to correct

or sequester data

State and

Local

Agencies Ž

Annual

Quality

Assurance

Report to

Management

Executive summary. 

Precision, bias, and

system and

performance audit

results.

EPA Regional

Office

Ž

Annual

Quality

Assurance

Final Report 

Executive summary. 

Precision, bias, and

system and

performance audit

results.

OAQPSEMAD

Ž
PM2.5 STN QAPP

Section No. 21

Revison No.: 4.1

Date: 12/00

Page 3 of 5

< How often should control limits be recalculated? Statistical control limits should be

calculated as soon as there are enough observations to make a reliable sample. Seven or

eight observations are often sufficient. Control limits should not be recalculated too often. 

For a parameter that is charted monthly or quarterly, annual recalculation of control limits

should be sufficient. 

< What if there is a significant process change? Any significant change, such as replacement

of a standard or major overhaul of the instrument, may be reason to restart the control

charting process. This means that existing control limits may not apply to subsequent

observations, and it is necessary to collect a new set of data for calculating revised control

limits.

Self-Assessment Results—STN samplers should be subject to internal technical systems audits, audits

of data quality, and performance evaluations by State and local agencies like all other monitoring

equipment at NAMS sites. If problems are found, corrective actions should be initiated immediately

and documented using the CAR process. Results of self-assessments should be summarized in the next

annual QA report to management. Unsatisfactory results and corrective actions should be discussed.

Independent Assessment Results—Under the STN, external technical system audits, audits of data

quality, and performance evaluations may be conducted by a variety of authorities including EPA

Regional Offices, particularly during the initial phases of network operation. If deficiencies are found,

corrective actions should be initiated and documented. Recommendations and corrective actions should

be discussed in the annual QA report to management.

Data Set Review— Following Level 0 and Level 1 data validation by the STN Laboratory, chemical

species concentration data will be sent to the State and local agencies for review. Upon acceptance of

the level 0 & 1 data it will be entered into AIRS data base. State and local agencies will perform

Level 2 and Level 3 data validation and will report the results of the validation in the annual QA report

to management. These two data validation levels are defined as follows:

• Level 2 data validation involves comparisons with other independent data sets for external

consistency. These comparisons include, for example, intercomparing collocated

measurements.

• Level 3 validation involves a more detailed analysis as part of the data interpretation

process when inconsistencies in analysis and modeling results are found to be caused by

measurement errors.
PM2.5 STN QAPP

Section No. 21

Revison No.: 4.1

Date: 12/00

Page 4 of 5

Quality Assurance Report to Management—The annual QA report to management is a key synopsis

of an organization's operations. It should include an executive summary of all activities; a detailed

summary of accuracy and precision achieved; and discussion of outstanding problems, CARs, and audit

findings. STN samplers should be discussed specifically with regard to achieving the measurement

quality objectives for total error defined in Section 7.0 of this QAPP. Because the STN is a new effort,

systematic problems should be highlighted so that corrective actions can be taken at a networkwide

level. 

Information about the STN monitoring sites operated by an organization should be an integral part of

the annual QA report to management. The QA handbook recommends the following general content

for the annual QA report to management:

< Executive summary—a short section summarizing the report. It should contain a checklist

graphic showing how the reporting organization has met its quality goals during the reporting

period.

< Network background and present status

< Data quality objectives for measurement systems

< QA procedures

< Results of QA activities

< Recommendations for further QA work, with suggestions for improving performance and

fixing problems with equipment, personnel training, infrastructure needs, and so on.

21.2 Additional Quality-Related Reports for the STN

The primary additional quality-related report for the STN is the STN Sample Request. Success of the

STN is critically dependent on planning and communications among the reporting organization, the DO

PO, and the STN Laboratory. Because the laboratory is responsible for distributing filters and sampling

modules on an extremely tight schedule, it must know monitoring schedules and filter requirements well

in advance. This is done through the STN sample request process. Accurate sample requests must be

transmitted to the STN Laboratory no less than 3 months in advance. Ordering the correct number of

filters and other media can be a lengthy process because some manufacturers require several months

for the special filter conditioning required for STN. Firing of quartz filters and conditioning of nylon

filters can take extra time if done at the STN Laboratory. 

The format of the STN Sample Request Form will be developed by the DOPOs, EPA/OAQPS, and

the STN Laboratory. Each sample request should provide the following information for each site, at a

minimum:

< AIRS site code

< Name and address of the STN sampling site

< Name and address of reporting organization

< Name, telephone number, and e-mail address of reporting organization's administrative

contact for the STN program
PM2.5 STN QAPP

Section No. 21

Revison No.: 4.1

Date: 12/00

Page 5 of 5

< Name, telephone number, and e-mail address of STN site operator

< Address for receiving unexposed module sets

< Number of STN samplers operated at the site

< Type of STN sampler(s) (i.e., manufacturer and model number)

< Summary of filters and denuders to be used and analytes to be determined (the normal

configuration for each monitor type will be sent unless exceptions are specified in the

request; these exceptions include extra sampling channels, filter types, and so on)

< Any special requests, such as "extra" modules for the reporting organization's quality control

program

< Scheduled dates of sampling (specific dates are necessary, not "1-in-3" for example)

21.2.1 STN Sample Request Changes

Because the sample requests are made several months in advance, a reporting organization may need to

make changes to previously submitted requests before the sampling date. This could occur because of

a substitution of a different sampler model, change of shipping address, addition of filter channels, and

so on. In this case, the DOPO will be informed immediately so that the STN Laboratory can be

notified of the change. Small changes can usually be accommodated, but changes involving substantially

more filters (e.g., going from every-third-day sampling to daily sampling at a site) might require

significant lead time for the STN Laboratory to accommodate.
PM2.5 STN QAPP

Section No. 22

Revision No.: 4

Date: 6/00

Page 1 of 13

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 will be 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 DQOs. 

Verification and validation are not the same as data quality assessment or evaluation of the DQOs,

processes which are described later in this 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.

After the data set has been subjected to the verification and validation process, it is reported to the

AIRS by the STN Laboratory. Data validation 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 AIRS 

< Number of flagged observations sent to AIRS, categorized by analyte and flag

< Number of invalid observations (not sent to AIRS), by analyte

< Statement of significant corrective actions taken.

22.1 Data Verification and Validation Responsibilities

Verification of data for the PM2.5 chemical Speciation Trends Network is the joint responsibility of the

reporting organization, which runs the field component of the program, and the STN 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.

22.2 Corrective Action Reporting Process

Each reporting organization and the STN laboratory should have a Corrective Action Reporting (CAR)

process in place. Ideally, this process should closely resemble corrective action procedures used on

other monitoring activities conducted by the organization. This process should consist of the following

elements:
PM2.5 STN QAPP

Revison No.: 2

Section No. 22

Date: 6/00

Page 2 of 11

TABLE 22-1. DATA VERIFICATION ACTIVITIES FOR THE PM2.5 SPECIATION TRENDS NETWORK

Verification Activity Reporting Organization STN Laboratory 

Data source attribution. 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 reporting organization should compare the

information on the custody and field data form

(CAFDF) with labels on modules received. Report any

discrepancies to the STN laboratory.

The CAFDF 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 noted and

corrected using the CAR process. 

The STN Laboratory is responsible for

generating the CAFDF 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 CAFDF sheet.

The 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 noted and

corrected using the CAR process.

Results for samples that cannot be positively

identified must be flagged as invalid in AIRS.

Site selection and monitor placement. The reporting organization is responsible for ensuring

that all siting criteria have been met when originally

siting an STN monitor. Continued compliance with

siting criteria should be verified at least annually by the

reporting organization.

If the Laboratory is notified that a particular

STN monitor is in violation of siting criteria,

the corresponding AIRS data may have to be

flagged or invalidated. This decision should be

made jointly with the reporting organization

and EPA.

Integrity of sample handling. This involves verification

that the SOPs for sample handling have been followed

so that the physical integrity of the sample and its

positive identity 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.

The reporting organization should develop and follow

SOPs for sample handling.

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 STN

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 STN laboratory should develop and

follow SOPs for sample handling.

The laboratory should conduct internal audits

and submit to external audits and reviews of its

sample handling and data processing systems.

The STN laboratory should cooperate with

investigations of data integrity initiated by a

reporting 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.
PM2.5 STN QAPP

Revison No.: 2

Section No. 22

Date: 6/00

Page 3 of 11

TABLE 22-1. (continued)

Verification Activity Reporting Organization STN Laboratory 

Checks on sample containers and preservation methods.

Specific checks on sample containers include

examination for physical integrity and comparison with

the CAFDF 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 4oC.

The field operation is responsible for checking the

integrity of shipping containers and individual modules

upon receipt or deployment at the site. The laboratory

should be notified immediately of any damage that may

have occurred in shipment.

The field operator is responsible for chilling the ice

substitute and inserting a properly initialized min/max

thermometer prior to shipping the exposed sample

modules back to the STN laboratory. Use of the

thermometer is optional, depending on the study. 

The CAR process should be followed if a systematic

problem is suspected.

The STN laboratory is responsible for

properly packaging the modules in shipping

containers that include the required number of

ice substitutes.

The STN laboratory is responsible for

notifying the carrier and initiating claims for

shipping damage.

The STN laboratory is responsible for

checking the condition of the shipping

container, its interior temperature, and

individual modules upon receipt from the field.

The STN laboratory must note any

discrepancies that might affect sample validity

in the DBMS. The reporting 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.

Procedures to ensure that data were generated as

specified in the sampling or analysis SOP.

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. 

The STN laboratory and the EPA STN Regional

Coordinator should be notified if serious procedural

issues are raised.

The CAR process should be followed to 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. 

Reporting organization(s) with affected

samples and the EPA Project Officer (PO) for

the STN laboratory contract should be notified

if serious procedural issues are raised.

The CAR process should be followed to

rectify systematic procedural problems.
PM2.5 STN QAPP

Revison No.: 2

Section No. 22

Date: 6/00

Page 4 of 11

TABLE 22-1. (continued)

Verification Activity Reporting Organization STN Laboratory 

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.

Systematic problems that lead to unacceptably large

biases should be investigated and documented using the

CAR process. 

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 STN 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

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 AIRS as soon as feasible. The

reporting organization should also be notified

when its data are flagged.

Data corrections and flagging should be noted

in regular QC reports to management.
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 5 of 13

< A description of the organizational responsibilities and procedures for instituting corrective

actions for the STN program. This would be appropriately placed in the organization's STN

SOPs or in the QMP. If an adequate process already exists in the organization, it is not

necessary to document it separately for the STN.

< 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 annual QC

report to management or equivalent document. Dates and sites of reportable data affected by

the problem should a 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 STN 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. Each SOP that involves the use of multipoint 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

< 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
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 6 of 13

TABLE 22-2. QUALITY CONTROL DATA FOR STN 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 at field sites. Data

should not be numerically corrected for field blank levels. Data should not generally be

invalidated or flagged unless the field blank levels approach environmental levels. The

STN laboratory must notify the reporting organization when a high field blank is found.

Trip blank Joint lab and

field

High trip blanks (with or without a corresponding high field blank) may indicate a

laboratory problem. Corrective actions should begin in the laboratory. Reportable data

should not be corrected for trip blank values. Data should not be flagged or invalidated

unless the blank value approaches environmental levels.

Sampler leak check

failed

Field Leak checks should be investigated as soon as they are detected. Any leak that could

potentially cause a data error (i.e., one that directly affects the flow through one or more

sampling modules) must be documented. If possible, the operator making the leak check

should estimate the extent of the leak. It is not generally possible to provide an exact

correction factor for data taken while a leak exists. The operator should also try to

determine when the leak began. Data back to the last successful leak check may be

suspect. Leaks that could potentially cause an error of 10% or more in actual flow rate

should be brought to the attention of the STN laboratory immediately so that data can be

flagged or invalidated appropriately.

Sampler temperature

or barometric

pressure 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. The

problem should be analyzed by someone with an understanding of how the sampler's flow

depends on the sensor reading; it may be necessary to contact the manufacturer to

determine this. If it appears that the failure could cause an error of 10% or more in

actual flow rate, the problem should be brought to the attention of the STN laboratory so

that data can be flagged or invalidated appropriately.

Filter integrity

inspections

Lab and field Filters that fail the visual integrity inspection 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 CAFDF form. Data entry

personnel should make the appropriate entry when the form is input into the DBMS. 

The original data or CAFDF 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, 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 QC samples are run in the gravimetric and chemical laboratories. In

many cases, instrumentation problems 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 by set limits defined in the

method. 

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 STN program, so reanalysis may be possible at a later time;

however, this is less accurate and more costly than immediate reanalysis.)

