UCMR 3 Laboratory 

Approval Requirements 

and Information 

Document
Office of Water (MLK 140)

EPA 815-R-10-004

December 2010

http://water.epa.gov/drink
Page 1 of 41

UCMR 3 

Laboratory Approval Requirements 

and Information Document

Version 1.0

December 2010

Technical Support Center 

Standards and Risk Management Division 

Office of Ground Water and Drinking Water 

U.S. Environmental Protection Agency 

Cincinnati, OH 45268 

Laboratory Manager: ________________________________ 

This signature affirms that the Laboratory Manager

and staff anticipated to participate in UCMR 3 have read the

UCMR 3 Laboratory Approval Requirements and Information Document. 
Page 2 of 41

Foreword

The proposed Revisions to the Unregulated Contaminant Monitoring Regulation (UCMR 3) for 

Public Water Systems [40 CFR Part 141, National Primary Drinking Water Regulations] require 

public water systems (PWSs) collect specific data and information during a defined monitoring 

period. The proposed rule for the third UCMR (UCMR 3) establishes requirements and 

specifications for the collection and reporting of UCMR 3 data to the United States 

Environmental Protection Agency (EPA). This technical manual serves as a support document 

for laboratories interested in becoming approved to analyze samples collected at PWSs to meet 

the UCMR 3 requirements for chemical contaminants. 

The main objective of this UCMR 3 Laboratory Approval Requirements and Information 

Document (referred to as the UCMR 3 Lab Approval Manual) is to provide laboratories with 

detailed information on the UCMR 3 laboratory approval process. The document is intended to: 

• describe the laboratory approval process for chemical contaminants, 

• describe the procedures that EPA uses to assess a laboratory's ability to produce data of 

known accuracy and precision, 

• describe the laboratory data quality control requirements for UCMR 3 chemical analyses,

and

• clarify specific analytical procedures for UCMR 3. 

Within twelve months or less of the publication of the UCMR 3 final rule the UCMR 3

Laboratory Approval Program (LAP) is expected to close and a UCMR 3 Laboratory Manual 

will be published that supersedes this Lab Approval Manual. Copies of the UCMR 3 Lab 

Manual will be sent to all laboratories that attain EPA approval to support UCMR 3. 

Laboratories will be required to follow the UCMR 3 Laboratory Manual to process UCMR 3

samples collected at PWSs and maintain their status as an EPA approved UCMR 3 laboratory. 

This document was prepared by EPA’s Office of Ground Water and Drinking Water (OGWDW), 

Standards and Risk Management Division (SRMD), Technical Support Center (TSC), 

Cincinnati, Ohio. Additional information on the UCMR 3 program can be found at the UCMR 3

website, 

http://water.epa.gov/lawsregs/rulesregs/sdwa/ucmr/ucmr3/index.cfm
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Disclaimers 

1. Mention of trade names or commercial products does not constitute endorsement or 

recommendation for use. 

2. This document describes the provisions of the proposed UCMR 3 program, the approved 

analytical methods for UCMR 3 chemical contaminants, and EPA regulations that establish 

legally binding requirements. However, this document does not substitute for those 

provisions or regulations. Contaminants and methods identified in this document are 

subject to change over the course of development and promulgation of the final 

UCMR 3. 

3. Laboratory approval to perform UCMR 3 analyses will only apply during UCMR 3

monitoring. If new drinking water regulations are promulgated using similar analyses and

the same methods, laboratories will then be required to be certified through the process 

appropriate to their primacy agent (i.e., their State and/or EPA Region). 

4. The UCMR 3 approval process is not related to the laboratory certification process for 

conducting compliance monitoring under other National Primary Drinking Water 

Regulations (NPDWRs). A laboratory’s approval for UCMR 3 analyses has no impact on 

their certification to perform compliance monitoring under other NPDWRs. 
Page 4 of 41

Contents

Foreword ........................................................................................................................................ 2

Disclaimers..................................................................................................................................... 3

Acronyms and Abbreviations ...................................................................................................... 6

Section 1. Introduction ................................................................................................................. 9

1.1 Background on the Unregulated Contaminant Monitoring Regulation ................................. 9

1.2 Ensuring Data Quality for UCMR 3 ...................................................................................... 9

Section 2. UCMR 3 Laboratory Approval Process .................................................................. 11

2.1 Registration for the UCMR 3 Laboratory Approval Program ............................................. 11

2.2 UCMR 3 LAP Applications ................................................................................................ 11

2.3 UCMR 3 Proficiency Testing .............................................................................................. 12

Section 3. Laboratory Quality Management Plan and UCMR 3 Quality Assurance 

Project Plan ..................................................................................................................... 14

3.1 Laboratory Quality Management Plan ................................................................................ 14

3.2 UCMR 3 Quality Assurance Project Plan ........................................................................... 16

Section 4. Approved Methods for UCMR 3 Monitoring ......................................................... 17

Section 5. Initial Demonstration of a Laboratory's Ability to Perform UCMR 3 

Analyses ........................................................................................................................... 22

Section 6. Minimum Reporting Levels ...................................................................................... 24

Section 7. Quality Control Requirements ................................................................................. 26

7.1 Initial Calibration of Analytical Instruments ....................................................................... 27

7.2 Continuing Calibration Checks ........................................................................................... 29

7.3 Surrogate Requirements and Criteria .................................................................................. 30

7.4 Internal Standard Requirements and Criteria ...................................................................... 32

7.5 Laboratory Reagent Blank ................................................................................................... 34

7.6 Laboratory Fortified Blank .................................................................................................. 35

7.7 Laboratory Fortified Sample Matrix (Spiked Sample) ........................................................ 36

7.8 Analytical Sequence ............................................................................................................ 37

Appendix A. Requirements for UCMR 3 Metal Analysis ....................................................... 39

Section 8. References .................................................................................................................. 40
Page 5 of 41

Tables

Table 1. UCMR 3 List 1 Assessment Monitoring Chemical Analytes and Methods ................... 20

Table 2. IDC Requirements .......................................................................................................... 23

Table 3. Initial Calibration Acceptance Criteria ........................................................................... 28

Table 4. CCC Acceptance Criteria................................................................................................ 30

Table 5. Surrogate Standards, Concentrations and Criteria .......................................................... 31

Table 6. Internal Standards, Concentrations and Criteria ............................................................. 33

Table 7. Laboratory Reagent Blank Criteria ................................................................................. 35

Table 8. Laboratory Fortified Blank Acceptance Criteria ............................................................ 36

Table 9. Specifics for the Determination of Metals for UCMR 3 ................................................ 39

Examples 

Example 1. Calculation of the PIR Limits .................................................................................... 25

Example 2. Valid Analysis Sequence for Method 537 ................................................................. 38
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Acronyms and Abbreviations

13C-PFDA

13C-PFHxA

13C-PFOA

13C-PFOS

Perfluoro-n-[1,2-13C2]decanoic acid

Perfluoro-n-[1,2-13C2]hexanoic acid

Perfluoro-[1,2-

13C2]octanoic acid

Sodium perfluoro-1-[1,2,3,4-

13C4]octanesulfonate

APHA American Public Health Association 

ASTM ASTM International

AWWA American Water Works Association 

Bi Bismuth

BFB 4-bromofluorobenzene 

C18 Octadecyl-functionalized silica gel

CAS Chemical Abstract Service

CCC Continuing calibration check

CFR Code of Federal Regulations

Co Cobalt

d3-NMeFOSAA N-deuteriomethylperfluoro-1-octanesulfonamidoacetic acid

d5-NEtFOSAA N-deuterioethylperfluoro-1-octanesulfonamidoacetic acid

DCA Dichloroacetate

EPA United States Environmental Protection Agency

Estriol-d2 16α-hydroxyestradiol-d2

GC/MS Gas chromatography/mass spectrometry

HRPIR Half range for the prediction interval of results 

IC Ion chromatography 

ICP/MS Inductively coupled plasma - mass spectrometer 

ID Identification

IDA Initial demonstration of accuracy

IDC Initial demonstration of capability

IDP Initial demonstration of precision

In Indium 

L Liter

LAP Laboratory Approval Program

LCMRL Lowest concentration minimum reporting level

LC-ESI-MS/MS Liquid chromatography electrospray ionization tandem mass spectrometry