If QC results indicate an unacceptable uncertainty and the analysis cannot be reproduced,

the data must be invalidated or flagged. 
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 7 of 13

< Procedures for correcting data taken with out-of-limits calibrations. (This must be done

carefully.) Errors other than simple drift (e.g., noise and nonlinearity) should generally not be

corrected by recalculation; instead, the instrument should be repaired and the samples rerun if

possible.

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; 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; the

positions of vials in an autosampler 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 (typically, either arithmetically or logarithmically

equidistant).

< Enough points should be included 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 provenance is referred to as "Level 0" verification and is

performed by the STN laboratory. The elements below summarize the criteria to be applied during

Level 0 verification of the data set:

< Data source attribution—Verify that the site, date, time, and channel assignments are correct. 

Logbooks, reporting forms, data custody sheets, and electronic data transmittals should be

consulted if a problem of attribution is suspected.

< CAFDF verification—All CAFDF forms for filters and denuders will be checked for

completeness at the STN laboratory before they are entered into the database and archived. 

Missing CAFDF information should be identified by the data entry operator and brought to the

attention of the SHAL supervisor. The laboratory QC supervisor should determine the validity

of any samples for which mandatory CAFDF information is missing. It may be necessary to

contact the reporting organization to attempt to fill in this information.

< Holding times and conditions—The shipping and receiving documentation for all PM2.5

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 AIRS if holding times and shipping/storage conditions

were violated. The STN laboratory QA Manager, in consultation with EPA and the laboratory

supervisor(s), will decide the validity of any samples for which these conditions have been

violated.

< Data transmission and recording integrity—Each error in data integrity that is identified must be
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 8 of 13

investigated and corrected and/or appropriate actions taken. The QC supervisor should

determine whether an uncorrectable data transmission error affects data validity. The CAR

process should be used with problems of a systematic nature.

< Calibration status of sampler and sensors—The reporting organization must have a means for

verifying that 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 AIRS. It is the responsibility of the reporting organization to

identify such data to the STN laboratory because sampling records received by the laboratory

may not include all the necessary information.

< Audit status—The reporting organization must verify that all monthly, quarterly, and other

scheduled audits have been performed on time. Samples taken when a systems audit or

transfer standard recertification was past due must be appropriately flagged in AIRS. It is the

responsibility of the reporting organization to identify such data to the STN laboratory because

sampling records received by the laboratory may not include all the necessary information.

< Operational flags—All operational flags generated by the sampler electronically or recorded on

a data sheet by the operator will be entered into the database. A translation between sampler

codes and AIRS validation flags will be developed as the STN program progresses. Some

serious sampler flags may also result in automatic invalidation of the corresponding sample.

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 AIRS 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 data are not reported to AIRS. 

The following items are involved with validation of the PM2.5 chemical speciation field data:

< Operational data screening—temperature, barometric pressure, flow, and other operational

data are screened for compliance with acceptance limits established for the STN program.

< Filter inspections and other manual verification procedures performed by the site operator and

STN laboratory personnel.

< Validation flags attached and reported—A limited number of flags are provided in AIRS to

document exceptional conditions that apply to specific data items. Only valid data are reported

to AIRS.

< 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 AIRS.
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 9 of 13

< Random data assessment and review—The STN laboratory QA Manager or designee will

manually review up to 5 percent of the data. This review may be done either before or after

transmission to AIRS (any corrections will be made retroactively). The check will include an endto-end check of data entry, calculations, and identification. Original CAFDF files will be examined

and compared to final data printouts. Flagged data will be checked to ensure that flags have been

correctly applied. Reporting organizations are encouraged to implement a similar program of data

checking. 

< Additional validation pertaining to laboratory analyses. 

22.7 Data Screening Techniques used by RTI

The following procedures will be performed by RTI before the data is sent to the DOPOs. 

Preliminary Crosstab Reports by site, POC, and scheduled dates 

These are examined and anomalous results are investigated and corrected. The following crosstab

tables will be generated:

< Chain of Custody form number for each event - include field and trip blanks, routine samples,

unscheduled blanks. Missing cells in the table are investigated.

< total counts of AIRS-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 SHAL 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 1 - 4 below. The QAO reviews these results

and investigates problems. Outlier checks include the following:

< Lower Limit on PM2.5 Mass - Routine samples only

< Mass Balance - 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 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 10 of 13

Entry and Verification of Data Changes from the States and AIRS Data Verification

The following step is done approximately two months after validation of the preliminary data set.

< Changes requested by the state agencies are entered into RTI's data base.

< The AIRS 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 AIRS data table which are compared with previously

generated crosstab tables for that reporting batch. These are inspected as described in step 1

above. 

< After any anomalies are corrected the AIRS 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

Percentile Tail Analyte(s) Sample Type Limit

::g

Flagged

Analytes

Internal

Flag

5.0 UPPER PM25 Mass FIELD BLANK 50.00 PM25 Mass QL1

5.0 UPPER PM25 Mass TRIP BLANK 34.00 PM25 Mass QL1

Table 22-4 Statistical Validation Limits for Routine Data

Percentile Tail Analyte(s) Sample Type Limit

::g/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 QMP

2.0 UPPER Mass Ratio ROUTINE 1.32 all analytes QMP

2.0 LOWER Sulfur/Sulfate Ratio ROUTINE 0.25 ions, XRF QCR

2.0 UPPER Sulfur/Sulfate Ratio ROUTINE 0.45 ions, XRF QCR
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 11 of 13

Table 22-5. Mapping of Outlier Flags onto AIRS Codes

Objective Cause Found for Level 1 Outlier

AIRS codes

If NOT Invalid

(Suspicious)

If Invalid

• Lab Error

• Filter Damage

• Module Assignment Error

• Sampler Malfunction

• Unusual Conditions noted by operator

• Unknown Cause

• [1]

• [1]

• [1]

• (N/A)

• [2]

• T

• AR

• AJ

• AQ or AR

• AN

• [3]

• AS

Notes:

[1] - No appropriate AIRS validity status code exists in current AIRS.

[2] - Use the applicable AIRS validity status code, or T.

[3] - Use the applicable AIRS null value code, or AM.

(N/A) - Not Applicable

Table 22-6. Automated Range Checks

Parameter Limits AIRS Flag or Action

Exposure Duration, t exp 23<texp<25 hrs AN - machine malfunction

AQ - collection error

AV - power failure

 or other code as appropriate

Holding Time before removal from sampler,

tpick-up

tpick-up < 96 hrs AM - miscellaneous void

(pick-up holding time is not defined in

current AIRS)

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

22.8 Treatment of Deviations from Requirements

Deviations from requirements call for a variety of response activities that are summarized below:

Flag Data in AIRS—Chemical speciation data should be marked with a data validity flag only if the

data are considered valid for most purposes and uses. 
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 12 of 13

Invalidate Data in AIRS—Data of uncertain provenance and data with unacceptable levels of

uncertainty should not be included in AIRS. These data will be reported as missing. 

CAR Process—The CAR process 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 STN 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. 

This process should involve consideration of the primary DQO of trend detection described in Section

7.0. 

Notification of EPA or Other Stakeholders—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 STN laboratory (through channels approved by the DOPO) to

provide documentation of corrective actions that might affect the data validation status of reportable

data. The State reporting organizations should include significant QA problems in their annual QA

reports to management.

22.9 Verification and Validation Criteria: Field Component

Table 22-3 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. 
PM2.5 STN QAPP

Section No. 22

Revison No.: 4

Date: 6/00

Page 13 of 13

TABLE 22-7. DATA VERIFICATION AND VALIDATION SUMMARY

Item Criteria

Applicable

to Comment

Flag in

AIRS 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 !

CAFDF records for filters and

denuders

Must be

present

CAFDF

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 filter Review and determine impact on

data validity

! "

Electronic data transmission No errors

reported

Electronicall

y 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

recertificatio

n records

Dates of recertifications should

be verified before data are

reported

"

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 AIRS

! "

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

" "

Notes:

"Flagging or invalidation is optional. Reporting 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 AIRS without a flag if the data need not be

qualified to the data user, (2) flag the data and report to AIRS 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 AIRS).

!Flagging or invalidation is mandatory. When this symbol is shown in the "Flagging" column and the "Invalidation" column is blank,
PM2.5 STN QAPP

Section No. 23

Revison No.: 4

Date: 6/00

Page 1 of 4

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 DQOs 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 STN laboratory, which conduct the chemical

analyses and reports the validated concentration values to AIRS. This section focuses on the

verification and validation methods applied by the reporting organizations after the first stages of

validation have been completed by the STN laboratory.

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 STN laboratory issues unexposed sample module kits to the reporting agencies along

with a partially completed custody and field data form CAFDF.

2. The reporting agency exposes the filters, fills in the necessary data about the exposure on

the CAFDF form, and returns them to the STN laboratory.

3. The STN laboratory enters the data recorded on the CAFDF, performs the data analyses,

and enters the results into the data system. 

4. The STN 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 STN laboratory transmits the data and

associated validation flags in hardcopy and electronic form to the DOPO, who in turn

distributes the data to the respective ROs. 

6. The RO completes the verification and validation process at levels 2 and 3 based on

information compiled from previous PM2.5 research programs, guidance from CASAC and

Expert Panel on PM2.5 Speciation, its own internal records, audit results, and other

information available from site operators and other local sources. 

7. The ROs forwards the validated data back to the STN laboratory for submission to AIRS. 

8. Further statistical validation may be performed by EPA and others as needed.
PM2.5 STN QAPP

Section No. 23

Revison No.: 4

Date: 6/00

Page 2 of 4

23.2 Personnel Responsibilities within the Reporting Organization

The RO should assign data validation responsibilities according to its organizational structure and the

needs of this program. 

Within the RO, the following roles and responsibilities for STN data validation may be defined.

Program Manager—The RO's manager for the PM2.5 chemical STN is ultimately responsible for

meeting schedules, for ensuring that qualified staff perform data management and validation functions,

and for delivering valid data to AIRS. The RO's STN 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 STN program. 

Data Validation Specialist—The Data Validation Specialist is the person who conducts the actual

examination of data received from the STN 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 QA supervisor responsible for the STN 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 STN 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.

The following sections describe the verification and validation procedures that should be applied by

ROs to the partially validated data received from the STN laboratory.

23.3 Completion of Level 0 Data Verification and Validation

The first step in the RO's data verification and validation process should be to confirm that the data are

correctly accounted for according to the RO's own records. The STN laboratory will have checked

the data according to its shipping and receiving records and the CAFDFs and will have flagged any

discrepancies in data attribution. The Data Validation Specialist should examine each discrepancy that

the STN laboratory has flagged as suspicious due to uncertain attribution or problems with chain of

custody. The RO should examine its copy of the CAFDF, shipping and receiving records, operator

logbooks, and any other relevant records to address the problem. (The STN laboratory may have

already contacted the RO, via the DOPO, regarding problems of data attribution, so a repeated check

of a previously investigated problem may not be necessary.) The RO 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. 
PM2.5 STN QAPP

Section No. 23

Revison No.: 4

Date: 6/00

Page 3 of 4

< If the STN laboratory has flagged data as misassigned (i.e., assigned to the wrong sampling

date, site, analyzer, or channel), the RO may edit the data so that monitoring data are

correctly assigned. This may only be done if verifiable information can be found in the RO's

operating records that allows 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 RO can make

this correction directly, but it is recommended that this information be passed back to the

STN laboratory, via the DOPO, so that the calculation can be verified.

< If the RO 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 RO 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:

< 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 audit bias found in 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. 

< Collocated Sample Results—Performance on collocated duplicates should be evaluated if

information is available. 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.

< 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 RO 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.
PM2.5 STN QAPP

Section No. 23

Revison No.: 4

Date: 6/00

Page 4 of 4

< 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 d 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 STN laboratory. 

< Corrective Action Requests that Affect Data Quality—The Data Validation Specialist

should review any CARs in effect when the samples were acquired. Any CARs that could

affect the data should be evaluated and appropriate actions taken with regard to flagging or

invalidating the data. 

23.4.2 Automated Methods

Because the data will be delivered from the STN laboratory to the ROs in electronic format, automated

checking could be implemented. Some automated screening methods that might be considered include

the following:

< Interparameter Checks—These include ion ratio and mass balance checks that use data

from a number of different channels. 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 chemical speciation

concentration measurements (the actual environmental measurements, rather than QA

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 1 or 2 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. 

Specific information about the automated screening methods will be coordinated by EPA and

distributed to STN field and laboratory personnel.
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 1 of 7

24.0 Reconciliation with Data Quality Objectives

Results obtained must be reconciled with the requirements defined by the data user or decision-maker,

as specified by the DQOs for the project (U.S. EPA, 1994). The methods used to analyze the data are

based on the statistical model described fully in Data Quality Objectives for the Trends Component

of the PM2.5 Speciation Network (U.S. EPA, 1999a) and outlined in Section 7.0 of this QAPP. It is

expected that actual data acquired under the Speciation Trends Network will depart in various ways

from the original conditions and assumptions of the DQO study. This section discusses these issues

along with how they will be resolved and how limitations on the use of the data will be reported to

decision-makers.

24.1 DQO for Chemical Speciation Trends

The primary DQO for the chemical speciation network is defined as the ability to detect a +5 percent

annual trend within 5 yr with statistical power of 0.80. A research study (U.S. EPA, 1999a)

summarized in Section 7.0 of this QAPP indicated that this would be a feasible DQO for the chemical

STN, based on a review of similar species concentration data obtained from samples collected in the

past at an urban site in the IMPROVE network. 

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 yr 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

yr) 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 well-controlled, it may be possible to diagnose a trend smaller

than +5 percent or to identify a trend in less than 5 yr.

To satisfy the primary DQO, it is only necessary to demonstrate that the 5-yr 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. It is hoped that the DQO for diagnosing

trends will be met for PM2.5 mass as well as for the chemical species used in the DQO feasibility study

(U.S. EPA, 1999a). 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 energy-dispersive

X-ray fluorescence [EDXRF])

< Large background variability near the analytical method’s detection limit

< Large proportion of nondetects, thus weakening the statistical power of the analysis

< High variability in concentration of the species in the environment
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 2 of 7

< Seasonal variability

< The presence of local sources (ocean, nearby construction, industrial or residential

sources).

24.2 Interim Evaluations of Data Quality

The STN 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 yr. 

There 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 yr. 

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 (DQA) is appropriate after 1 yr of sampling;

however, more exhaustive analysis should be done after 2 or 3 yr of data have been collected, as

described in the next section. 

The STN 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). Likewise, a 5 percent coefficient of variation (CV) in flow rate (random error)

will result in a 5 percent CV in the concentration (approximately). Flow rate is a significant contributor

to overall error, but it is an incomplete estimate of total measurement error because it does not include

several 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 bias and reproducibility. 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.
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 3 of 7

Field Blank Results—Field blanks provide information on contamination due to handling operations. 

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. 

Collocated Sampling Results—These results are potentially the most complete of the measurements of

end-to-end error. When starting up a new chemical speciation sampler at a site, it is a good idea to

collect a number of duplicates with the collocated sampler. Approximately 10 valid duplicate samples

should be considered the minimum for estimating the total error. 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 STN

laboratory will provide EPA with regular QA summary reports that will include the necessary

information for assessing this and other components of analytical 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 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 that a siting problem 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.

The recommended interim method for estimating total measurement error is to calculate the total error

based on 10 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:
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 4 of 7

(24-1)

(24-2)

(24-3)

1. Calculate the duplicate difference for each observation, as follows:

where

di = percent difference for observation i

Yi = primary (station) sampler concentration value

Xi = 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 (MDL). 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:

where

CVi = CV for observation i

di = 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 within a given

time period for a particular chemical species (or total mass) designated by the subscript j:

where

CVj = pooled CV for species j over the specified time period

CVi,j = CV for species j, observation i

nj = number of paired observations made for species j over the time period.

4. Compare the CVjresults 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. 
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 5 of 7

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 yr, 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 STN 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:

< Increase the Frequency of Sampling—The DQO study (U.S. EPA, 1999a) showed that

1-in-3 d sampling was adequate to meet the DQO based on the IMPROVE data set, while

daily sampling was unnecessary and 1-in-6 d 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. 
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 6 of 7

< Improve QC and Maintenance—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. 

24.3 Assessing and Reporting Chemical Speciation Trends

At the end of the first 5 yr of monitoring, each reporting agency will assess whether or not the DQO 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, NC.

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?

< 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 Chemical STN Research Objectives

There are several important research objectives for the STN data other than trend identification (U.S.

EPA, 1999b). These include model development and validation, source attribution, State

implementation plan (SIP) 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 
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 7 of 7

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. 
PM2.5 STN QAPP

Section No. 24

Revison No.: 4.1

Date: 12/00

Page 8 of 7

24.5 References

U.S. EPA (Environmental Protection Agency). 1994. Guidance for the Data Quality Objectives

Process: EPA QA/G-4, Report No. EPA/600/R-96/055, U.S. EPA, Washington, DC.

U.S. EPA (Environmental Protection Agency). 1998. Guidance for Data Quality Assessment -

Practical Methods for Data Analysis, EPA/600/R-96/084, U.S. Environmental Protection Agency,

Office of Research and Development, Washington, DC. January 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 the Ambient Monitoring Technical Information Center [AMTIC] at

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

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

Guidance Document (Third Draft), U.S. EPA, Research Triangle Park, NC. January 5, 1999.
APPENDIX A-1

SOP 5000STN

CONDENSED OPERATING PROCEDURE

FOR FIELD INSTALLATION 

OF PM2.5 SPECIATION SAMPLERS
SOP # 5000STN PM2.5 Sampler Installation

Rev. # 1

Date: September 30, 1999

Page 1 of 5

CONDENSED STANDARD OPERATING 

PROCEDURE (SOP) FOR FIELD INSTALLATION

OF PM2.5 SPECIATION SAMPLERS

Prepared by: Date: 

Prepared by: Date: 

Prepared by: Date: 

Reviewed by: Date: 

Approved by: Date: 

PM2.5 Speciation Trends Network

Office of Air Quality Planning and Standards

U.S. Environmental Protection Agency

Research Triangle Park, NC 27709
SOP # 5000STN PM2.5 Sampler Installation

Rev. # 1

Date: September 30, 1999

Page 2 of 5

1.0 Purpose and Applicability

This document outlines the procedure for field installation and setup of several

commercially available PM2.5 speciation samplers. For more detailed information

regarding field installation of these samplers, refer to the specific sampler’s operator’s

manual.

2.0 Safety Precautions

2.1 To avoid electrical hazards, all sampler installation procedures should be conducted with

the sampler disconnected from the AC power source.

2.2 Observe proper lifting procedures when unpacking and moving sampler components.

2.3 Read, understand, and follow all safety precautions for each sampler outlined in the

sampler’s operator’s manual.

2.4 Once sampler installation is complete, secure the sampler to the field sampling platform to

ensure that it does not tip over during high wind speed events.

2.5 Care must be taken when operating or calibrating the units in inclement weather. Safety is

paramount.

3 .0 Siting

3.1 Ensure the sampler is level.

3.2 Ensure the sampler inlet is separated by at least 1 m, but no more than 4 m, from other

PM2.5 samplers and that the sampler has an unobstructed air flow of a minimum of 2 m in

all directions. For collocated sampler studies, position the sampler’s inlets exactly 1 meter

apart.

4.0 Sampler Setup Procedures

4.1 Andersen (RAAS) - Sampler Installation

4.1.1 Basic Assembly Steps

1. Locate the pump/base stand and attach the four stabilizing “L” shaped bracket feet.

2. Locate the base stand so one of the widest sides will represent the front or back. 

Carefully lift the main housing squarely onto the base stand.

3. Open the housing door. Locate the four holes inside on the bottom panel to align, insert

and tighten the four 1⁄4-20 screws and washers provided.

4. Remove one front or backside panel to the pump base by loosening the four captive

screws.

5. Pump base vacuum and power lines can be extended up through the round hole in the

housing base.

6. Attach tubing to the available compression thread fitting nearest the large ball valve

connected to the flow manifold assembly on the floor of the housing base.
SOP # 5000STN PM2.5 Sampler Installation

Rev. # 1

Date: September 30, 1999

Page 3 of 5

7. Insert the pump power cord into the outlet labeled “pump.”

8. Locate the sample flow splitter assembly. Install the downtube and sample inlet

components. Refer to the operator’s manual for this multi-step process.

9. Next, install the two large sample manifolds. Note: The left and right devices are mirror

images and are interchangeable. Install the left side manifold first. The manifolds slide into

grooves provided on the inside roof of the sampler case.

10. Locate and install the two cyclone assemblies.

11. Select one of the two possible locations for the ambient temperature radiation shield. 

Secure the unit upright so the support arm extends upward at 45 degrees and the shield’s

protective fins angle downward.

12. Run the ambient thermocouple through the middle hole and plug it into the ambient

temperature receptacle on the inside back panel.

13. Set up the flow manifold and its flow sensors and critical orifices. Ensure the vacuum

pump pressure sensor tubing (small) is connected on the right side of the flow manifold and

to the labeled panel position “pressure pump.” Refer to the operator’s manual.

14. Install the sampling train assemblies. Refer to the operator’s manual for details.

15. General system setup is complete.

4.2 Met One (SASS) – Sampler Installation

4.2.1 Tripod and Mast Installation

1. Spread the three legs of the tripod by applying tension to the support brackets. Make the

tripod steady.

2. Note the “UP” mark on the mast. Slide the mast into the top of the tripod collar allowing

the lower-most stop to pass the collared key-way. The paired stops in the mast limit the

mast from striking the ground.

3. Position the lower support brackets and tighten all hardware using a crescent wrench.

4. Securely anchor the tripod feet to the sampling platform using wood screws.

4.2.2 Sampling Head and Solar Shield Installation

Note: This installation may require two workers.

1. Remove the pin from the lower shield and slide down the mast. Allow the solar radiation

shield to rest on the paired stops.

2. Install two 8-32 x 3/16" cap-screw stops into tapped holes at the top of the mast and

tighten them.

3. While supporting the upper sample head/shield assembly, feed the tube and cable harness

into the top of the mast. Lift the sample head/shield and place the hub onto the top of the

mast.

4. Rotate the sample head and the shield until the hub engages the notch and the cap screw

stops.

5. Tighten the two allen key screws in the hub and the two thumbnuts.
SOP # 5000STN PM2.5 Sampler Installation

Rev. # 1

Date: September 30, 1999

Page 4 of 5

6 Raise the lower radiation shield and engage the slot for positioning. Insert the pin into the

shield and mast.

7 Lift the entire mast assembly, allowing the lowermost stops to pass through the top collar

key-way. Rotate the mast, allowing stops to align and drop into the top collar groove.

8 Secure the mast to the tripod by tightening the bolts in the upper and lower collars.

4.2.3 Control Box Installation

1. Install the control box onto the mast using the two U-bolts. Position the bottom of the

control box on the top of the upper collar on the mast.

2. Connect the sampling head fan and filter temperature cable to the third connector from the

right on the bottom of the control box. 

3. Connect the ground cable on the control box stud to an electrical earth-ground connector.

4.2.4 Ambient Temperature Sensor Installation

1. Install the ambient temperature sensor onto the mast using two U-bolts. 

2. Position the sensor onto the mast immediately above the top of the control box. Sensor

position should be at a 180 degree angle from the control box door.

3. Connect the ambient temperature sensor cable to the second connector from the right on

the bottom of the control box.

4.2.5 Pump Box Installation

1. Place the pump box on the sampling platform between the legs of the tripod.

2. Connect the five numbered sample flow lines, exiting the bottom of the mast, to the

numbered quick disconnects located on the side of the pump box.

3. Connect the 14-pin communication cable, exiting the bottom of mast, to the first connector

from the right on the bottom of the control box. Note: The quick disconnects have

internal shut-off valves if a sample channel is not used.

4. Connect the AC power cable to the 115 VAC/60 Hz source to provide power to the

SASS.

4.3 URG (MASS 400 and MASS 450)--Sampler Installation

1. Position the MASS sampler’s case so that it is resting on the top cover.

2. Align the stand on the bottom of the unit and attach it using the provided 1⁄4-20 nuts and

washers.

3. Turn the sampler’s case to the upright position.

4. Remove the top and the back panel of the sampler.

5. Run the ambient temperature thermocouple through the middle hole on the top cover.

6. Reinstall the top cover and the back panel.

7. Install the ambient temperature radiation shield and insert the ambient air thermocouple

sensor assembly.
SOP # 5000STN PM2.5 Sampler Installation

Rev. # 1

Date: September 30, 1999

Page 5 of 5

8. Install the sampler inlet tube (downtube/denuder) and WINS impactor. As this is done,

verify that all O-rings are in place, fit snugly, and none are frayed, split or broken.

9. The MASS 400 and MASS 450 sampler units must be placed on the platform according

to the inlet height (within 1 m) and inlet horizontal separation (greater than 1, but less than

4 m) specifications that apply to collocated samplers.
APPENDIX A-2

SOP 5100STN

CONDENSED STANDARD OPERATING

PROCEDURE FOR THE MET ONE SASS
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 1 of 10

CONDENSED STANDARD OPERATING 

PROCEDURE (SOP) FOR THE MET ONE SASS

Prepared by: Date: 

Prepared by: Date: 

Reviewed by: Date: 

Approved by: Date: 

PM2.5 Speciation Trends Network

Office of Air Quality Planning and Standards

U.S. Environmental Protection Agency

Research Triangle Park, NC 27709
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 2 of 10

1.0 Purpose and Applicability

This condensed standard operating procedure (SOP) outlines procedures for field

operations and quality control checks of the Met One SASS PM2.5 speciation sampler. For

more detailed information regarding operation of this sampler, refer to the Met One SASS

operator’s manual.