LC/MS/MS Liquid chromatography/tandem mass spectrometry

LFB Laboratory fortified blank 

LFSM Laboratory fortified sample matrix
Page 7 of 41

Acronyms and Abbreviations

LFSMD

LRB

mL

Laboratory fortified sample matrix duplicate

Laboratory reagent blank

Milliliter

Mo

MRL

m/z

NA

NERL

OEI

Molybdenum 

Minimum reporting level

Mass to charge ratio

Not applicable 

National Exposure Research Laboratory

Office of Environmental Information

OGWDW

ORD

PFBS

Office of Ground Water and Drinking Water

Office of Research and Development 

Perfluorobutanesulfonic acid

PFHpA

PFHxS

Perfluoroheptanoic acid

Perfluorohexanesulfonic acid

PFNA Perfluorononanoic acid

PFOA Perfluorooctanic acid

PFOS Perfluorooctanesulfonic acid

PIR Prediction interval of the result 

PIRlower Lower PIR limit

PIRupper

PT

PWS

QA

QAPP

QC

QCS

QMP

RSD

Upper PIR limit

Proficiency testing

Public water system

Quality assurance

Quality Assurance Project Plan

Quality control 

Quality control sample

Quality Management Plan

Relative standard deviation

RPD

s 

Relative percent difference

Standard deviation 

Sc Scandium 

SDVB

SDWA

SDWARS

SIM

SM

Polystyrenedivinylbenzene

Safe Drinking Water Act

Safe Drinking Water Accession and Review System

Selective ion monitoring 

Standard Methods for the Examination of Water and Wastewater

SOP Standard operating procedure
Page 8 of 41

Acronyms and Abbreviations

SPE Solid phase extraction

Sr Strontium 

Tb Terbium 

TSC Technical Support Center 

THF-d8 Tetrahydrofuran-d8

UCMR Unregulated Contaminant Monitoring Regulation 

UCMR 1 First Unregulated Contaminant Monitoring Regulation 

UCMR 2 Second Unregulated Contaminant Monitoring Regulation 

UCMR 3 Third Unregulated Contaminant Monitoring Regulation 

(v:v) Volume to volume 

V Vanadium 

VOC Volatile organic contaminant 

WEF Water Environment Federation 

x Mean

μL Microliter
Page 9 of 41

Section 1. Introduction

1.1 Background on the Unregulated Contaminant Monitoring Regulation

The Safe Drinking Water Act (SDWA), as amended in 1996, requires the EPA to establish 

criteria for a program to monitor unregulated contaminants and to publish a list of contaminants 

to be monitored every five years. In fulfillment of this requirement, EPA published the proposed 

contaminant lists for the first and second UCMRs (i.e., UCMR 1 and UCMR 2, respectively) in 

the Federal Register in September 1999 and August 2005. Previously UCMR established a threetiered approach for monitoring contaminants based on the availability of analytical methods. 

UCMR 3 monitoring will utilize a similar three-tiered approach, and the monitoring period is 

proposed from January 2013 through December 2015. 

EPA identified 28 chemical contaminants for the proposed UCMR 3. Monitoring for these 

contaminants is supported by ten analytical methods. EPA identified 30 total contaminants for 

the proposed UCMR 3, including two viruses. Virus analyses will be conducted by laboratories 

under contract with EPA and are not addressed in this document. 

Laboratories should be aware that this document is based upon the proposed UCMR 3 and 

will be revised once the final UCMR 3 rule is promulgated. Contaminants and methods 

identified in this document are subject to change. 

1.2 Ensuring Data Quality for UCMR 3

Data reported under UCMR 3 must meet specific accuracy and precision targets to achieve the 

objectives of the program. During UCMR 3 development, EPA established criteria to ensure that 

data generated during the monitoring period are high in quality. Maintaining data comparability 

between laboratories is essential, and will allow the data to be used in sophisticated statistical 

analyses to reliably predict the national occurrence of the 28 chemical contaminants in drinking 

water. EPA ensures the integrity of the data by: 1) defining and maintaining strict requirements 

for sample collection, sample handling, processing and analysis, data reporting, and 2) assisting 

the drinking water industry in identifying qualified laboratories which can accurately and reliably 

perform the analyses required by UCMR 3. 

The laboratory approval process described in this document ensures that analytical data 

generated for the UCMR are of adequate quality. EPA used a similar laboratory approval 

approach in UCMR 1 and UCMR 2 and believes this process is adequate and generates quality

data. A description of the consequent Laboratory Approval Program (LAP) and its requirements 

for UCMR 3 are presented in this UCMR 3 Lab Approval Manual, including: 
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• a description of the UCMR 3 laboratory approval process; 

• the required quality assurance (QA) documentation that must be prepared and followed at 

EPA-approved UCMR 3 laboratories;

• a summary of the UCMR 3 chemical contaminant analytical methods, minimum reporting 

levels (MRLs), and initial demonstration of capability (IDC) requirements; and

• laboratory data quality control (QC) requirements for UCMR 3 analyses. 

Laboratories must follow the procedures outlined in this document to obtain approval for the 

analysis of UCMR 3 samples.
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Section 2. UCMR 3 Laboratory Approval Process

Laboratories analyzing samples for UCMR 3 chemical contaminants must follow the process

outlined in this section to obtain approval. Approval is by method and individual laboratory.

A laboratory may apply for approval for any number of UCMR 3 methods. If a laboratory 

organization has multiple locations, each laboratory must complete the process independently. 

2.1 Registration for the UCMR 3 Laboratory Approval Program

Laboratories interested in UCMR 3 laboratory approval should contact EPA as soon as possible. 

Laboratories can request UCMR 3 registration information now, but no later than 90 days after 

publication of the UCMR 3 final rule. EPA anticipates the final UCMR 3 will be published in 

early 2012. Laboratories should send a letter of interest with contact information, including an email address, to the following address: 

UCMR Laboratory Approval Coordinator 

U.S. Environmental Protection Agency 

Technical Support Center 

26 West Martin Luther King Drive (MS 140) 

Cincinnati, OH 45268 

or to the e-mail address: UCMR_Sampling_Coordinator@epa.gov

Upon receipt of correspondence from a laboratory indicating their interest in participating in the 

UCMR 3 LAP, EPA will e-mail UCMR 3 registration information to the laboratory. 

The laboratory must complete the UCMR 3 registration sheet, indicating the UCMR 3 chemistry

methods for which they are seeking approval, and return it to EPA at the above e-mail address. 

Laboratories will be asked to provide their EPA Lab ID code on the registration sheet. If a 

laboratory does not have an EPA Lab ID code, one will be assigned. Registration information

must be received by EPA no later than 100 days after publication of the UCMR 3 final rule.

2.2 UCMR 3 LAP Applications 

EPA will forward the appropriate application packet to the laboratory based on the information 

provided on the registration sheet. The application packet will include a general application, and 

a method-specific application for each method selected on the registration sheet. 

To complete these applications, laboratories are required to: 

• Document drinking water certification by a state or regional Certification Authority for the 

analysis of samples using gas chromatography, liquid chromatography, ion 

chromatography, and/or inductively coupled plasma mass spectrometry methods. 

• Provide personnel and QA information, including a copy of the Table of Contents from the 

laboratory’s Quality Management Plan (QMP; see Section 3.1). 
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• Provide information regarding analytical equipment and sample handling procedures. 

• For each method for which the laboratory is seeking approval, submit data from: 1) an IDC 

study (see Section 5); 2) analysis of laboratory reagent blank (LRB) samples (see Section 

7.5); and 3) analysis of a set of laboratory fortified sample matrix (LFSM), LFSM duplicate 

(LFSMD), and the corresponding unfortified drinking water sample (see Section 7.7). Data 

submitted must include labeled chromatographic and/or spectrometric traces, quantitation 

reports, surrogate recovery results and internal standard recovery results. 

• Document that they are willing to post UCMR 3 results to the EPA’s electronic data 

reporting system, the Safe Drinking Water Accession and Review System (SDWARS). 

Laboratories must report field sample results and associated QC data, as required by 

SDWARS, within the proposed 60 days from the sample collection date. Failure to post 

data to SDWARS may result in EPA revoking the laboratory’s approval status. Once 

approval is revoked, the laboratory cannot be reapproved during the UCMR 3 monitoring 

period. 

 

Completed applications should be returned as soon as possible. EPA will acknowledge receipt of 

application materials in correspondence to the laboratory. 

EPA will review the submitted application materials. If all requested information is present and 

acceptable, EPA will notify the laboratory that they are eligible to participate in a UCMR 3

proficiency testing (PT) study. If deficiencies are identified in the application materials, EPA 

will identify the area(s) of deficiency and necessary corrective actions in a report to the 

laboratory. Laboratories who receive a deficiency report will have the opportunity to make 

corrective actions and submit new application information. EPA anticipates the UCMR 3 LAP 

application period will close in May 2012. 

2.3 UCMR 3 Proficiency Testing 

EPA anticipates conducting up to three PT studies prior to, and a minimum of one PT study 

after, publication of the UCMR 3 final rule. Upon successful completion of the application 

process, each laboratory must pass one PT study for each method for which they are seeking 

approval. When the laboratory’s application for a specific method is reviewed and determined to 

meet the UCMR 3 method criteria, that laboratory can participate in EPA’s UCMR 3 PT study 

for that method. Participation in a PT study is method-specific; i.e., a laboratory is not required 

to concurrently participate in a PT study for all methods for which they are seeking approval. 

EPA will send a method-specific PT ampule to laboratories, with instructions and a cover letter 

specifying a due date for reporting results to EPA. The laboratory will always have a minimum 

of two weeks to perform the analysis. Laboratories should not assume that all UCMR 3 analytes 

for a method will be present in a PT ampule for that method. Laboratories that do not pass the PT 

study for a given method can participate in the next PT study for that method, if one is 

scheduled. However, laboratories that have passed a PT study for a given method will not 

receive additional PT samples for that method during subsequent UCMR 3 PT studies. 

Upon successful participation in a PT study for a specific method, the laboratory will be notified 

in writing that it has met the initial approval criteria for each method. 
Page 13 of 41

Laboratories that pass a PT study prior to publication of the UCMR 3 final rule will be granted 

“Pending Approval” for UCMR 3. Final approval may be contingent upon: 1) changes applied to 

the final rule as a result of public comments to the proposed rule, and 2) resolution of any 

findings resulting in a laboratory audit. Laboratories are not authorized to analyze UCMR 3

monitoring samples until they receive formal “Final Approval” in writing from EPA. EPA will 

not accept analytical results for UCMR 3 samples collected prior to the monitoring date specified 

in the final UCMR 3. 
Page 14 of 41

Section 3. Laboratory Quality Management Plan and UCMR 3

Quality Assurance Project Plan

A QMP is a document that describes the general practices of an organization or program. The 

QMP may be viewed as the "umbrella" document under which individual projects are conducted. 

A Quality Assurance Project Plan (QAPP) documents details specific to an individual project 

within the organization or program. 

3.1 Laboratory Quality Management Plan

Laboratories analyzing samples for UCMR 3 are required to adhere to defined QA/QC 

procedures. This ensures that analytical data generated for UCMR 3 are scientifically valid and 

are of known and acceptable precision and accuracy. Each laboratory must have a written 

description of its QA activities detailed in a QMP, which describes the QA management of dayto-day routine operations. A QMP documents how an organization will plan, implement, and 

assess the effectiveness of its QA and QC operations. Specifically, it describes how an 

organization structures their quality system, including: quality policies and procedures; areas of 

application; and roles, responsibilities, and authorities. The QMP must be kept current during the 

time the laboratory is performing UCMR 3 measurements. Laboratories are required to submit a 

copy of the Table of Contents from their QMP to EPA as part of the UCMR 3 LAP (see Section 

2.2). 

Certain sections of the laboratory QMP can reference existing documented procedures, such as 

the laboratory's standard operating procedures (SOPs), EPA analytical methods, or other 

literature (e.g., Standard Methods for the Examination of Water and Wastewater). More 

information regarding laboratory QMPs can be found in EPA Requirements for Quality 

Management Plans (QA/R-2, see Section 8 References).

At a minimum, the laboratory’s QMP should address the following topics: 

1) Laboratory organization and responsibility 

• The laboratory’s organizational chart showing lines of authority, including QA Managers 

• A list of key individuals responsible for producing valid measurements and conducting 

routine assessments of QC procedures and measurements

• Identification of the person(s) responsible for internal audits/reviews of the implementation 

of the QMP and its requirements 

• A description of laboratory training to keep personnel current on regulations, methods, etc. 

2) Field sampling

• Personnel responsible for collecting samples 

• Procedures for sample collection, preservation, containment, holding times, and transport 

to the laboratory 
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3) Laboratory sample handling procedures

• Procedures for sample receipt, including criteria for the rejection of samples that do not 

meet shipping, holding time and/or preservation requirements 

• Bench sheets used upon sample receipt, during extraction/digestion of samples, and during 

analysis of samples, extracts or digestates

• Storage requirements for samples, extracts, and digestates, including criteria for 

temperature and holding times

• Sample tracking used to maintain the integrity of all samples from receipt by the laboratory 

through analysis and reporting to disposal 

4) Chemical, reagent and standard control procedures

• Procedures for preparation, labeling, documentation and storage of reagents, chemicals, 

calibration standards, surrogate standards, internal standards, etc.

• Frequency of initial calibration, continuing calibration checks (CCCs), and validation of 

calibrations

5) Analytical procedures

• Reference methods and corresponding SOP numbers/names used for each type of analysis. 

• Location of SOPs

• Frequency of SOP review

• Analytical instrument identification/labeling

• Identification of which analytical instruments are used for each type of analysis 

6) Data reduction, verification, validation and reporting 

• Process for converting raw data to reportable concentrations 

• Process for ensuring the accuracy of data transcription and calculations 

• Process for validatinJGDWD.data

• Process and format forUHSRUWLQJUHVXOWVWRFOLHQWV .reporting results to clients

• Procedure used for data corrections 

7) QC Procedures

• Types and frequency of QC sample analysis

• MRL verification procedures, criteria and frequency

• Use and criteria for internal and surrogate standards 

• Procedures for IDCs, and preparation of control charts
Page 16 of 41

8) Preventive maintenance

• Equipment manual location and availability 

• Spare parts inventory 

• Schedule and procedures for, and documentation of, preventative maintenance

9) Corrective action

• Response to obtaining unacceptable results from the analysis of PT samples or internal QC 

checks

• Identification of the person(s) responsible for determining that corrective action is 

necessary, and ensuring that it is completed

• Procedure for documenting actions taken and their effectiveness

10) Record Keeping

• Procedure for maintaining records, including duration and location 

• Procedure for backing-up databases/electronic files

The laboratory QMP should be concise but responsive to the above-listed items. The QMP 

maintains and improves data dependability and quality. 

3.2 UCMR 3 Quality Assurance Project Plan

All laboratories seeking approval to perform chemical analyses for UCMR 3 are required to 

prepare a QAPP specific to UCMR 3. The UCMR 3 QAPP supplements the laboratory QMP by 

documenting the specific changes in sample handling, analytical methods, QC, and data 

reporting that the laboratory makes to address the UCMR 3 requirements. Laboratories must 

make this document available to EPA for review, if requested. 

More information regarding the preparation of a QAPP can be found in EPA Requirements for 

Quality Assurance Project Plans (QA/R-5, see Section 8 References).
Page 17 of 41

Section 4. Approved Methods for UCMR 3 Monitoring

Laboratories must use the methods specified in CFR §141.40(a)(3) Table 1 to perform UCMR 

analyses during the 3-year monitoring period. The proposed UCMR 3 methods are summarized 

below and listed in Table 1. UCMR 3 laboratories must follow all analytical and QC procedures 

outlined in the methods and in this document (see Section 7). Analyses may be conducted only 

by laboratories formally approved by EPA for UCMR 3. Sampling and analysis for UCMR 3

shall not begin prior to the monitoring date specified in the final rule. 

EPA Method 200.8 Rev. 5.4, ASTM Method D5673-10, or SM 3125 

Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma – Mass 

Spectrometry 

Total recoverable analytes in a 100 milliliter (mL) water sample are solubilized by gentle heating 

(i.e., digestion) with nitric acid (do not use hydrochloric acid) on a hot plate (or hot block) that 

is set no higher than 85°C. (Note: For UCMR 3, all samples must be digested, regardless of 

sample turbidity and method.) When the sample volume has been evaporated to approximately 

20 mL (this should take about two hours), it is refluxed for an additional 30 minutes and then 

removed from heat and allowed to cool. The cooled sample is quantitatively transferred to a 50 

mL Class A glass flask or cylinder. An aliquot of a solution containing internal standards 

bismuth (Bi), indium (In), scandium (Sc), and terbium (Tb) is added and the solution is diluted to 

volume. The sample is then introduced by pneumatic nebulization into an argon-based, hightemperature radiofrequency plasma where energy transfer processes cause desolvation, 

atomization and ionization. The ions are extracted from the plasma through a differentially 

pumped vacuum interface and separated on the basis of their mass-to-charge ratio (m/z) by a 

quadrupole mass spectrometer. The ions are then detected by an electron multiplier or Faraday 

detector, and the ion information is processed by a computer-based data handling system. See 

Appendix A of this manual for important details regarding specific UCMR 3 analytical 

requirements. 

 

EPA Method 300.1, ASTM Method D6581-08, or SM 4110D 

Determination of Inorganic Anions in Drinking Water by Ion Chromatography 

A 10mL aliquot of sample is fortified with the surrogate standard dichloroacetate (DCA) and 

filtered through a 0.45 micron particulate filter using a syringe filtration apparatus. Fifty 

microliters (μL) of the filtrate is injected into an ion chromatograph fitted with: an anionexchange guard column, an anion-exchange analytical column, a background conductivity 

suppressor device, a conductivity cell detector and a data acquisition system. The anions in the 

sample are separated on the basis of their relative affinities for the low-capacity, strongly basic 

anion exchange columns. The separated anions are directed through the suppressor device where 

they are converted to their highly conductive acid forms, while the conductivity of the eluent is 

greatly decreased. The acid forms of the anions are measured by conductivity and identified on 

the basis of retention time as compared to calibration standards analyzed under identical 
Page 18 of 41

conditions. The concentration of each analyte in the sample is calculated by comparing the area 

of its peak to a standard curve developed from the analysis of the calibration standards. 

EPA Method 522

Determination of 1,4-Dioxane by Solid Phase Extraction (SPE) and Gas Chromatography/Mass 

Spectrometry (GC/MS) with Selected Ion Monitoring (SIM) 

A water sample is spiked with the isotopically labeled surrogate standard 1,4-dioxane-d8. The 

sample is extracted using one of two SPE options. In option 1, a 500 mL sample is passed 

through a method-specific, pre-packed cartridge composed of a 6 mL polypropylene tube 

containing 2 grams of coconut charcoal. These cartdridges are commercially available from 

Restek Corp. or United Chemical Technologies Inc. but equivalent brands with a particle size of 

80-120 mesh (approximately 150 μm) meeting all QC criteria in the method may be used. In 

option 2, a 100mL sample is extracted on a Waters AC-2 Sep-Pak or Supelco ENVI-Carb Plus 

cartridge or equivalent. In both options, the analytes are eluted from the solid phase with 

dichloromethane, and the extract is concentrated and fortified with the internal standard 

tetrahydrofuran-d8 (THF-d8). The final extract is dried with anhydrous sodium sulfate and 

injected using splitless injection onto a high-resolution fused silica capillary gas chromatography

column interfaced to a mass spectrometer operated in the SIM mode. Sample extract components 

are separated by the column and identified by comparing the acquired mass spectra and retention 

times to reference spectra and retention times for calibration standards acquired under identical 

GC/MS conditions. Analyte and surrogate standard concentrations are calculated using the multipoint calibration curve established in the method. 