2.0 Precautions

2.1 Read and thoroughly understand the operator’s manual before beginning field operations. 

The flow rate and temperature calibrations of the sampler must be checked and, if

necessary, adjusted to specifications prior to taking the first sample. Consult the operator’s

manual for calibration instructions.

2.2 Use only the sampling cassettes, sent to you from the laboratory, for the designated

sampler and location.

2.3 Exercise great care in placement and handling of sampling cassettes to avoid

contamination.

2.4 The sharp cut cyclone must be attached to the inlet of the sampling cassette before

sampling.

3.0 Equipment and Supplies

3.1 Have the STN Custody and Field Data Form for the particular sampler, for the particular

sampling day, with you when visiting the site. Have an STN QA/QC Report Form if a

quality control check is due.

3.2 Sampler operator’s manual and field notebook.

3.3 Met One SASS speciation sampler, accessories, and any tools needed.

3.4 SASS cassettes, pre-loaded with filters and denuders for up to five channels. Field blank

cassette(s) for use on every 10th sampling day. All these items will be supplied from the

support laboratory.

3.5 Sharp cut cyclone for each sampling cassette. Label the cyclone to correspond to a single

sample channel position and dedicate the cyclone to use with this channel.

3.6 Shipping coolers, frozen ice substitutes, and Federal Express labels for shipment of

sampling modules and reports to analytical support laboratory. These will be supplied by

the support laboratory.

3.7 Independent methods for quality control checks of sampler operation.

3.7.1 Date and time. Calendar check. Accurately set watch.

3.7.2 Leaks. Device to close sample flow pathway (plug for inlet to sharp-cut

cyclone).

3.7.3 Temperature. Thermocouple or thermistor-based digital thermometer transfer

standard, with current NIST traceability.

3.7.4 Pressure. Aneroid barometer or equivalent transfer standard with current

NIST traceability.

3.7.5 Flow rate. Low pressure flow transfer standard with leak-tight connection
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 3 of 10

tubing. Examples: frictionless piston or soap film flowmeter; orifice-type

flowmeter, either with current NIST traceability.

4.0 Sampler Operating Procedures

Record information about the sample, the field blank, or the trip blank on an individual PM2.5

STN Custody and Field Data Form (CAFDF) (see Figure 4-1).

4.1 Sample Preparation and Programming the Met One Sampler

1. Remove the protective end caps from the cassette. Attached a dedicated sharp cut cyclone to

each cassette. Install loaded filter cassettes in predetermined (color-coded) sampling channel

locations according to the information given on the CAFDF sent from the support laboratory. 

Load field blank cassette(s) every 10 sampling days. Do not activate flow to field blank

channel(s). Place cassette caps in a clean plastic bag and store for later use to seal used

cassettes for return to the laboratory. 

2. Press F2 key to set up Start/Stop times in the sampler.

3. If possible, key in information (including the unique custody/data form number assigned by the

laboratory) to the sampler memory to allow later matching of the stored data with the analytical

results.

4. Edit START Date/Time, and END Date/Time using the arrow keys. The STN network will

collect 24-hour samples, beginning at midnight.

5. Select “SAVE” to save the programmed event.

6. Press F1 to review the programmed event, and then select “EXIT”.

7. Make entries to the CAFDF.

4.2 Data Retrieval

1. At the end of the sample run, select “SUMMARY” option from the main screen.

2. Record end date/time, sample retrieval date/time, specified post-sampling information, and

free-form comments on the CAFDF. Please double-check entries and write clearly! 

3. Download sampler data from RS232 port to laptop computer or to Met One SASS data

transfer module.

4.

4. Retain data file disk file for later use in data validation. Do not ship it to the support

laboratory. .
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 4 of 10

5. Select “EXIT” to complete the data retrieval.

4.3 Filter Cassette Handling

The field operator will encounter filter cassettes for several uses. These are for routine (every

third day) sampling, field blanks (sent from the laboratory for use on every tenth sampling day),

and trip blanks (sent every thirty sampling days).

It is highly recommended that sampling modules (i.e. cassettes, filter packs) be removed

from the sampler within 48 hours after the sampling period ends. For a one-in-three day

schedule this will be necessary since the next sampling day’s cassettes must be installed. 

Once the sampled cassettes are removed, separate the sharp cut cyclone for reinstallation with

the next set of cassettes, cap or cover the cassette openings, store the cassettes in the shipping

container or cooler, complete the CAFDF, and return all to the field office. The sampled cassettes

and paperwork must be properly packaged in a cooler, ready for pickup by Federal Express,

within 96 hours after the sampling period ends. The support laboratory will provide specific

directions for packaging and shipment and days for shipment. Protect samples from direct sunlight

and extreme heat during transport from the site to the field office; store them in a secure, airconditioned area until just before packaging them in the cooler. 

Days of the week for shipment will be arranged in coordination with the DOPO and

laboratory. Do not ship on Fridays unless prior arrangements are made with the DOPO and

laboratory. 

Routine Samples

1. At the end of the sample run, lower the sampler’s lower radiation shield.

2. Rotate each canister counterclockwise to remove from its sampling position. Remove the

cyclone. Cap the cassette inlet and outlet with yellow end caps. Place or store the

cyclones in a clean spot. Reinstall cyclones on the cassettes for the next sampling run.

Every 30 days of use, clean the cyclone per instructions given in the operator’s manual.

3. Place each filter cassette into a zip-lock style bag and then place it in the proper location

in the storage bin or cooler. 

4. Complete all paperwork. 

5. Clean the area around the sample head; wipe connections with a clean cloth or paper

towel. Install a new filter cassette by aligning screws in slots and rotate it

counterclockwise to secure. Take care to properly match the SASS cassette to the

correct sampler inlet.
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 5 of 10

Field Blank Filters

1. Field blank filters, loaded into cassettes, will be shipped from the laboratory. They will

have a separate STN Custody and Field Data Form (CAFDF) with them. They are to be

used during the same time interval as the routine sample cassettes.

2. Visit site at the time regularly scheduled for setting up a new sampler run. Install the field

blank cassettes (and sharp-cut cyclones) in the channel locations as indicated by the

CAFDF. 

3. After a minute or two, remove the field blank cassettes from the sampler, detach the

cyclones, cap the cassettes, and return them to their spot in the shipping bin or cooler. 

4. Proceed to install the routine sample cassettes according to schedule.

5. Complete and sign the CAFDF for the field blank cassettes and ship them back to the

laboratory, in their own cooler, at the same time as the routine samples.

Trip Blank Filters

1. Trip blank filters, loaded into cassettes, will be shipped from the laboratory. They will

have a separate CAFDF with them. They are to be used during the same time interval as

the routine sample cassettes.

2. These cassettes should be carried to the site but left in the cooler or carrying container.

They should not be installed in the sampler. 

3. Complete and sign the CAFDF for the trip blank cassettes and ship them back, in their

own cooler, to the laboratory at the same time as the routine samples are shipped. 

4.4 Denuder Handling

The support laboratory will change the denuder when it is due for replacement. The denuder is

an integral part of the sampling cassette.

5.0 Sampler QA/QC Procedures

Certain quality control checks must be conducted at the time of sampler startup and at monthly or

quarterly intervals thereafter. Carry out these checks before making any adjustments to the

sampler. Record information about the site, the sampler, and the results of scheduled or special

(unscheduled) quality control checks on the PM2.5 STN QA/QC Report Form, Figure 5-1. This

report form originates at the field site. The site operator should keep the original on file and send 

a copy to the State or local agency QA Manager. Do not send the QA/QC Report Form to the

support laboratory. Any actions taken to service or calibrate the speciation sampler after the

check must be recorded in brief on the form and in detail in the field operator’s notebook.
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 6 of 10

5.1 Date and Time Checks

Conduct these checks monthly or whenever daylight savings time changes occur. Compare the

date and time displayed on the sampler to the known date and to an accurately set watch. 

Record information on the QA/QC data form. Refer to Figure 5-1.

5.2 Monthly Leak Check

Performed upon startup, then monthly.

1. Place cassette containing filter/denuder and attached sharp cut point cyclone at the channel

location to be leak-checked. Use this cassette assembly for leak checks and flow rate

checks only. The cassette must contain the type of filter (and denuder, if included in the

cassette) normally used at this sampling channel location.

2. Press F3 key, and select “PUMP ON”.

3. Plug the Sample Inlet (e.g., Channel 1) with cap. Note the displayed flow. The indicated

flow rate should drop to 0.0 L/min. If it does not, check for leaks and repeat the

procedure until the leak check is completed successfully. Repeat for all channels in use.

4. Select “PUMP OFF” to stop the pump, and “EXIT”.

5. Release the vacuum slowly to avoid damaging the leak check filter.

5.3 Monthly Temperature Control Check

Performed upon startup and then monthly. Check the ambient and filter temperature sensors of

the sample by positioning the probe of a certified transfer standard digital thermometer in close

proximity to the sampler sensors. Allow time to achieve stable readings and record the results in the

field notebook and on the STN QA/QC report form. If the sampler and control check temperature

readings differ by more than + 2°C, trouble-shoot the system and recheck. If still out of tolerance,

conduct a multipoint calibration or replace the faulty sensor. Consult the manufacturer and the

operator’s manual for procedures.

5.4 Quarterly Temperature Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.3, but use a

temperature transfer standard that is independent of the one used for the monthly checks. Should

a temperature sensor not maintain its calibration after the monthly or quarterly checks,

maintenance and/or replacement of the faulty parts must occur.

5.5 Monthly Pressure Control Check

1. Compare the ambient barometric pressure readout from the sampler display screen with

the reading from a certified transfer standard barometer.

2. If the pressure readings differ by more than + 10 mm Hg, perform a multipoint calibration

of the sensor or replace the faulty sensor.
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 7 of 10

5.6 Quarterly Pressure Control Check

Follow the same steps as in Section 5.5, but use a pressure standard that is independent of the

one used for the monthly checks. Should the pressure sensor system not maintain its calibration after

the monthly or quarterly checks, maintenance and/or replacement of the pressure sensor system must

occur.

5.7 Monthly Flow Rate Control Check

Perform flow rate check upon startup, then monthly.

1. Use same cassette assembly called for in monthly Leak Check Procedure (Section 5.2).

2. Connect an external flow audit device to the cyclone sample inlet (e.g., Channel 1). Use a

low pressure drop certified flow transfer standard.

3. Press the F3 key, and select “PUMP ON”. 

4. Compare the flow rate measured by the external flow device with displayed value. (The

sampler is preset at 6.7 L/min). If the flow deviation exceeds + 4% (+ 0.27 L/min)

contact Met One for technical support since the critical orifice flow rates are set at the

factory.

5. Repeat the procedure for all flow channels in use.

5.8 Quarterly Flow Rate Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.7, but use a flow rate

transfer standard that is independent of the one used for the monthly checks. Should the flowrate

mechanism not maintain its calibration after the monthly or quarterly checks, maintenance and/or

replacement of the flow controller system(s) must occur. Consult the manufacturer or the

operator’s manual for procedures for maintenance, adjustment, and calibration of sample flow

rates.

6.0 Sampler Maintenance and Troubleshooting

1. Clean the solar radiation shield with wet cloth as required.

2. If flow rate falls off, or is variable, the unit may need factory servicing of the pump or of the

particle filter/critical orifice flow controllers.

3. Check O-rings for wear or damage. Make a comment on the CAFDF to the laboratory

of problems with cassette assemblies.

4. Record all maintenance and troubleshooting activities in the site notebook. On the

CAFDF, record activities that may affect the sample weight or analysis. 
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 8 of 10

BAR CODE GOES HERE PM2.5 STN CUSTODY AND

FIELD DATA FORM

White – return to lab

Yellow – site retains

Pink – lab retains Custody/Data Form No.

A. CUSTODY RECORD (Name, Date)

1. Laboratory, Out 3. Site, Out 

2. Site, In 4. Lab, In 

B. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name 

2. Sampler S/N 6. Intended date of use 

3. Sampler Type 7. Date of sampler set-up 

4. Sampler POC 8. Operator’s name 

C. SAMPLER CHANNEL COMPONENTS

Channel

Number

Component ID

No.

Component Description

1 kept at site SASS cyclone

1 I1234568 SASS cassette (Teflon filter) (GREEN)

2 kept at site SASS cyclone

2 I1234570 SASS cassette (MgO denuder, nylon filter) (RED)

3 kept at site SASS cyclone

3 I1234572 SASS cassette (quartz filter) (ORANGE)

D. START, END, AND RETRIEVAL TIMES

Channel No. Start date Start time End date End time Retrieval

date

Retrieval

time

1

2

3

E. SAMPLER CHANNEL INFORMATION (Post-Sampling)

Channel

No.