EPA Method 524.3 

Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas 

Chromatography/Mass Spectrometry 

A 5 mL aliquot of sample is transferred to a glass sparging vessel along with internal standards 

1,4-difluorobenzene, chlorobenzene-d5, and 1,4-dichlorobenzene-d4 and surrogate standards

methyl-t-butyl-ether-d3, 4-bromofluorobenzene (BFB), and 1,2-dichlorobenzene-d4. Volatile 

organic contaminants (VOCs) are purged from the water using helium, and trapped on sorbent 

material. After drying, the trap is heated and backflushed with helium to transfer the VOCs 

directly into the gas chromatograph inlet. From the inlet, operated in split mode, analytes are 

transferred onto the capillary GC column where they are separated using a gas chromatograph

operated in temperature programming mode. Analytes eluting from the GC column are directed 

into a mass spectrometer for detection and quantitation. The method analytes are identified by 

comparing the acquired mass spectra and retention times to reference spectra and retention times 

for calibration standards acquired under identical GC/MS conditions. The concentration of each 

analyte is calculated using the internal standard technique and response curves obtained using 

procedural calibration. 
Page 19 of 41

EPA Method 537 

Determination of Selected Perfluorinated Alkyl Acids in Drinking Water by Solid Phase 

Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS) 

A 250 mL water sample is fortified with surrogates perfluoro-n-[1,2-13C2]hexanoic acid 

(

13C-PFHxA), perfluoro-n-[1,2-13C2]decanoic acid (13C-PFDA), and N-deuterioethylperfluoro-1-

octanesulfonamidoacetic acid (d5-NEtFOSAA). Method analytes and surrogates are extracted by 

passing the sample through an SPE cartridge containing polystyrenedivinylbenzene (SDVB). 

The analytes are eluted from the solid phase with a small volume of methanol. The extract is 

concentrated to dryness with nitrogen in a heated water bath. Internal standards perfluoro-[1,2-

13C2]octanoic acid (13C-PFOA), sodium perfluoro-1-[1,2,3,4-13C4]octanesulfonate (13C-PFOS), 

and N-deuteriomethylperfluoro-1-octanesulfonamidoacetic acid (d3-NMeFOSAA) are added, 

and the extract is adjusted to a 1mL volume with 96:4% (v:v) methanol:water. The analytes are 

chromatographically separated by injecting a 10μL aliquot onto a C18 column in a liquid 

chromatograph system that is interfaced to tandem mass spectrometers. After elution from the 

column, method analytes are identified by comparing the acquired mass spectra and retention 

times to reference spectra and retention times for calibration standards acquired under identical 

LC/MS/MS conditions. The concentration of each analyte is calculated using the internal 

standard technique.

EPA Method 539 

Determination of Hormones in Drinking Water by Solid Phase Extraction (SPE) and Liquid 

Chromatography Electrospray Ionization Tandem Mass Spectrometry (LC-ESI-MS/MS)

A 1 liter (L) water sample is fortified with surrogate standards ethynylestradiol-d4 and bisphenol 

A-d16. Method analytes and surrogates are extracted by passing the sample through an SPE 

cartridge containing C18 functional groups. The analytes are eluted from the solid phase with a 

small volume of methanol. The extract is concentrated to dryness with nitrogen in a heated water 

bath. A solution containing internal standards 16α-hydroxyestradiol-d2 (Estriol-d2), 13C6-

Estradiol, 13C2-ethynylestradiol, and testosterone-d3 is added, and the extract is adjusted to a 1mL 

volume with 50:50% (v:v) methanol:water. The analytes are chromatographically separated by 

injecting an aliquot onto a C18 column in a liquid chromatography system that is interfaced to 

tandem mass spectrometers. After elution from the column, method analytes are identified by 

comparing the acquired mass spectra and retention times to reference spectra and retention times 

for calibration standards acquired under identical LC-ESI-MS/MS conditions. The concentration 

of each analyte is calculated using the internal standard technique. 
Page 20 of 41

Table 1. UCMR 3 List 1 Assessment Monitoring Chemical Analytes and Methods

1-Analytical 

Method 2-Contaminant

3-CAS Registry 

Number

Quant Ions 

Parent/Daughter

(m/z)

5-MRL

(μg/L)

EPA 200.8, 

STM D5673-10, or 

SM 3125 

Trace Element 

Metals by ICP/MS*

cobalt (Co) 7440-48-4 59 1.0 

molybdenum (Mo) 7439-98-7 98 1.0 

strontium (Sr) 7440-24-6 88 0.3 

vanadium (V) 7440-62-2 51 0.2 

EPA 300.1, 

STM D6581-08, or 

SM 4110D 

Inorganic anions by 

IC

chlorate 14866-68-3 Not applicable 

(NA) 20 

EPA 522 

1,4-Dioxane by 

GC/MS

1,4-dioxane 123-91-1 88 0.07 

EPA 524.3 

VOCs by GC/MS

1,1-dichloroethane 75-34-3 63 0.03 

1,2,3-trichloropropane 96-18-4 110 0.03 

1,3-butadiene 106-99-0 54 0.1 

bromochloromethane 

(halon 1011) 74-97-5 128 0.06 

chlorodifluoromethane 

(HCFC-22) 75-45-6 51 0.08 

chloromethane 74-87-3 50 0.2 

bromomethane 74-83-9 94 0.2 

n-propylbenzene 103-65-1 91 0.03 

sec-butylbenzene 135-98-8 105 0.04 

4-Suggested 

A

A
Page 21 of 41

Table 1. UCMR 3 List 1 Assessment Monitoring Chemical Analytes and Methods

1-Analytical 

Method 2-Contaminant

3-CAS Registry 

Number

4-Suggested 

Quant Ions 

Parent/Daughter

(m/z)

5-MRL

(μg/L)

EPA 537 

Perfluorinated 

compounds by 

LC/MS/MS

perfluorooctanesulfonic 

acid (PFOS) 1763-23-1 499/80 0.04 

perfluorooctanoic acid 

(PFOA) 335-67-1 413/369 0.02 

perfluorohexanesulfonic 

acid (PFHxS) 355-46-4 399/80 0.03 

perfluoroheptanoic acid 

(PFHpA) 375-85-9 363/319 0.01 

perfluorononanoic acid 

(PFNA) 375-95-1 463/419 0.02 

perfluorobutanesulfonic 

acid (PFBS) 375-73-5 299/80 0.09 

EPA 539 

Hormones by 

LC/MS/MS

17α-ethynylestradiol 57-63-6 295.1/144.7 0.0009 

17β-estradiol 50-28-2 271.2/144.7 0.0004 

equilin 474-86-2 267.1/142.7 0.004 

estriol 50-27-1 287/144.7 0.0008 

estrone 53-16-7 268.9/144.7 0.002 

testosterone 58-22-0 289.1/96.8 0.0001 

4-androstene-3,17-dione 63-05-8 287.1/96.6 0.0003 

* See Appendix A of this manual for specific requirements. 

Explanation of Table 1 column headings: 

1 Analytical Method: Method number and condensed method name for methods that must be used to 

analyze samples for the applicable UCMR 3 contaminant(s). Reference information for the methods is 

listed in Section 8 References.

2 Contaminant: The name of the contaminant and abbreviation (if applicable) to be analyzed.

3 CAS Registry Number: A unique numerical identifier for the chemical, assigned by Chemical Abstract 

Service (CAS), a division of the American Chemical Society.

4 Suggested Quant Ions: Acceptable mass to charge ion ratio to be used for the quantitation of the analyte, 

for methods using MS. For MS/MS methods, the precursor/product ions are listed. For the metals methods 

(EPA 200.8, ASTM D5673-10, SM 3125), all listed isotopes must be monitored. 

5 Minimum Reporting Level: The lowest concentration of each analyte that must be reported to EPA.
Page 22 of 41

Section 5. Initial Demonstration of a Laboratory's Ability to 

Perform UCMR 3 Analyses

Each laboratory seeking approval for UCMR 3 methods must complete an initial demonstration 

of capability study for each method. EPA recognizes that a laboratory may use multiple 

instruments and analysts to perform analysis. If more than one analyst performs UCMR 3

analyses, EPA recommends that each analyst perform an IDC study before they are allowed to 

analyze UCMR 3 samples. Similarly, an IDC study should be performed using each instrument 

that will be used to analyze UCMR 3 samples. This will ensure that each operator and each 

instrument maintains the minimum quality standards. Data from each of these tests should be 

maintained at the laboratory for EPA’s review in the event that the Agency wishes to conduct an 

audit before or during the UCMR 3 monitoring and data analysis period. 

IDC study data must be submitted as part of the laboratory approval application package. One set 

of IDC study data, representative of typical performance of the operators and instruments used 

for the applicable method, should be included in the application package for each method. The 

UCMR 3 method-specific application sheets provide the format for reporting these data. 

EPA recommends that the laboratory verify the instrument calibration and sensitivity prior to 

performing the IDC study. The calibration curve must encompass the MRL concentration.

The IDC study involves demonstration of: 1) low system background, 2) precision, 3) accuracy, 

and 4) the laboratory’s ability to achieve the MRLs, as follows: 

1. Initial Demonstration of Low System Background – Analyze an LRB to verify that 

none of the analytes of interest are found above 1⁄3 to 1⁄2 the MRL, depending on the 

method used (Table 2).

 

2. Initial Demonstration of Precision (IDP) – Analyze 4 to 7 laboratory fortified blank 

(LFB) samples, consisting of reagent water fortified at the "precision demonstration" 

concentration for each analyte of interest (i.e., 2xMRL to 5xMRL). EPA recommends 

that these samples be fortified with a solution of method analytes obtained from a source 

external to the laboratory and different from the source of the calibration standards. The 

relative standard deviation (RSD) of the resulting analytical data set must meet the 

criterion specified in Table 2. 

3. Initial Demonstration of Accuracy (IDA) – Calculate the average recovery for the data 

set generated for the IDP (see preceding paragraph) using Equation 1. The average 

recovery must meet the criterion specified in Table 2. 

%100 1 ×÷

∑=

actual

n

i

i

LFB

n

LFB

Equation 1
Page 23 of 41

4. MRL Verification - Laboratories must verify they can achieve the UCMR 3 MRL for 

each analyte according to the procedure outlined in Section 6. 

Table 2. IDC Requirements

Analytical Method

LRB 

Requirement

Acceptable 

Precision

Acceptable 

Recovery 

(Accuracy) MRL Requirement

EPA 200.8,

ASTM D5673-10, 

SM 3125 

Metals

No analyte 

>1⁄3MRL

RSD ≤ 10% 85 – 115% of true 

value 

Achieve laboratory 

MRLs at or below 

values listed in Table 1 

for each of the UCMR 

3 analytes

EPA 300.1, ASTM 

D6581-08, 

SM 4110D 

Chlorate

RSD ≤ 15% 75 - 125% of true 

value

EPA 522

1,4-Dioxane RSD < 20% 80 – 120% of true 

value

EPA 524.3

VOCs

No analyte 

>1⁄2MRL RSD ≤ 20% 80 – 120% of true value

EPA 537

Perfluorinated 

Compounds No analyte 

>1⁄3MRL

RSD < 20% 70 – 130% of true 

value

EPA 539

Hormones RSD ≤ 20% 70 – 130% of true 

value
Page 24 of 41

Section 6. Minimum Reporting Levels

The UCMR 3 analyte MRLs were statistically established by EPA using the lowest concentration 

minimum reporting levels (LCMRLs) determined by multiple laboratories according to the 

procedure detailed in Statistical Protocol for the Determination of The Single-Laboratory Lowest 

Concentration Minimum Reporting Level (LCMRL) and Validation of the Minimum Reporting 

Level (MRL). The MRLs established for the UCMR 3 analytes are presented in Table 1, and are 

considered technically feasible without placing undue burden on laboratories. All laboratories 

performing analysis for the UCMR 3 must be able to measure the analyte concentrations at these 

levels with specified accuracy and precision. (See Section 7 for the criteria.)

As part of the UCMR 3 LAP application process, laboratories must verify they can achieve the 

UCMR 3 MRLs for each analyte according to the procedure in CFR §141.40(a)(5) and outlined 

below. 

1. Fortify, process and analyze seven replicate LFBs. These LFBs must: contain all 

dechlorinating agents and preservatives specified by the method, contain each UCMR 3

analyte of interest at a concentration at or below the UCMR 3 MRL, and be processed 

through the entire method procedure (i.e., including extraction or digestion, where 

applicable). 

2. Using the results from the analysis of the 7 replicates, calculate the mean (0) and standard 

deviation (s) for these replicates. Determine the half range for the prediction interval of 

results (HRPIR) using Equation 2: 

 HRPIR ×= s963.3 Equation 2

3. Confirm that the upper and lower limits for the prediction interval of the result (PIR = 

Mean + HRPIR) meet the upper and lower recovery limits. 

The upper PIR limit must be ≤150 percent recovery:

 %150%100

TrueValue

x HRPIR ≤×

+ Equation 3

The lower PIR limit must be ≥50 percent recovery:

 %50%100

TrueValue

x HRPIR ≥× − Equation 4

The MRL is validated if both the upper and lower PIR limits meet these criteria. 

These calculations are illustrated in Example 1. 

 
Page 25 of 41

Example 1. Calculation of the PIR Limits (where the true value of the LFB concentration is 0.60μg/L) 

LFB Results (x) 0.60 0.59 0.55 0.60 0.62 0.58 0.67 

Step 1. Calculate the Mean ( )

6014.0x

7

21.4

x

n

LFB

x

n

1i

i

= =→=→

∑=

Step 2. Calculate the Standard Deviation (S)

( )

0372.0s

6

0083.0

s

1n

LFB x

s

n

1i

2

i

=→ =→ −

−

=

∑=

Step 3. Calculate the Half Range for the PIR (HRPIR)

HR s963.3 HR 0372.0963.3 HR 147.0 PIR PIR PIR =→×=→×=

Step 4. Calculate the Upper PIR Limit (PIR upper)

%100 PIR %7.75

60.0

147.06014.0 %100 PIR

TrueValue

x HR PIR upper upper

PIR

upper →× = − →× = − =

→Passes Criterion (≤ 150%)

Step 5. Calculate the Lower PIR Limit (PIR lower)

%100 PIR %7.75

60.0

147.06014.0 %100 PIR

TrueValue

x HR PIR lower lower

PIR

lower →× = − →× = − =

→ Passes Criterion ( ≥ 50%)
Page 26 of 41

Section 7. Quality Control Requirements

Laboratories applying for approval to analyze samples for UCMR 3 must use the analytical 

methods specified in Section 4 of this manual. Laboratories must follow the QC procedures 

outlined in the method(s) and in this UCMR 3 Lab Approval Manual. 

EPA’s LAP is an effort to promote the generation of consistently accurate, precise, comparable 

and representative data for UCMR 3. EPA is requiring the implementation of specific QC 

procedures, some of which may not be required by an individual UCMR 3 method. The criteria 

specified in this manual must be followed, even if they are not required by the method. However, 

this manual is not exhaustive in describing the QC procedures required for UCMR 3; methodspecific QC requirements that are not described here must also be followed. 

An extraction or digestion batch is defined as all samples prepared/extracted/digested together 

by the same person during a work day. The same lots of reagents/solvents and internal 

standard/surrogate standard/analyte fortification solutions must be used for all samples included 

in a batch. For methods that use SPE techniques, it is preferable to use the same lot of pre-tested 

SPE medium. A maximum of 20 field samples (i.e., non-QC samples) can be included in an 

extraction or digestion batch. The extraction/digestion batch must be identified with a unique and 

traceable ID code or name.

In preparing samples for analysis, each digestion or extraction batch must include the following 

QC samples, at a minimum: 

• an LRB, 

• an LFB spiked at a concentration less than or equal to the MRL (LFB≤MRL), 

• and a LFSM/LFSMD pair spiked at a low or mid-level concentration (rotating 

concentrations from batch to batch) 

Results from the analysis of these QC samples are used to evaluate the validity of the sample 

processing procedures and techniques. Further explanation of the UCMR 3 requirements and 

criteria for these QC samples is presented in Sections 7.5 through 7.8. 

An analytical batch is defined as a group of field samples analyzed using the same instrument 

within a 24-hour period. For UCMR 3, analytical batches cannot include more than 20 field 

samples. QC samples are not counted in determining the number of samples in the analytical 

batch. The 24-hour period begins with the analysis of the first low-level CCC standard and ends 

with the analysis of the final mid- or high-level CCC standard. The analytical batch may or may 

not be comprised of field samples that were processed together in the same extraction or 

digestion batch. Ideally, however, field samples and corresponding QC samples in the same 

extraction or digestion batch should be analyzed in the same analytical batch. Each analytical 

batch must be identified with a unique and traceable ID code or name that is different than the 

extraction or digestion batch ID used in processing the samples. Field samples with QC failures 

may be re-analyzed at the end of the analytical batch, followed by an ending CCC. However, if 
Page 27 of 41

this is not possible, the re-analysis will need to be performed in a new analytical batch with a 

different ID. 

All the UCMR 3 methods require fortification of field samples, QC samples, and calibration 

standards with surrogate and/or internal standards. The method-specific surrogate and internal 

standard requirements and criteria are summarized in Sections 7.3 and 7.4, respectively. The

surrogate and internal standards must be monitored during analysis of calibration standards 

(Section 7.1 and 7.2) as well as field and QC samples. 

Laboratory personnel involved in UCMR 3 must be very familiar with general and methodspecific procedures to: 

• prepare, label and store standards and reagents; 

• prepare samples for analysis; 

• calibrate and operate the analytical instrumentation; 

• monitor system performance; 

• troubleshoot problems; 

• maintain thorough documentation of activities; 

• and review and report data 

7.1 Initial Calibration of Analytical Instruments

Each method describes initial calibration procedures used to determine the concentrations of the 

method analytes. Some methods allow more than one option. The laboratory must select and 

follow one of the initial calibration procedures outlined in the approved method in order to meet 

the requirements of UCMR 3. For mass spectometry methods, laboratories must meet the 

method-specific mass spectrometer tuning criteria prior to performing the initial calibration

procedure. 

If allowed by the method, different types of calibration (e.g., linear regression, quadratic fit, 

response factor calculation) and different fit types (e.g., forcing the curve through the origin, 

ignoring the origin, weighting factors) may be used for different analytes within a given method. 

However, the same calibration and fit type must be used for a given analyte for all analyses that 

are based on a given initial calibration. If modifications to the calibration or fit type are made, 

the instrument must be recalibrated.

The calibration curve for each UCMR 3 method must span the expected concentration range of 

the samples being analyzed, and must include a standard with a concentration less than or equal 

to the MRL. Some methods specify the minimum number and maximum range of standard 

concentrations to use for the calibration curve, and some do not. Laboratories must use a 

minimum of five calibration standards for all UCMR 3 methods. More than five standards 

must be used if specified by the method, such as EPA Method 524.3. 

The recovery of UCMR 3 analytes, surrogate standards and internal standards must be monitored 

in the initial calibration standards using the calibration curve created from the initial calibration

data. Recoveries must meet the criteria defined in Table 3. If any surrogate or internal standard 
Page 28 of 41

fails the criterion in a calibration standard, the data from that standard cannot be used in 

calculating the calibration curve. If all surrogate and internal standards pass the criteria, and a 

subset (but not all) of the analytes pass the recovery criterion, only the data for the passing 

analytes may be used in calculating the calibration curve. Standards with failed recoveries must 

be reanalyzed (and possibly re-prepared) until passing data are generated. 