Run

Time

Run

Time, Flag

Sample

Volume

(m3)

Avg.

flow

(L/min)

Avg.

flow CV

(L/min)

Avg.

ambient

T (°C)

Max.

 ambient

T (°C)

Min.

ambient

T (°C)

1

2

3

Channel

No.

aT

Flag

Avg. Filter

T (°C)

Max. Filter

T (°C)

Min. Filter

T (°C)

Avg. BP

(mm Hg)

Max. BP

(mm Hg)

Min. BP

(mm Hg)

1

2

3

F. Comments 

(Revised 9/27/99: 5100)

Figure 4-1. STN Custody and Field Data Form With Entries for the Met One SASS Sampler.
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 9 of 10

QA/QC Form No. PM2.5 STN QA/QC REPORT FORM c. 1 (site retains)

c. 2 (Agency QAM)

A. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name

2. Sampler S/N 6. Interval: Month _______ Quarter ______ Special

______

3. Sampler Type 7. Date(s) of QA/QC Checks 

4. Sampler POC 8. Operator’s Name 

B. DATE AND TIME CHECKS (Transfer Standard Name ____________ Transfer Standard ID Number ____________)

Sample display date/time Transfer standard date/time Date and time agree ± 5 min? Action taken (a)

C. LEAK CHECKS (Transfer Standard Name ___________________ Transfer Standard ID Number ______________)

Channel number Manufacturer’s specifications met? Action taken and recheck results (a)

1

2

3

4

5

D. TEMPERATURE CHECKS (Transfer Standard Name _____________ Transfer Standard ID Number __________)

Sensor location Sampler display (°C) Transfer standard (°C) Agreement ± 2 °C ? Action taken and

recheck results (a)

Ambient

Filter

E. PRESSURE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ____________)

Sensor location Sampler display,

(mm Hg) 

Transfer standard,

(mm Hg)

Agreement within

± 10 mm Hg?

Action taken and

recheck results (a)

Ambient

F. FLOW RATE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ___________)

Channel number Sampler display,

(L/min)

Transfer standard

display, (L/min)

Design flow rate,

(L/min)

Agreement within

± 10 percent? (b) 

Action taken and

recheck results (a)

1

2

3

4

5

G. COMMENTS 

(Revised 09/23/99)

(a)Fully describe actions taken in field notebook. 

(b) Sampler flow rate must agree with both transfer standard and design flow rate to pass.

Figure 5-1. STN QA/QC Report Form.
SOP # 5100STN Met One SASS

Rev. # 1

Date: September 30, 1999

Page 10 of 10

7.0 References

1. Operation Manual (Draft). Spiral Aerosol Speciation Sampler SASS. Met One

Instruments. June 8, 1998.

2. Met One SASS (Chemical Speciation) Sampler “Quick Operation.” Met One

Instruments. Not dated.
APPENDIX A-3

SOP 5200STN

CONDENSED STANDARD OPERATING

PROCEDURE FOR THE ANDERSEN RAAS
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 1 of 12

CONDENSED STANDARD OPERATING

PROCEDURE (SOP)

FOR THE ANDERSEN RAAS

Prepared by: Date: 

Prepared by: Date: 

Reviewed by: Date: 

Approved by: Date: 

PM2.5 Speciation Trends Network

Office of Air Quality Planning and Standards

U.S. Environmental Protection Agency

Research Triangle Park, NC 27709
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 2 of 12

1.0 Purpose and Applicability

This condensed standard operating procedure (SOP) outlines procedures for field

operations of the Andersen RAAS PM2.5 speciation sampler. For more detailed information

regarding operation of this sampler, refer to the latest edition of the Andersen RAAS

operator’s manual.

2.0 Precautions

2.1 Read and thoroughly understand the operator’s manual before beginning field operations. 

The flow rate, temperature, and barometric pressure calibrations of the sampler must be

checked and, if necessary, adjusted to specifications prior to taking the first sample.

Consult the operator’s manual for calibration instructions.

2.2 Use only the sampling modules, sent to you from the laboratory, for the designated

sampler and location.

2.3 Exercise great care in placement and handling of sampling modules to avoid contamination.

3.0 Equipment and Supplies

3.1 Have the STN Custody and Field Data Form for the particular sampler, for the particular

sampling day, with you when visiting the site. Have an STN QA/QC Report Form if a

quality control check is due.

3.2 Sampler operator’s manual and field notebook.

3.3 Andersen RAAS speciation sampler and accessories.

3.4 A set of three laboratory-supplied, pre-loaded sampling modules (filter holders) containing

Teflon, nylon, and quartz filters, respectively. A separate sampling module containing a

cassette with glass fiber or other filter for use in the fourth flow channel to maintain proper

flow distribution (the latter module is kept at the site). Field blank modules for use on

every 10th sampling day. Denuder tube to remove acidic vapors. Shipping containers

(coolers), frozen ice substitutes, and Federal Express labels for shipment of sampling

modules, denuders, and reports to the analytical laboratory. All these items will be

supplied from the support laboratory.

3.5 Independent methods for verifying proper sampler operation.

3.5.1 Date and Time. Calendar check. Accurately set watch.

3.5.2 Leaks. Device to close sample flow pathway (flow rate adapter).

3.5.3 Temperature. Thermocouple or thermistor-based digital thermometer, with

current NIST traceability. Tegam® temperature calibrator assembly.

3.5.4 Pressure. Aneroid barometer or equivalent transfer standard with current

NIST traceability.
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 3 of 12

3.5.5 Flow rate. Low-pressure flow device with leak-tight connection tubing. 

Examples: frictionless piston or soap film flowmeter; orifice-type flowmeter; or

RAAS flow calibration kit with reference dry gas meter. Each should have

current NIST traceability.

3.5.6 As an option, a multi-purpose device for checking temperature, pressure, and

flow rate simultaneously.

4.0 Sample Operating Procedures

Record information about the sample, the field blank, or the trip blank on an individual PM2.5

STN Custody and Field Data Form (CAFDF) (see Figure 4-1). 

4.1 Sample Preparation and Programming the Andersen RAAS Sampler

1. Remove the plastic tranport bin containing the three capped sampling modules from the

cooler. Each sampling module is bar-coded with a number and is color-coded. Care

must be taken to place the correct sampling module in the corresponding RAAS sampling

channel. Place the plastic caps in plastic bags in the bin to maintain their cleanliness and

for safekeeping. These will be used to seal the modules following sampling. Install fresh

denuder(s) if a change is due.

2. Install the loaded sampling modules in predetermined sampling channel locations

according to instructions in the RAAS Operator’s Manual and sample channel

information given on the CAFDF sent from the support laboratory. Refer to Section 4.3,

below, for sample module handling techniques.

3. Consult the RAAS operator’s manual, section 5, for guidance on entering site

information. If desired, key in the custody/data form number (this is printed on the

CAFDF) to the “User Info 1" field. Double-check the entry. Press the “Enter” key and

return to the main menu.

4. From main menu, choose the “Setup Run” option, and press the “Enter” key to select

Filter 1.

5. Press the “Enter” again.

6. Enter the start date (MMDDYY format) and press the “Enter” key.

7. Enter the sample duration in hours, press “Enter” to complete setup.

8. Make entries to the CAFDF.

4.2 Data Retrieval

3. At the end of the sample run, return to the main screen.

4. Select “View Run”, and choose the “Last Sample” option.

5. Record end date/time, sample retrieval date/time, specified post-sampling information,

and free-form comments on the CAFDF. Please double-check entries and write

clearly using a ball-point pen!

6. Return to the main screen by pressing the “Cancel” button.

7. Download data electronically to a laptop computer or to the Andersen DataLink
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 4 of 12

accessory. Refer to Section 7 of the operator’s manual for further instruction on data

logging. Retain the data file disk for later use in data validation. Do not send it to the

support laboratory. 

4.3 Sample Module Handling

The field operator will receive pre-loaded sampling modules for several uses. These are for

routine (every third day) sampling, field blanks (sent for use on every tenth sampling day), and

trip blanks (sent every thirty sampling days).

It is required that sampling modules be removed from the sampler within 48 hours after

the sampling period ends. For a one-in-three day schedule this will be necessary since the

next sampling day’s sampling modules must be installed.

Once the sampling modules are removed from the sampler, cap them, store in plastic bags in

the correct spot in the transport bin, and return all to the field office. The used sampling modules and

paperwork must be properly packaged in a cooler, ready for pickup by Federal Express,

according to the schedule provided by the support laboratory. Protect samples from direct sunlight

and extreme heat during transport from the site to the field office; store them in a secure, airconditioned area until just before packaging them in the cooler.

Days of the week for shipment will be arranged in coordination with the DOPO and the

support laboratory. Do not ship on Fridays or the day before a holiday unless prior

arrangements are made with the DOPO and laboratory. 

Routine Samples

1. Within 48 hours after the end of a sample run, remove the sampling module(s) from the

upstream SVL coupler and from the downstream tubing assembly. Cap both ends of the

module.

2. Install a new sampling module for the next run.

3. Place used sampling modules (capped and inside a plastic bag) in slots in the transport

bin. Complete all paperwork, insert it in the plastic bag provided, and place on top of the

modules in the bin. Place the plastic top on the bin and place the bin in the cooler for

shipment to the laboratory. Follow packing directions provided by the laboratory.

Field Blank Filters

1. Field blank filters, pre-loaded into sampling modules, will be shipped from the laboratory

for use every 10th sampling day. They will have a separate CAFDF with them. They

are to be used during the same time interval as the routine sampling modules.

2. Visit the site at the time regularly scheduled for setting up for a new sampler run. Install

the field blank modules in the channel locations as indicated by the CAFDF. 
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 5 of 12

3. After a minute or two, remove the field blank modules, cap them, place each inside a

plastic bag, and return them to the transport bin.

4. Proceed to install the routine sample modules according to schedule.

5. Complete and sign the CAFDF for the field blank modules and ship it and the field blank

modules back to the laboratory at the same time as the routine samples are shipped.

Trip Blank Filters

1. Trip blank filters, loaded into capped sampling modules, will be shipped from the

laboratory for use every 30th sampling day. They will have a separate CAFDF with

them. They are to be used during the same time interval as the routine sample modules.

2. Trip blank modules should be carried to the site but left in the transport bin inside the

cooler. They should not be installed in the sampler. 

3. Complete and sign the CAFDF for the trip blank filter cassettes and ship it and the trip

blank modules back to the laboratory at the same time as the routine samples are

shipped. 

4.4 Denuder Handling

If it is time to refurbish the denuder(s), remove it, cap the ends, wrap it in protective material

(polyurethane foam pipe insulation and bubble packaging), and place it in a sturdy cardboard box for

shipment back to the laboratory for refurbishment. Install a fresh denuder, supplied from the support

laboratory. 

5.0 Sampler QA/QC Procedures

Certain quality control checks must be conducted at the time of sampler startup and at monthly

or quarterly intervals thereafter. Carry out these checks before making any adjustments to the

sampler. Record information about the site, the sampler, and the results of scheduled or special

(unscheduled) quality control checks on the PM2.5 STN QA/QC Report Form, Figure 5-1.

This report form originates at the field site. The site operator should keep the original on file

and send a copy to the State or local agency QA Manager. Any actions taken to service or

calibrate the speciation sampler after the check must be recorded in brief on the form and in

detail in the field operator’s notebook.

5.1 Date and Time Checks

Conduct these checks monthly or whenever daylight savings time changes occur. Compare the

date and time displayed on the sampler to the known date and to an accurately set watch. 

Record information on the QA/QC report form. Refer to Figure 5-1.
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 6 of 12

5.2 Monthly Leak Check

Perform leak check upon startup, then monthly.

1 Install a sampling module containing a filter at the channel location to be leak-checked. 

Use this sampling module for leak checks and flow rate audits only. The module must

contain the type of filter normally used at this sampling channel location. A denuder must

also be in place if called for in the sampling protocol.

2 Remove the sampler inlet assembly. Attach an Andersen flow audit adapter to the down

tube and close the adapter.

3 From the main menu select the “Leak Check” option and press “Enter.” The system

evacuates air and the pump continues to run. The screen must indicate a flow of less than

0.08 L/min for a period of at least 3 minutes. If the system fails this criterion, check for

leaks in the system and repeat the leak check until it is passed successfully. Press the

“Cancel” key when finished.

4 Release vacuum slowly to avoid filter damage.

5.3 Monthly Temperature Control Check

Performed upon startup, then monthly.

1. From the main menu, choose “Maintenance” option and then select “Monitor” option. 

The screen will display real-time values for temperature and pressure.