Table 3. Initial Calibration Acceptance Criteriaa

Analytical Method Internal Standard Response

Analytes 

>MRL

Analytes 

≤MRL

Surrogate 

Standard

EPA 200.8, 

ASTM D5673-10, 

SM 3125 

Metals

90 – 110% 85 – 115% NA 60 – 125% of the response in the 

calibration blank 

EPA 300.1, ASTM 

D6581-08, 

SM 4110D 

Chlorate

85 – 115%b

 75 – 125%c 90 – 115% NA

EPA 522

1,4-Dioxane 80 – 120%d

 60 – 140%e

70 – 130% 

70 – 130% of the response in the 

most recent previous CCCf

EPA 524.3 

VOCs

70 – 130% 50 – 150% 

EPA 537

Perfluorinated 

Compounds

 70 – 140% of the response in the 

most recent previous CCCf

EPA 539

Hormones

70 – 130% of the response in the 

most recent previous CCCf

a

For methods 522, 524.3, 537, and 539 calibration standard responses must be entered into the calibration curve 

equation and the resultant calculated analyte concentrations must meet the accuracy criteria listed in the table

b Applies to all chlorate methods when the true concentration of the analytes is >10xMRL. c Applies to all chlorate methods when the true concentration of the analyte is ≤10xMRL. d Applies to all Method 522 Initial calibration standards except the lowest concentration. e Applies only to the lowest Initial calibration concentration for Method 522. f If there is no previous CCC, the responses for an internal standard in all the initial calibration standards must 

Recovery as % of true value 

be within 20% of each other. 

All UCMR 3 methods require verification of the initial calibration with a Quality Control Sample 

(QCS) prepared from a source different than that used to prepare the initial calibration standards. 

If a second source is not available, the QCS should be prepared from a different lot of the source 

used to prepare the initial calibration standards. EPA recommends preparing the QCS at a 

concentration near the mid-point of the calibration curve. The QCS must contain internal 

standard(s) from the same source used in the initial calibration standards. The acceptance criteria 

for the QCS are the same as those for CCC standards with concentrations greater than the MRL 
Page 29 of 41

(see Section 7.2), with the exception of the metals methods for which the criterion is ±10%. The 

initial calibration must be verified with a QCS each time a new analyte primary dilution standard 

is prepared, and at least quarterly. 

Laboratories must adhere to the holding time limitations for standard solutions, as well as other 

reagents and solutions, as specified in the individual methods. Expiration dates for prepared 

solutions cannot extend beyond the expiration date for the stock solution(s) from which they 

were prepared. If multiple stock solutions are used, the shortest expiration date applies. It is 

critical that laboratories closely monitor the expiration of calibration standards. 

7.2 Continuing Calibration Checks

Once established, the calibration curve for a method must be verified each day that analysis is 

conducted. For all UCMR 3 methods, the initial calibration must be verified with a low-level 

(i.e., concentration ≤ MRL) CCC standard prior to the analysis of field (i.e., non-QC) 

samples. Even if the calibration curve is established on the day of analysis by analyzing the 

entire suite of initial calibration standards, laboratories must analyze a low-level CCC standard 

prior to field samples. The initial calibration must also be verified throughout each day by 

analyzing a CCC standard after every tenth field sample, and at the end of the analytical 

batch, alternating between the mid- and high-level concentrations on the calibration curve.

CCC standards must meet the criteria defined in Table 4. The low-level CCC standard must meet 

method criteria before any samples are analyzed, and all samples must be bracketed by CCC 

standards that pass method criteria. Analytical results for a group of up to 10 samples are 

considered valid only if the CCC standards analyzed before and after the group meet the criteria.

If criteria are not met for a CCC standard, then the source of the problem must be identified and 

eliminated. This may require instrument maintenance and the generation of a new instrument 

calibration curve according to the method initial calibration procedures. All samples or extracts 

analyzed between the failing CCC standard and the last acceptable CCC standard must be 

reanalyzed for the failing analyte(s) after the problem is resolved. If the samples or extracts 

cannot be reanalyzed, then data for the problem analyte(s) are considered invalid for those 

samples and the data must not be reported. Laboratories reporting invalid data will be subject 

to revocation of UCMR 3 laboratory approval status.
Page 30 of 41

Table 4. CCC Acceptance Criteria

Analytical Method

Recovery as % of true value

Internal Standard Response

Mid and 

High Level 

CCC

(Analytes 

>MRL)

Low Level 

CCC

(Analytes

≤MRL)

Surrogate 

Standard

EPA 200.8, 

ASTM D5673-10, 

SM 3125 

Metals

85 – 115% 80 – 120% NA 60 – 125% the response in the 

calibration blank 

EPA 300.1, ASTM 

D6581-08, 

SM 4110D 

Chlorate

85 – 115%a

 75 – 125%b 90 – 115% NA

EPA 522

1,4-Dioxane 

70 – 130% 50 – 150% 70 – 130% 

±30% the response in the most 

recent previous CCC and ±50% the 

average response in the initial 

calibration

EPA 524.3 

VOCs

EPA 537

Perfluorinated 

Compounds

70 - 140% the response in the most 

recent previous CCC and ±50% the 

average response in the initial 

calibration

EPA 539

Hormones

±50% the average response in the 

initial calibration

a Applies to all chlorate methods when the true concentration of the analytes is >10xMRL.

b Applies to all chlorate methods when the true concentration of the analyte is ≤10xMRL. 

7.3 Surrogate Requirements and Criteria

Surrogate analyte(s) are required for all UCMR 3 methods, with the exception of the metals 

methods. A surrogate is a pure analyte that is very unlikely to be found in any sample. It is added 

to the aqueous sample in a known amount before the sample is processed, and is measured with 

the same procedures used to measure other sample components. The purpose of a surrogate 

analyte is to monitor method performance for each sample, from processing through analysis. 

Surrogate recovery must be monitored for each field sample, standard and QC sample. 

Therefore, surrogate analyte(s) must be added to all aqueous samples including LRBs, LFBs, 

LFSMs and LSFMDs, and to all standards. During IDC studies, such as demonstrations of 

accuracy and precision and MRL verifications (see Section 5), the surrogate standard recovery 

must pass the acceptance criteria.

The method-recommended surrogate analytes are listed in Table 5, along with recommended 

concentrations and the analytical acceptance criteria. When the method provides flexibility in the 
Page 31 of 41

selection of the surrogate or its concentration, EPA allows the same flexibility for UCMR 3. 

However, the concentration of each surrogate analyte must be the same in field and QC samples, 

or their extracts/digestates (whichever is introduced into the analytical instrument), as it is in the 

calibration standards. 

Table 5. Surrogate Standards, Concentrations and Criteria

Analytical Method Recommended Surrogate Standard 

Recommended 

Concentration in 

Sample

Criteria

(% recovery of 

true value)

EPA 200.8, 

ASTM D5673-10, 

SM 3125 

Metals

NA

EPA 300.1, ASTM 

D6581-08, 

SM 4110D 

Chlorate

0.5 mg/mL DCAa 1 mg/L 90 – 115%

EPA 522

1,4-Dioxane 

200 μg/mL or 

2000 μg/mL 1,4-Dioxane-d8

10 μg/L

70 – 130% 

EPA 524.3 

VOCs

1000 – 2500 μg/mL 

Methyl-t-butyl-ether-d3, BFB, & 

1,2-Dichlorobenzene-d4 

At the mid-level of 

the initial 

calibration for 

analytesb

EPA 537

Perfluorinated 

Compounds

1 – 4 ng/μL 

13C-PFHxA, 13C-PFDA, 

& d5-NEtFOSAA

40 – 160 ng/L

EPA 539

Hormones

7.0 μg/mL Ethynylestradiol-d4 70 ng/L

2.5 μg/mL Bisphenol A-d16 25 ng/L

a A surrogate standard must be used, regardless of which method is selected. An alternate to DCA may be used, 

provided it is an analyte not present in drinking water at concentrations greater than 5% of the fortified level. 

b For example, 5μg/L if using full scan mode and 0.5μg/L if using SIM mode.

Acceptance 

The percent recovery of the surrogate in a sample is calculated by comparing the analytically 

measured concentration to the fortified concentration, as in Equation 5: 

 

 

Surrogate % Recovery = Measured [surrogate] X 100% Equation 5

 Expected [surrogate] 

If the surrogate in a specific sample does not meet the acceptance criteria, then the laboratory 

should process a new aliquot of the sample. If this is not possible, then the data for that sample 

are considered suspect for the analysis in question, and should be flagged as not meeting QC 

criteria. Data for samples with failed surrogate standard recovery must not be reported. If 
Page 32 of 41

possible, the laboratory should process a new aliquot of the sample. 

If the surrogate recovery in an LRB or LFB fail the acceptance criteria, all data for other samples 

in the extraction or in the analytical batch for methods that require the direct analysis of samples 

(i.e., the chlorate methods and EPA 524.3), are invalid and must not be reported. If possible, the 

laboratory should process new aliquots of the affected samples. 

If the surrogate recovery in an LFSM or LFSMD fail the acceptance criteria, but all other batch 

QC pass, only the fortified matrix sample with the failed surrogate is impacted and cannot be 

reported. If the LFSM fails, the LFSMD data should be substituted for the LFSM such that 

accuracy can be assessed. If both LFSM and LFSMD fail, no matrix spike data should be 

reported. 