2. Check the ambient, manifold, and cabinet temperature sensors of the sampler by

positioning the probe of a certified transfer standard digital thermometer in close proximity

to each sampler sensor. Allow time to achieve stable readings and record the results in

the field notebook. 

3. Alternatively, use the Tegam thermocouple calibrator to input -30, 0, and 45°C settings

and record the corresponding temperatures indicated by the RAAS. (Allowable error is

+ 2 °C.) If the sampler and control check temperature readings differ by more than +

2°C, trouble-shoot the system and recheck. If still out of tolerance, conduct a multipoint

calibration or replace the faulty sensor.

5.4 Quarterly Temperature Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.3, but use a

temperature transfer standard that is independent of the one used for the monthly checks. 

Should a temperature sensor not maintain its calibration after the monthly or quarterly checks,

maintenance and/or replacement of the faulty parts must occur.

5.5 Temperature Calibration

1. Unplug the thermocouple labeled “Ambient” on the panel and connect a Tegam®

temperature calibrator.
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 7 of 12

2. From the main screen select “Maintenance” option, then choose “Calibrate”, and select

“Ambient” to calibrate the ambient temperature in the system. 

3. When the system prompts for a low ambient temperature value (-20°C), enter low value

on the Tegam calibrator.

4. Enter value of the Tegam calibrator into the system using numeric keypad.

5. Now the system prompts for a high ambient temperature value (40°C). Enter high value

on the Tegam calibrator.

6. Enter value of the Tegam calibrator into the system using numeric keypad.

7. Change value of the Tegam calibrator and verify this change in the display screen. (The

allowable error is + 2°C.)

8. At the end of ambient temperature calibration, save the calibration by selecting “Yes”

option when the sampler display prompts to do so. 

9. Repeat the procedure to calibrate the meter temperature and the filter temperature.

5.6 Monthly Pressure Control Check

Performed upon startup, then monthly.

1. Compare the ambient barometric pressure readout from the sampler display screen with

the reading from a certified transfer standard barometer.

2. If the pressure readings differ by more than + 10 mm Hg, perform a multipoint calibration

of the sensor or replace the faulty sensor.

5.7 Quarterly Pressure Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.6, but use a pressure

standard that is independent of the one used for the monthly checks. Should the pressure sensor

system not maintain its calibration after the monthly or quarterly checks, then calibration, maintenance,

and/or replacement of the pressure transducer must occur.

5.8 Meter and Barometric Pressure Calibrations

1. Connect a pressure calibration apparatus to the port on the panel located inside of the

unit. Connect one end of a tee to a NIST-traceable external pressure gauge by tubing. 

Connect the other end of the tee to the pressure calibration port in the system by tubing. 

Attach a plastic syringe to the tee’s middle junction by tubing.

2. From the main screen select “Maintenance” option, then choose “Calibrate,” and select

“Meter Drop” to calibrate the meter pressure drop in the system. 

3. When the system prompts for a low pressure value, pull the plunger from the syringe until

the external pressure gauge reads approximately 600 mm Hg. 

4. Clamp the tubing between the syringe and the tee to hold the pressure, and key the exact

value shown by the external pressure gauge into the system. 

5. When the system prompts for a high pressure value, push the plunger until the external

pressure gauge reads approximately 800 mm Hg. 
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 8 of 12

6. Hold pressure, and enter the exact value shown by the external pressure gauge into the

system using the keypad. 

7. Change the value in the external pressure gauge using the syringe and check whether the

value matches with the value shown on the screen. (The allowable error is + 5 mm Hg.)

8. At the end of meter drop pressure calibration, save the calibration by selecting the “Yes”

option when the sampler screen prompts to do so. 

9. Repeat the above procedure to calibrate the barometric pressure sensor.

5.9 Monthly Flow Rate Control Check

Perform the flow rate control check upon startup, then monthly.

1. Use same sampling module called for in Monthly Leak Check procedure (Section 5.2).

2. For denuder channels, disconnect the top of the denuder from the sample manifold

channel outlet. For other channels, disconnect the sampler module from the sample

manifold outlet. Use compression fittings supplied with the sampler to attach a certified

flow transfer standard to the denuder inlet or the sampling module inlet, depending on the

channel to be checked.

3. From the main menu select the “Verify Flow” option to start the flow verification process.

4. After one minute, compare the flow displayed on the screen with the flow indicated by the

external flow meter.

5. Repeat the flow audit procedure for all channels. Channels 1, 2, 5, and 4 flow rates are

preset at 16.7, 7.3, 7.3, and 16.7 L/min, respectively. If the channel’s flow rate error is

greater than 10%, the channel requires flow calibration using a reference dry gas meter

(consult operator’s manual), or maintenance of the pump, or maintenance of the critical

orifice flow controller.

5.10 Quarterly Flow Rate Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.9, but use a flow rate

transfer standard that is independent of the one used for the monthly checks. Should the flow

rate mechanism not maintain its calibration after the monthly or quarterly checks, maintenance

and/or replacement of the flow controller system(s) must occur.

6.0 Sampler Maintenance and Troubleshooting

1. Clean dust from the interior of the sampling cabinet. Use a damp cloth. Clean at least

monthly or more often if local conditions warrant.

2. Pay close attention to O-rings for signs of wear or loosening. Replace O-rings promptly

and leak check the system after replacement.

3. The sample inlet, down tube, and fine particulate cyclones will require periodic cleaning

and maintenance for proper operation. The manufacturer recommends the cyclones be

disassembled and cleaned every 30 sampling days. Refer to Section 11 of the RAAS

operator’s manual for detailed information. 
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 9 of 12

4. Refer to the Andersen RAAS operator’s manual, Section 12, for a thorough discussion of 

troubleshooting techniques.

5. Record all maintenance and troubleshooting activities in the site notebook. On the

CAFDF, record activities that may affect the sample weight or analysis results. 

7.0 References

1. RAASTM Operator’s Manual. Model RAAS2.5-400 Chemical Speciation Monitor. 

Thermo-Andersen Instruments, Inc. Smyrna, GA. Revision 2. September 27, 2000. 
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 10 of 12

BAR CODE GOES HERE PM2.5 STN CUSTODY AND

FIELD DATA FORM

c. White (return to lab)

c. Yellow (site retains)

Custody/Data Form No. c. Pink (lab)

A. CUSTODY RECORD (Name, Date) BIN ID:

1. Laboratory, Out 3. Site, Out 

2. Site, In 4. Lab, In 

B. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name 

2. Sampler S/N 6. Intended date of use 

3. Sampler Type 7. Date of sampler set-up 

4. Sampler POC 8. Operator’s name 

C. SAMPLER CHANNEL COMPONENTS

Channel

Number

Component ID

No.

Component Description

1 I1234567 RAAS module (filter holder) (Teflon filter) (GREEN) 

2 Kept at Site RASS denuder assembly (MgO) (RED)

2 I1234569 RAAS module (nylon filter) (RED)

5 I1234570 RAAS module (quartz filter) (YELLOW)

4 Kept at Site RAAS module (cellulose filter) (BLUE). Operator replaces filter after each run.

D. START, END, AND RETRIEVAL TIMES

Channel No. Start date Start time End date End time Retrieval

date

Retrieval

time

1

2

5

4

E. SAMPLER CHANNEL INFORMATION (Post-Sampling)

Channel

No.

Elapsed

sample time

E. S. time

Flag

Sample

Volume (m3)

Avg. flow

(L/min)

Avg. ambient

T (°C)

Max. ambient

T (°C)

Min. ambient

T (°C)

1

2

5

4

Channel

No.

Avg. BP

(mm Hg)

Max. BP

(mm Hg)

Min. BP

(mm Hg)

aFlow

Flag

aT

Flag

Pump P

(mm Hg)

Manifold

T (°C)

1

2

5

4

F. Comments 

(Revised 02/14/01: 5200)

Figure 4-1. STN Custody and Field Data Form With Entries for the RAAS Sampler.
SOP # 5200STN Andersen RAAS

Rev. # 2

Date: February 14, 2001

Page 11 of 12

QA/QC Form No. PM2.5 STN QA/QC REPORT FORM c. 1 (site retains)

c. 2 (Agency QAM)

A. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name

2. Sampler S/N 6. Interval: Month _______ Quarter ______ Special

______

3. Sampler Type 7. Date(s) of QA/QC Checks 

4. Sampler POC 8. Operator’s Name 

B. DATE AND TIME CHECKS (Transfer Standard Name ____________ Transfer Standard ID Number ____________)

Sample display date/time Transfer standard date/time Date and time agree ± 5 min? Action taken (a)

C. LEAK CHECKS (Transfer Standard Name ___________________ Transfer Standard ID Number ______________)

Channel number Manufacturer’s specifications met? Action taken and recheck results (a)

1

2

5

4

D. TEMPERATURE CHECKS (Transfer Standard Name _____________ Transfer Standard ID Number __________)

Sensor location Sampler display (°C) Transfer standard (°C) Agreement ± 2 °C ? Action taken and

recheck results (a)

Ambient

Cabinet

Manifold

E. PRESSURE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ____________)

Sensor location Sampler display,

(mm Hg) 

Transfer standard,

(mm Hg)

Agreement within

± 10 mm Hg?

Action taken and

recheck results (a)

Ambient

Pump

F. FLOW RATE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ___________)

Channel number Sampler display,

(L/min)

Transfer standard

display, (L/min)

Design flow rate,

(L/min)

Agreement within

± 10 percent? (b) 

Action taken and

recheck results (a)

1

2

5

4

G. COMMENTS 

(Revised 02/14/99: 5200)

(a)Fully describe actions taken in field notebook. 

(b) Sampler flow rate must agree with both transfer standard and design flow rate to pass.

Figure 5-1. STN QA/QC Report Form.
APPENDIX A-4

SOP 5300STN

CONDENSED STANDARD OPERATING

PROCEDURES

FOR THE URG MASS 400 AND URG MASS 450
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 1 of 5

CONDENSED STANDARD OPERATING

PROCEDURES (SOP)

FOR THE URG MASS 400 AND URG MASS 450

Prepared by: Date: 

Prepared by: Date: 

Reviewed by: Date: 

Approved by: Date: 

PM2.5 Speciation Trends Network

Office of Air Quality Planning and Standards

U.S. Environmental Protection Agency

Research Triangle Park, NC 27709
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 2 of 5

1.0 Purpose and Applicability

This condensed standard operating procedure (SOP) outlines procedures for field

operations of the University Research Glassware (URG) Models 400 and 450 MASS PM2.5

speciation samplers. The MASS 400 is a stand-alone system designed to collect trace

metals, anions, and cations. The MASS 450 is a stand-alone system designed to collect

samples for analysis of organic and elemental carbon and semivolatile organic particles. 

For more detailed information regarding operation of either sampler, refer to the URG

MASS operator’s manual.

2.0 Precautions

2.1 Read and thoroughly understand the operator’s manual before beginning field operations. 

The flow rate, temperature, and pressure calibrations of the sampler must be checked and,

if necessary, adjusted to specifications prior to taking the first sample. Consult the

operator’s manual for calibration instructions.

2.2 Use only filter packs and denuders, sent to you from the laboratory, for the designated

sampler and location.

2.3 Exercise great care in placement and handling of sampling modules (i.e., filter packs and

denuders) to avoid contamination.

3.0 Equipment and Supplies

3.1 Have the STN Custody and Field Data Form for the particular sampler, for the particular

sampling day, with you when visiting the site. Have an STN QA/QC Report Form if a

quality control check is due.

3.2 Sampler operator’s manual and field notebook.

3.3 URG MASS 400 and 450 speciation samplers and accessories.

3.4 Teflon filter packs, pre-loaded with filters, for two channels. Field blank modules for use

on every 10th sampling day. Annular denuder for the MASS 400 sampler. Shipping

containers, frozen ice substitutes, and Federal Express labels for shipment of sampling

modules, denuders, and reports to analytical support laboratory. All of this equipment will

be supplied from the support laboratory.

3.5 Independent methods for verifying proper sampler operation.

3.5.1 Date and time. Calendar check. Accurately set watch.

3.5.2 Leaks. Device to close sample flow pathway (flow rate adapter).

3.5.3 Temperature. Thermocouple or thermistor-based digital thermometer transfer

standard with current NIST traceability. Tegam temperature calibrator assembly.

3.5.4 Pressure. Aneroid barometer or equivalent transfer standard with current NIST

traceability.

3.5.5 Flow rate. Low-pressure flow device with leak-tight connection tubing. 

Examples: frictionless piston or soap film flowmeter; orifice-type flowmeter; or

reference dry gas meter with thermometer and tubing connections. Each should

have current NIST traceability.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 3 of 5

4.0 Sampler Operating Procedures

Record information about the sample, the field blank, or the trip blank on an individual PM2.5

STN Custody and Field Data Form (CAFDF) (see Figure 4-1). The procedures given below

apply to both the MASS 400 and MASS 450 stand-alone systems.

4.1 Sample Preparation and Programming the URG MASS 400 or 450 Sampler

1. Remove caps from the filter packs. Store the caps in a clean plastic bag. The caps will be

used to seal the filter pack following sampling. Install loaded filter packs in the sampling

channel locations according to the sample channel information given on the CAFDF sent

from the support laboratory. Channel 1 is the MASS 400 sampler; channel 2 is the

MASS 450 sampler. Refer to Section 4.3. 

2. From main menu, choose the “Setup Run” option, and press the “Enter” key to select

Filter 1. User information and filter ID number can be entered at this time. Key in the

custody/data form number (this is printed on the CAFDF). Double-check the entry.

3. Press the “Enter” key again.

4. Enter the start date (MMDDYY format) and press the “Enter” key.

5. Enter the sample duration in hours, then press “Enter” to complete setup.

6. Make entries to the CAFDF.

4.2 Data Retrieval

1. At the end of the sample run, return to the main screen.

2. Select “View Run”, and choose “Last Sample” option to view information about the

previous sampling event.

3. Record the end date/time, sample retrieval date/time, specified post-sampling information,

and free-form comments on the CAFDF. Please double-check entries and write

clearly!

4. Return to the main screen by pressing the “Cancel” button.

5. Download data electronically to a laptop computer or to the MASS Data Link accessory. 

Refer to Section 7 of the operator’s manual for further instruction on data logging. Retain

the data file disk for later use in data validation. Do not send it to the support laboratory.

4.3 Filter Pack Handling

The field operator will be shipped filter packs for several uses. These are for routine (every third

day) sampling, field blanks (sent for use on every tenth sampling day), and trip blanks (sent every

thirty sampling days).

It is highly recommended that sampling modules (i.e. filter packs) be removed from the

sampler within 48 hours after the sampling period ends. For a one-in-three day schedule this

will be necessary since the next sampling day’s filter packs must be installed. 
SOP # 5400STN Packing Instructions

Rev. # 1

Date: December 20, 2000

Page 4 of 4

Once the sampled filter packs are removed from the sampler, cap both ends , place the filter

packs in plastic zip-lock bags, store them in the shipping container , and return them to the field

office. The sampled filter packs and paperwork must be properly packaged in a cooler,

ready for pickup by Federal Express, within 96 hours after the sampling period ends. The

support laboratory will provide specific directions for packaging and shipment and days

for shipment. Protect samples from direct sunlight and extreme heat during transport from the

site to the field office; store them in a secure, air-conditioned area until just before packaging

them in the cooler. 

Days of the week for shipment will be arranged in coordination with the DOPO and

laboratory. Do not ship on Fridays or the day before a holiday unless prior arrangements

are made with the DOPO and laboratory. 

Routine Samples

6. At the end of sample run, remove the tubing located at the bottom of the filter pack.

7. Gently twist (1⁄4 turn) to unlock the WINS impactor/filter assembly from the down tube

connector. Note: The filter holder is threaded to the WINS impactor.

8. Holding the WINS upright in one hand, unscrew the filter pack from the WINS.

9. Cap both ends of the just-removed filter pack. Attach a new filter pack to the WINS

impactor.

10. Align WINS to the down tube connector and twist (1/4 turn) to lock.

11. Connect tubing to the bottom of the filter pack.

12. Place each used filter pack into individual, prelabeled zip-lock style bags and place in the

cooler.

Field Blank Filters

1. Field blank filters, loaded into filter packs, will be shipped from the laboratory. They will

each have a separate CAFDF with them. They are to be used during the same time

interval as the routine sample filter packs.

2. Visit the site at the time regularly scheduled for setting up for a new sampler run. Install

the field blank filter packs in the MASS 400 and MASS 450 sampling channel locations

as indicated by the CAFDF. 

3. After a minute or two, remove the field blank filter packs, cap them, place each inside a

plastic zip-lock bag, and return them to the shipping container.

4. Proceed to install the routine sample filter packs according to schedule.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 5 of 11

Trip Blank Filters

1. Trip blank filters, loaded into filter packs, will be shipped from the laboratory. They will

have a separate STN Custody and Field Data Form (CAFDF) with them. They are to

be used during the same time interval as the routine sample filter packs.

2. The trip blank filter packs should be carried to the site but left in the cooler

containers. They should not be installed in the sampler.

3. Complete and sign the CAFDF for the trip blank filter packs and ship them back to the

laboratory at the same time as the routine samples.

4.4 Denuder Handling

If it is time to refurbish the denuder(s), follow these steps for the MASS 400 or 450.

1. Remove the sampler inlet head. Disconnect the downtube (it contains the denuder),cap

it, and place it in the cooler. Replace with a fresh downtube/denuder. Reinstall the

sample inlet.

2. Place the denuder in the appropriate slot in the shipping cooler to be returned to the

laboratory for refurbishment.

5.0 Sampler QA/QC Procedures

Certain quality control checks must be conducted at the time of sampler startup and at

monthly or quarterly intervals thereafter. Carry out these checks before making any

adjustments to the samplers. Record information about the site, the samplers, and the

results of scheduled or special (unscheduled) quality control checks on the PM2.5 STN

QA/QC Report Form, Figure 5-1. The site operator should keep the original on file and

send copies to the State or local agency QA Manager and to the analytical laboratory. This

report form originates at the field site. Any actions taken to service or calibrate the

speciation sampler after the check must be recorded in brief on the form and in detail in the

field operator’s notebook.

5.1 Date and Time Checks

Conduct these checks monthly or whenever daylight savings time changes occur. Compare the

date and time displayed by the samplers to the known date and to an accurately set watch.

Record this information on the QA/QC field data form. See Figure 5-1.

5.2 Monthly Leak Check

Perform leak check upon startup, then monthly.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 6 of 11

1. Place filter pack containing filter at channel location to be leak-checked. Use this

filter pack assembly for leak checks and flow rate checks only. The filter pack must

contain the type of filter normally used at this sampling channel location. A denuder

should also be in place if called for in the sampling protocol.

2 Attach a flow rate adapter to the down tube and close the adapter.

3. From the main menu select the “Leak Check” option and press “Enter”. The system

evacuates air and the pump continues to run. The screen must indicate a flow of less

than 0.08 L/min for a period of 10 minutes. The timer will reset if flow exceeds 0.08

L/min. If the system fails this criterion, check for leaks in the system and repeat the leak

check until it is passed successfully. Press “Cancel” or any other key when finished.

4. Release vacuum slowly to avoid filter damage and splashing impactor oil.

5.3 Monthly Temperature Control Check

Performed upon startup, then monthly.

1. From the main menu, choose “Maintenance” option and then select “Monitor” option.

The screen will display real-time values for temperature and pressure.

2. Check the ambient, meter, and filter temperature sensors of the sample by positioning

the probe of a certified transfer standard digital thermometer in close proximity to the

sampler sensors. Allow time to achieve stable readings and record the results in the field

notebook and on the STN QA/QC report form.

3. Alternatively, use the Tegam thermocouple calibrator to input -30, 0, and 45EC

settings and record the corresponding temperatures indicated by the MASS sampler.

(Allowable error is + 2EC.) If the sampler and control check temperature readings

differ by more than + 2EC, trouble-shoot the system and recheck. If still out of

tolerance, conduct a multipoint calibration or replace the faulty sensor. 

5.4 Quarterly Temperature Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.3, but use a

temperature transfer standard that is independent of the one used for the monthly checks.

Should a temperature sensor not maintain its calibration after the monthly or quarterly

checks, maintenance and/or replacement of the faulty parts must occur.

5.5 Temperature Calibration

1. Unplug the thermocouple labeled “Ambient” on the panel and connect a Tegam

temperature calibrator.

2. From the main screen select “Maintenance” option, then choose “Calibrate”, and

select “Ambient” to calibrate the ambient temperature in the system.

3. When the system prompts for a low ambient temperature value (-20EC), enter low 

value on the Tegam Calibrator.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 7 of 11

4. Enter value of the Tegam Calibrator into the system using numeric keypad.

5. Now the system prompts for a high ambient temperature value (40EC). Enter high

value on the Tegam Calibrator.

6. Enter value of the Tegam Calibrator into the system using numeric keypad.

7. Change value of the Tegam Calibrator and verify this change in the display screen 

(The allowable error is + 2EC.)

8. At the end of ambient temperature calibration, save the calibration by selecting “Yes”

option when the instrument prompts.

9. Repeat the procedure to calibrate the meter temperature and the filter temperature.

5.6 Monthly Pressure Control Check

Performed upon startup, then monthly.

1. Compare the ambient barometric pressure readout from the sampler display screen

with the reading from a certified transfer standard barometer.

2. If the pressure readings differ by more than + 10 mm Hg, perform a multipoint

calibration of the sensor or replace the faulty sensor.

5.7 Quarterly Pressure Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.6, but use a

pressure standard that is independent of the one used for the monthly checks. Should the

pressure sensor system not maintain its calibration after the monthly or quarterly checks,

maintenance, and/or replacement of the pressure transducer must occur.

5.8 Meter and Barometric Pressure Calibrations

1. Connect a pressure calibration apparatus to the port on the panel located inside of the 

unit. Connect one end of a tee to an external pressure gauge by tubing. Connect the

other end of the tee to the pressure calibration port in the system by tubing. Attach a

plastic syringe to the middle tee junction by tubing.

2. From the main screen select “Maintenance” option, then choose “Calibrate”, and

select “Meter Drop” to calibrate the meter pressure drop in the system.

3. When the system prompts for a low pressure value, pull the plunger from syringe until

the external pressure gauge reads approximately 600 mm Hg.

4. Clamp the tubing between the syringe and the tee to hold the pressure, and key the

exact value shown by external pressure gauge into the system.

5. When the system prompts for a high pressure value, push the plunger until the

external pressure gauge reads approximately 800 mmHg.

6. Hold the pressure, and enter the exact value shown in external pressure gauge into the

system using keypads.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 8 of 11

7. Change the value in the external pressure gauge using the syringe and check whether

the value matches with the value shown on the screen. (The allowable error is + 5 mm

Hg.)

8. At the end of meter drop pressure calibration, save the calibration by selecting the

“Yes” option when the instrument prompts.

9. Repeat the procedure to calibrate the barometric pressure sensor.

5.9 Monthly Flow Rate Control Check

Perform flow rate control check upon startup, then monthly.

1. Use same filter pack assembly called for in monthly Leak Check Procedure

(Section 5.2).

2. Connect a flow audit adapter to the down tube. Open the adapter and connect a

certified flow transfer standard to the adapter inlet.

3. From the main menu select the “Verify Flow” option to start the flow verification

process.

4. After one minute, compare the average flow displayed on the sampler’s screen with

flow indicated by the external flow meter.

5. Repeat the flow audit procedure for the other URG unit. The channels are preset at a

flow of 16.7 L/min. If the channel’s flow error is greater than 2%, that channel’s

flow rate control mechanism requires calibration or servicing.

6. If a dry gas meter is used for flow rate checks, the meter’s calibration coefficient,

initial and final volume readings, and temperature must be entered in response to the

screen prompts in order for the sampler to compute a flow rate for comparison. Refer

to the operator’s manual for details.

5.10 Quarterly Flow Rate Control Check

Performed each calendar quarter. Follow the same steps as in Section 5.9, but use a flow

rate transfer standard that is independent of the one used for the monthly checks. Should

the flowrate mechanism not maintain its calibration after the monthly or quarterly checks,

maintenance and/or replacement of the flow controller system(s) must occur.

6.0 Sampler Maintenance and Troubleshooting

1. Clean dust from the interior of the sampling cabinets. Use a damp cloth. Clean at

least monthly or more often if local conditions warrant.

2. The MASS 400 and MASS 450 employ the FRM WINS impactor system to remove 

coarse particles. A periodic cleaning and maintenance schedule similar to that for FRM

samplers should be instituted.

• Every 5 sampling days. Service water collector bottle and clean or change out

 the impactor well filter and oil.

• Monthly. Clean sampler inlet surfaces. Examine O-rings of WINS and replace if

 needed.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 9 of 11

• Quarterly. Inspect O-rings of inlet. Clean sampler downtube (denuder

 downtube is cleaned and refurbished in the laboratory). Inspect and service

 other O-rings, vacuum tubing, and other pneumatic and electrical connections.

 Inspect and service cooling air intake filter and fan.

3. Refer to the URG MASS 400 and 450 operator’s manual for further information on

electrical and pneumatic system maintenance.