7.4 Internal Standard Requirements and Criteria

Internal standards are required for calibration and quantitation purposes in all UCMR 3 methods, 

with the exception of the chlorate methods. An internal standard is a pure analyte that is added to 

a sample or sample extract/digestate in a known amount. It is used to measure the relative 

responses of other method analytes and surrogate standards that are components of the same 

solution. The internal standard must be an analyte that is not a sample component. When used, 

the internal standard is added to all samples, standards, and QC samples or their 

extracts/digestates. During IDC studies, such as demonstrations of accuracy and precision and 

MRL verifications (see Section 5), the internal standard recovery must pass the acceptance 

criteria.

 

For UCMR 3 analysis, EPA is requiring the use of the method specific internal standards to 

ensure the comparability of results amongst laboratories. Table 6 lists the internal standards, 

along with recommended concentrations and the analytical acceptance criteria. When the method 

provides flexibility in the concentration of the internal standard, EPA allows the same flexibility 

for UCMR 3. However, the concentration of each internal standard must be the same in field and 

QC samples, or their extracts/digestates (whichever is introduced into the analytical instrument), 

as it is in the calibration standards.
Page 33 of 41

Table 6. Internal Standards, Concentrations and Criteria

Analytical Method Internal Standard 

Recommended 

Concentration Acceptance Criteria

EPA 200.8, 

ASTM D5673-10, 

SM 3125 

Metals

Bi, In, Sc, & Tb 20 - 200μg/L 60 – 125% the response in 

the calibration blank 

EPA 300.1, 

ASTM D6581-08, 

SM 4110D 

Chlorate

NA

EPA 522

1,4-Dioxane THF-d8

500 ng/mL in final 

extract or standard ±30% the most recent 

previous CCC and ±50% 

the average area in the 

initial calibration

EPA 524.3 

VOCs

1,4-Difluorobenzene, 

Chlorobenzene-d5, 

1,4-Dichlorobenzene-d5

Mid-level*

EPA 537

Perfluorinated 

Compounds

13C-PFOA, 13C-PFOS, 

d3-NMeFOSAA

10 - 40 pg/μL in final 

extract or standard

70 - 140% the most recent 

previous CCC and ±50% 

the average area in the 

initial calibration

EPA 539

Hormones

Estriol-d2, 13C6-Estradiol, 

13C2-Ethynylestradiol, 

Testosterone-d3

5 - 20 ng/mL in the 

final extract or 

standard

±50% the average area in 

the initial calibration

* For example, 5 μg/L if using full scan mode and 0.5 μg/L if using SIM mode.

If the internal standard recovery in a sample fails the acceptance criteria, then the results for that 

sample are invalid. Data for samples with failed internal standard criteria must not be 

reported. If possible, the laboratory should process a new aliquot of the sample. 

If the internal standard recoveries in an LRB or LFB fail the acceptance criteria, all data for other 

samples in the extraction or digestion batch, or in the analytical batch for methods that require 

the direct analysis of samples, are invalid and must not be reported. If possible, the laboratory 

should process new aliquots of the affected samples. 

If the internal standard recovery in an LFSM or LFSMD fail the acceptance criteria, but all other 

batch QC pass, only the fortified matrix sample with the failed internal standard is impacted and 

cannot be reported. If the LFSM fails, the LFSMD data should be substituted for the LFSM such 

that accuracy can be assessed. If both LFSM and LFSMD fail, no matrix spike data should be 

reported. 
Page 34 of 41

7.5 Laboratory Reagent Blank 

Laboratory reagent blanks are required in each batch of field samples for all of the methods 

approved for UCMR 3 monitoring. Methods that require the extraction or digestion of samples to 

prepare them for analysis must process a minimum of one LRB with every batch of 20 or fewer 

field samples, and an LRB must be included in every analytical batch. Methods involving the 

direct analysis of samples (i.e., the chlorate methods and EPA Method 524.3) require a minimum 

of one LRB analyzed with every batch of 20 or fewer field samples. For all the methods, an LRB 

is defined as an aliquot of reagent water that is treated exactly as a sample, including exposure to 

all glassware, equipment, solvents, reagents, internal standards and surrogate standards that are 

used with the other samples in the batch. This blank determines if method analytes or other 

interferences are present in the laboratory environment, reagents or apparatus. 

 

The goal for UCMR 3 is to ensure that background contamination levels are low enough that 

they do not interfere with accurate measurement of the UCMR 3 analytes. If any of the method 

analytes are detected in the LRB at a concentration greater than the criterion specified in Table 7, 

then no further analyses should be performed until the source of the problem is identified and 

eliminated. If the source is traced to any material that was used in the preparation of a batch of 

samples, then a new aliquot of each sample should be prepared. If the samples cannot be reprocessed, then all data for the problem analyte(s) are considered invalid for all samples in the 

batch, and the data should be flagged as not meeting the QC criteria. Data for samples 

processed with an LRB that fails the criteria must not be reported. 

Contamination problems that occur during sample processing cannot be detected until the 

analysis step. If a problem is discovered, then the data for one or more analytes in all the samples 

in the extraction or digestion batch are lost unless the laboratory has a back-up aliquot of each 

sample to extract. One reason EPA has limited the extraction/digestion batch to 20 field samples 

is to minimize the number of samples that may be lost due to a contamination problem. More 

than one batch of samples may be extracted within a day; an LRB must be extracted with each 

batch. 
Page 35 of 41

Table 7. Laboratory Reagent Blank Criteria 

Analytical Method LRB Acceptance Criteria

EPA 200.8, 

ASTM D5673-10, 

SM 3125 

Metals

The measured concentration of each target analyte must be <1⁄3MRL. 

Internal standard and surrogate standard recoveries must meet the 

criteria specified in Tables 5 and 6.

EPA 300.1, 

ASTM D6581-08, 

SM 4110D 

Chlorate

EPA 522

1,4-Dioxane 

EPA 524.3 

VOCs

The measured concentration of each target analyte must be <1⁄2MRL. 

Internal standard and surrogate standard recoveries must meet the 

criteria specified in Tables 5 and 6.

EPA 537

Perfluorinated Compounds The measured concentration of each target analyte must be <1⁄3MRL. 

Internal standard and surrogate standard recoveries must meet the 

EPA 539 criteria specified in Tables 5 and 6. Hormones

7.6 Laboratory Fortified Blank 

With the exception of EPA 524.3, all other methods approved for UCMR 3 monitoring require 

the extraction and analysis of an LFB. Since EPA 524.3 utilizes procedural calibration standards, 

there is no difference between the LFB and the CCC for ONLY this method. The LFB is an 

aliquot of reagent water or other blank matrix to which known quantities of the method analytes 

are added in the laboratory. The LFB is processed exactly like a sample, including the addition of 

sample dechlorinators/preservatives. The same lot of reagents and internal standard and/or 

surrogate standard fortifying solutions must be used for all samples included in a batch. The 

results from the analysis of LFBs determine whether the methodology is functioning, and 

whether the laboratory is capable of making accurate and precise measurements. Results from 

these QC samples provide information about the entire process, from sample processing to 

analyte separation and detection. 

An LFB must be processed with each extraction or digestion batch of 20 or fewer samples, and 

an LFB must be analyzed for every 20 (or fewer) samples. For UCMR 3, laboratories are 

specifically required to analyze an LFB fortified at or below the MRL prior to analyzing 

field samples. EPA recommends laboratories also process an additional mid- or high-level LFB, 

and analyze it later in the analytical batch. The measured concentration for each UCMR 3

analyte in the LFBs must meet the criteria listed in Table 8. If the recovery for any analyte in the 

low-level LFB (≤MRL) is not within the criteria, the analyst may elect to re-run it. However, if it 

fails again, the analyst must correct the problem before analyzing field samples. If the source is 

traced to any material that was used in the preparation of the batch of samples, then another 
Page 36 of 41

aliquot of each sample must be prepared for analysis. If this is not possible, then all data for the 

problem analyte(s) are considered invalid for all samples in the batch, and should be flagged as 

not meeting the QC criteria. Data for samples processed with an LFB that fails the criteria 

must not be reported. 

Table 8. Laboratory Fortified Blank Acceptance Criteria

Analytical Method 

Recovery as % of true value 

Internal Standard Response

Mid and 

High Level 

LFB 

Analytes 

>MRL

Low Level 

LFB 

Analytes 

≤MRL

Surrogate 

Standard

EPA 200.8, 

ASTM D5673-10, 

SM 3125 

Metals

85 – 115% 80 – 120% NA 60 – 125% the response in the 

calibration blank 

EPA 300.1, 

ASTM D6581-08, 

SM 4110D 

Chlorate

85 – 115%a

 75 – 125%b 90 – 115% NA

EPA 522

1,4-Dioxane 

70 – 130% 50 – 150% 70 – 130% 

±30% the response in the most 

recent previous CCC and ±50% 

the mean area measured in the 

initial calibration

EPA 537

Perfluorinated 

Compounds

70 - 140% the response in the 

most recent previous CCC and

±50% the average area measured

in the initial calibration

EPA 539

Hormones

±50% the average response in the 

initial calibration

a Applies to all chlorate methods when the true concentration of the analytes is >10xMRL.

b Applies to all chlorate methods when the true concentration of the analyte is ≤10xMRL. 

7.7 Laboratory Fortified Sample Matrix (Spiked Sample)

An LFSM is an aliquot of an environmental sample to which known quantities of the method 

analytes are added in the laboratory. This fortified sample is analyzed exactly like a field sample, 

and its purpose is to determine whether the sample matrix contributes bias to the analytical 

results. The concentrations of the analytes in the unfortified sample matrix must be determined in 

a separate aliquot. 

A technique to evaluate laboratory precision and accuracy for a method is to determine the 

precision of replicate analytical results from the separate processing and analysis of duplicate 

volumes of a sample. However, this technique is only useful when the original sample contains 
Page 37 of 41

background concentrations of the method analytes. Since the laboratory does not know which 

samples may contain measurable concentrations of target analytes, LFSMD samples are used to 

determine the precision of the UCMR 3 monitoring data. 