7.0 References

1. Model MASS 400, Model MASS 450 Operator’s Manual. URG Inc. Chapel Hill,

NC. April 17, 1998.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 10 of 11

QA/QC Form No. PM2.5 STN QA/QC REPORT FORM c. 1 (site retains)

c. 2 (Agency QAM)

A. CUSTODY RECORD (Name, Date) BIN ID:

1. Laboratory, Out 3. Site, Out 

2. Site, In 4. Lab, In 

B. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name 

2. Sampler S/N 6. Intended date of use 

3. Sampler Type 7. Date of sampler set-up 

4. Sampler POC 8. Operator’s name 

C. SAMPLER CHANNEL COMPONENTS

Channel

Number

Component ID

No.

Component Description

1 I1234567 MASS 400 denuder (sodium carbonate 

1 I1234567 MASS 400 Filter Pack (Teflon, Nylon fiters)

2 I1234569 MASS 450 Filter Pack (quartz)

D. START, END, AND RETRIEVAL TIMES

Channel No. Start date Start time End date End time Retrieval

date

Retrieval

time

1

2

E. SAMPLER CHANNEL INFORMATION (Post-Sampling)

Channel

No.

Elapsed

sample time

E. S. time

Flag

Sample

Volume (m3)

Avg. flow

(L/min)

Avg. ambient

T (°C)

Max. ambient

T (°C)

Min. ambient

T (°C)

1

2

Channel

No.

Avg. BP

(mm Hg)

Max. BP

(mm Hg)

Min. BP

(mm Hg)

aFlow

Flag

aT

Flag

Pump P

(mm Hg)

Manifold

T (°C)

1

2

F. Comments 

(Revised 02/14/01: 5200)

Figure 4-1. STN Custody and Field Data Form With Entries for the RAAS Sampler.
SOP # 5300STN URG MASS 400 & 450

Rev. # 1

Date: September 30, 1999

Page 11 of 11

QA/QC Form No. PM2.5 STN QA/QC REPORT FORM c. 1 (site retains)

c. 2 (Agency QAM)

A. SITE AND SAMPLER INFORMATION

1. Site AIRS Code 5. Site Name

2. Sampler S/N 6. Interval: Month _______ Quarter ______ Special

______

3. Sampler Type 7. Date(s) of QA/QC Checks 

4. Sampler POC 8. Operator’s Name 

B. DATE AND TIME CHECKS (Transfer Standard Name ____________ Transfer Standard ID Number ____________)

Sample display date/time Transfer standard date/time Date and time agree ± 5 min? Action taken (a)

C. LEAK CHECKS (Transfer Standard Name ___________________ Transfer Standard ID Number ______________)

Channel number Manufacturer’s specifications met? Action taken and recheck results (a)

1

2

5

4

D. TEMPERATURE CHECKS (Transfer Standard Name _____________ Transfer Standard ID Number __________)

Sensor location Sampler display (°C) Transfer standard (°C) Agreement ± 2 °C ? Action taken and

recheck results (a)

Ambient

Filter

Dry Gas Meter

Manifold

E. PRESSURE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ____________)

Sensor location Sampler display,

(mm Hg) 

Transfer standard,

(mm Hg)

Agreement within

± 10 mm Hg?

Action taken and

recheck results (a)

Ambient

Manifold

F. FLOW RATE CHECKS (Transfer Standard Name ________________ Transfer Standard ID Number ___________)

Channel number Sampler display,

(L/min)

Transfer standard

display, (L/min)

Design flow rate,

(L/min)

Agreement within

± 10 percent? (b) 

Action taken and

recheck results (a)

1

2

G. COMMENTS 

(Revised 02/14/99: 5200)

(a)Fully describe actions taken in field notebook. 

(b) Sampler flow rate must agree with both transfer standard and design flow rate to pass.

Figure 5-1. STN QA/QC Report Form.
APPENDIX A-5

SOP 5400STN

PACKING INSTRUCTIONS FOR THE

SPECIATION SAMPLER MODULES 
SOP # 5400STN Packing Instructions

Rev. # 1

Date: January 18, 2001

Page 1 of 6

STANDARD OPERATING PROCEDURES 

FOR PACKING INSTRUCTION OF THE

SPECIATION SAMPLERS

Prepared by: Date: 

Reviewed by: Date: 

Approved by: Date: 

PM2.5 Speciation Trends Network

Office of Air Quality Planning and Standards

U.S. Environmental Protection Agency

Research Triangle Park, NC 27709
SOP # 5400STN Packing Instructions

Rev. # 1

Date: January 18, 2001

Page 2 of 6

1.0 Purpose and Applicability

This condensed standard operating procedure (SOP) outlines the procedures for packing

the modules for the speciation samplers. The URG Models 400 and 450, Andersen RASS

and Met One SASS PM2.5 speciation sampler instructions are included in this SOP. 
SOP # 5400STN Packing Instructions

Rev. # 1

Date: January 18, 2001

Page 3 of 6

PACKAGING INSTRUCTIONS FOR ANDERSEN PM2.5 FILTER MODULES

1

Make sure the horizontal and vertical

dividers are arranged in the transport bin as

shown in the photo. 4

Place the remaining three polyethylene

foam squares on top of the three Andersen

sampling modules.

2 Place eight frozen FREEZ PAK®

s

(sealed in bags) and three of the

polyethylene foam squares in the bin

p arti

t ion

s as

s ho

w n.

5

Place the PM 2.5 STN CUSTODY AND

FIELD DATA FORM in the resealable

plastic bag and place the bag on top of the

bin contents.

3

Place the three Andersen sampling

modules (sealed in bags) on top of the

foam squares in the bin. 6

Place the clear plastic lid on the bin. (See

separate instructions for preparing the

cooler for shipment.)
SOP # 5400STN Packing Instructions

Rev. # 1

Date: January 18, 2001

Page 4 of 6

PACKAGING INSTRUCTIONS FOR URG PM2.5 SAMPLING MODULES

1

Make sure the horizontal and vertical dividers are

arranged in the transport bin as shown below. 4

Place the remaining two polyethylene foam squares

on top of the two URG sampling modules.

2

Place eight frozen FREEZ PAK®s (in sealed bags)

and two of the polyethylene foam squares in the bin

partitions as shown. 5

Place the PM 2.5 STN CUSTODY AND FIELD DATA

FORM in the resealable plastic bag and place the

bag on top of the bin contents.

3

Place the two URG sampling modules (in sealed

bags) on top of the polyethylene foam squares in

the bin. 6

Place the clear plastic lid on the bin. (See separate

instructions for preparing the cooler for shipment.)
SOP # 5400STN Packing Instructions

Rev. # 1

Date: January 18, 2001

Page 5 of 6

PACKAGING INSTRUCTIONS FOR MET ONE PM2.5 SAMPLING MODULES

1

Make sure the horizontal and vertical dividers are

arranged in the transport bin as shown in the photo. 4

Place the remaining three polyethylene foam

squares on top of the three Met One sampling

modules.

2

Place eight upright frozen FREEZ PAK®s (in sealed

bags) and three of the polyethylene foam squares in

the bin partitions as shown. 5

Place the PM 2.5 STN CUSTODY AND FIELD DATA

FORM in the resealable plastic bag and place the

bag on top of the bin contents.

3

Place the three Met One sampling modules (in sealed

bags) on top of the polyethylene foam squares in

the bin. 6

Place the clear plastic lid on the bin. (See separate

instructions for preparing the cooler for shipment.)
SOP # 5400STN Packing Instructions

Rev. # 1

Date: January 18, 2001

Page 6 of 6

PACKAGING INSTRUCTIONS FOR IGLOO ULTRACOLDTM 50 COOLERS

1

Place one of the custom-cut large rectangular blocks of

polyethylene foam in the bottom of the Igloo

UltraColdTM 50 Cooler. 4

Place twelve frozen FREEZ PAK®s on top of the bin in

two rows of six each. Make sure that the packs are

standing upright. Several operators have stated that

the packs may leak if they placed on their sides. It is

strongly recommended that the packs be placed

upright. 

2

Place the two smaller rectangular blocks of

polyethylene foam at the ends of the cooler as shown. 5

Place the remaining large block of polyethylene foam

on top of the bin in the cooler.

3

Place the transport bin containing the sampling

modules in the cooler between the polyethylene foam

blocks. 6

Close the cooler and place the preprinted return

FedEx airbill on top as shown.
APPENDIX A-6

CY-2001 1-IN-3 DAY SAMPLING AND

ALTERNATE SCHEDULE FOR THE

SPECIATION TRENDS NETWORK
CY-2001 STN Schedule

Rev. # 1

Date: December 20, 2000

Page 1 of 4

CY-2001 1-IN-3 DAY SAMPLING AND

ALTERNATE SCHEDULE FOR THE

SPECIATION TRENDS NETWORK

Prepared by: Date: 

Reviewed by: Date: 

Approved by: Date: 

PM2.5 Speciation Trends Network

Office of Air Quality Planning and Standards

U.S. Environmental Protection Agency

Research Triangle Park, NC 27709
CY-2001 STN Schedule

Rev. # 1

Date: December 20, 2000

Page 2 of 4

1.0 Purpose and Applicability

This appendix is designed to allow the operators, RTI lab personnel and EPA to verify and

plan the deployment the speciation modules within the Speciation Trends Network for

Calendar Year 2001. Please note there are two schedules. The first is the normal schedule

that will be operated by those agencies that will be able to deploy the sample modules

during the weekends. The second schedule is designed to allow the agencies that will not

be able to deploy the samples during the weekend. The difference is that alternating

Mondays and Fridays will be missed. 

Note: It is important to note that keeping to the schedule is extremely important to the

laboratory operations. If the modules are not placed in the sampler due to using the

Alternate Schedule, the unexposed modules must be sent back to contractor laboratory

when they are scheduled to be returned. This insures that the State or Local agency has

enough modules in the system. 
CY-2001 STN Schedule

Rev. # 1

Date: December 20, 2000

Page 3 of 4
CY-2001 STN Schedule

Rev. # 1

Date: December 20, 2000

Page 4 of 4
APPENDIX A-7

TECHNICAL GUIDANCE DOCUMENT

UPDATES
Appendix A-7

Rev. # 1

Date: December 20, 2000

Page 1 of 1

1.0 Purpose and Applicability

This appendix is designed to be a place holder for Technical Guidance Document Updates

that will be forward from time to time. As more information is gathered concerning the

QA and QC of speciation sampler, this information will be disseminated from OAQPS to

the State and Local Agencies through the DOPOs. This appendix is where these updates

are stored. 

 
TECHNICAL REPORT DATA

(Please read Instructions on reverse before completing)

1. REPORT NO.

 EPA-354/R01-001

2. 3. RECIPIENT'S ACCESSION NO.

4. TITLE AND SUBTITLE

Quality Assurance Guidance Document, Quality Assurance

Project Plan: PM2.5 Speciation Trends Network Field Sampling

 

5. REPORT DATE

 01/01

6. PERFORMING ORGANIZATION CODE

7. AUTHOR(S)

 Dennis Mikel, James Flanagan, David Musick, James Homalya

 

8. PERFORMING ORGANIZATION REPORT NO.

9. PERFORMING ORGANIZATION NAME AND ADDRESS

 U.S. Environmental Protection Agency

 Office of Air Quality Planning and Standards

 Research Triangle Park, NC 27711

10. PROGRAM ELEMENT NO.

11. CONTRACT/GRANT NO.

 

12. SPONSORING AGENCY NAME AND ADDRESS

 Director

 Office of Air Quality Planning and Standards

 Office of Air and Radiation

 U.S. Environmental Protection Agency

 Research Triangle Park, NC 27711

13. TYPE OF REPORT AND PERIOD COVERED

14. SPONSORING AGENCY CODE

EPA/200/04

15. SUPPLEMENTARY NOTES

16. ABSTRACT

The Quality Guidance Document is the Quality Assurance Project Plan that outlines the field operations for the

PM2.5 Speciation Trends Network. The guidance document gives details on how to

set-up, operate, and perform all quality control and assurance duties that are required to provide precise, accurate

and representative data for this program. This guidance document also has six appendices. The first four are

Standard Operating Procedures for Speciation samplers. The fifth appendix provides details on how to load filter

modules into coolers before they are shipped to the central laboratory. Appendix A-6 illustrates the 1 in 3 day

schedule for CY 2001. In addition, Appendix A-6 provides an alternate schedule for agencies that cannot operate

the samplers on weekends. 

17. KEY WORDS AND DOCUMENT ANALYSIS

a. DESCRIPTORS b. IDENTIFIERS/OPEN ENDED TERMS c. COSATI Field/Group

Air Quality Monitoring

Quality Assurance 

Air Pollution control

18. DISTRIBUTION STATEMENT

 Release Unlimited

19. SECURITY CLASS (Report)

 Unclassified

21. NO. OF PAGES

20. SECURITY CLASS (Page)

 Unclassified

22. PRICE

EPA Form 2220-1 (Rev. 4-77) PREVIOUS EDITION IS OBSOLETE