During the UCMR 3 monitoring period, the samples to be fortified must be UCMR 3 samples, 

and one set of LFSM/LFSMD/unfortified field sample must be processed with each batch. The 

LFSM/LFSMD fortification concentrations must be alternated between a low and mid-level

concentration. For example, a set of 40 field samples will require preparation and analysis of two 

LFSM/LFSMD sets, one set fortified at the low-level and one at the mid-level concentration. 

The low-level LFSM/LFSMD fortification concentration must be within ±50% of 

the MRL for each contaminant (e.g., for an MRL of 1.0μg/L, fortification levels 

between 0.50μg/L and 1.5μg/L are acceptable).

The mid-level LFSM/LFSMD fortification concentration must be near the 

mid-level calibration standard for each contaminant. Where possible (i.e., when 

the laboratory has data from previously analyzed samples), the fortification 

concentration should approximate the average concentration observed in previous 

analyses.

There are no target analyte recovery acceptance criteria specified for LFSM/LFSMD results. 

Data should not be rejected based on the recovery of fortified target analytes or the 

precision between the LFSM and LFSMD, provided that the analysis of the fortified sample 

yields acceptable internal standard and surrogate standard recoveries and all other batch QC are 

valid. 

7.8 Analytical Sequence

The sequence with which UCMR 3 field and QC samples are analyzed is important for assessing 

system performance. As described in Section 7.2, each analysis batch must begin with the 

analysis of a CCC at or below the MRL for each of the UCMR 3 analytes targeted by the 

method. This CCC≤MRL should be analyzed whether or not the initial calibration was generated 

the same day. Following the CCC≤MRL, the LRB should be analyzed, then the LFB≤MRL, and 

then up to 10 field samples. After 10 field samples, the calibration must be verified by the 

analysis of a mid- or high-level CCC. If this CCC passes the criteria, then up to 10 additional 

field samples may be analyzed. The batch must end with the analysis of a mid- or high-level 

(whichever was not analyzed after the 10th sample) CCC. If a second batch is started within the 

same 24-hour period, it must begin with the analysis of a CCC≤MRL. 
Page 38 of 41

Example 2 illustrates a valid analysis sequence for Method 537 that will meet the QC 

requirements. It provides suggestions for corrective action if the criteria are not met. 

Example 2. Valid Analysis Sequence for Method 537 

Injection 

#

Sample 

Description Acceptance Criteriaa Corrective Action

1 CCC≤MRL Recovery for each target analyte is 

50-150% of the true value 

Instrument maintenance to recover 

sensitivity, followed by recalibration 

and verification of sensitivity by a low 

level CCC

2 LRB All target analytes <1⁄3MRL 

concentration

Identify and correct source of 

contamination

3 LFB≤MRLb

 50-150% of the true value for each 

target analyte

Identify and correct source of problem

4 

through

13

Field Samples 

1-10 

Positive ID of an analyte is verified 

if the peak passes the retention time 

criterion and mass spectral 

identification is confirmed.

Identify and correct source of problem 

14 Mid-level CCCc Recovery for each target analyte is 

70-130% of the true value 

Instrument maintenance, followed by 

recalibration

15 LFSM of a 

Field Sample

At low-level fortification 

concentrations, 50-150% recovery. 

At mid-level fortification 

concentrations, 70-130% recoveryd

. 

If % recovery is out of the designated 

range, but laboratory performance for all 

other QC is acceptable, the recovery 

problem is judged to be matrix related, 

but is still reportable.

16 LFSMD of 

Field Sample

RPD between LFSM and LFSMD 

≤50% for low-level fortification 

concentrations and ≤30% for midlevel fortification concentrationsd

. 

If % recovery is out of the designated 

range, but laboratory performance for all 

other QC is acceptable, the recovery 

problem is judged to be matrix related, 

but is still reportable.

17

through

28

Field Samples 

11-20 

Positive ID of an analyte is verified 

if the peak passes the retention time 

criterion and mass spectral 

identification is confirmed.

Identify and correct source of problem 

29 Final high-level 

CCCc

Recovery for each analyte is 70-

130% of the true value 

Instrument maintenance, followed by 

recalibration a In all field and QC samples, and standards for Method 537: The area for the internal standard must be 70-

140% of the area in the most recent CCC and 50-150% of the average area measured during the initial calibration. 

Surrogate recovery must be 70-130% of the true value. b Quality conscious labs may choose to include an additional LFB, at rotating concentrations, later in the analysis 

batch. The criterion for LFBs fortified at a concentration >MRL is 70-130% of the true value for each target 

analyte. 

c Subsequent to the initial CCC≤MRL, CCC concentrations should be rotated between the mid and high

concentrations. d Failing these criteria does not invalidate the analysis batch under UCMR 3. See Section 7.7 for the specifications 

for low and mid-level fortification concentrations. 
Page 39 of 41

Appendix A. Requirements for UCMR 3 Metal Analysis

Table 9 presents specific requirements for the determination of UCMR 3 metal analytes in samples. The 

requirements follow EPA Method 200.8 Revision 5.4 for Total Recoverable Analytes in Aqueous 

Samples. In the analysis of UCMR 3 samples, laboratories must adhere to these specifications regardless 

of which method (EPA 200.8, ASTM D5673-10, or SM 3125) they have certification for. The following 

exceptions to EPA Method 200.8 apply to UCMR 3: 

1) For Section 11.0, use Section 11.2.2. 

2) In Section 11.2.3, omit the use of hydrochloric acid. 

3) Omit Section 11.2.8. 

Table 9. Specifics for the Determination of Metals for UCMR 3

Analyte 

Natural 

Isotopesa

% Relative 

Abundance

Additional 

Isotopes to 

Monitor 

Isotope to 

Report

Required Elemental & Molecular 

Equations

Co 59 100 --- 59 (1.000) (59C)

Mo

92 

94 

95 

96 

97 

98 

100 

14.84 

9.25 

15.92 

16.68 

9.55 

24.13 

9.63 

99 98 (1.000) (98C) – (0.146) (99C)

Isobaric elemental correction for Ruthenium. 

Sr

84 

86 

87 

88 

0.56 

9.86 

7.00 

82.58 

85 88 (1.000) (88C)

V 50 

51 

0.250 

99.750 

52 

53 51 

(1.000) (51C) – (3.127) [(53C) – (0.113) (52C)]

Isobaric polyatomic correction for chloride 

and sulfate matrix molecular ions.

Bib 209 100 --- 209 (1.000) (209C)

Inb 113 

115 

4.3 

95.7 

118 

120 115 

(1.000) (115C) – (0.016) (118C)

If Tin present, use the isobaric elemental 

correction. 

Scb 45 100 --- 45 (1.000) (45C)

Background molecular ions may interfere. 

Tbb 159 100 --- 159 (1.000) (159C)

a All must be monitored

b Internal standard
Page 40 of 41

Section 8. References

ASTM Standard D5673-10. Standard Test Method for Elements in Water by Inductively Coupled 

Plasma – Mass Spectrometry. American Society for Testing and Materials (ASTM), West 

Conshohocken, PA. 2005. Available at http://www.astm.org/Standards/D5673.htm

ASTM Standard D6581-08. Standard Test Methods for Bromate, Bromide, Chlorate, and 

Chlorite in Drinking Water by Suppressed Ion Chromatography. ASTM, West Conshohocken, 

PA. 2008. Available at http://www.astm.org/Standards/D6581.htm

EPA Method 200.8. Determination of Trace Elements in Waters and Wastes by Inductively 

Coupled Plasma – Mass Spectrometry, Revision 5.4, EMMC Version. Environmental 

Monitoring Systems Laboratory, Office of Research and Development (ORD), EPA, Cincinnati, 

Ohio 45268. Available at https://www.nemi.gov/

EPA Method 300.1. Determination of Inorganic Anions in Drinking Water by Ion 

Chromatography. National Exposure Research Laboratory (NERL), ORD, EPA, Cincinnati, 

Ohio 45268. Available for download at 

http://water.epa.gov/scitech/drinkingwater/labcert/analyticalmethods_ogwdw. cfm

EPA Method 522. Determination of 1,4-Dioxane by Solid Phase Extraction (SPE) and Gas 

Chromatography/Mass Spectrometry (GC/MS) with Selected Ion Monitoring (SIM), Version 1.0, 

September, 2008. EPA/600/R-08/101. NERL, ORD, EPA, Cincinnati, Ohio 45268. Available for 

download at http:/www.epa.gov/nerlcwww/ordmeth.htm

EPA Method 524.3. Measurement of Purgeable Organic Compounds in Water by Capillary 

Column Gas Chromatography/Mass Spectrometry, Version 1.0, June 2009. EPA 815-B-09-009. 

TSC, OGWDW, EPA, Cincinnati, Ohio 45268. Available for download from 

http://water.epa.gov/scitech/drinkingwater/labcert/analyticalmethods_ogwdw.cfm

EPA Method 537. Determination of Selected Perfluorinated Alkyl Acids in Drinking Water by 

Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS), 

Version 1.1, September 2009. EPA Document #EPA/600/R-08/092. NERL, ORD, EPA, 

Cincinnati, Ohio 45268. Available for download at 

http://www.epa.gov/nerlcwww/ordmeth.htm

EPA Method 539. Determination of Hormones in Drinking Water by Solid Phase Extraction 

(SPE) and Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry (LCESI-MS/MS), Version 1.0, November 2010. EPA Document #815-B-10-001. TSC, OGWDW, 

EPA, Cincinnati, Ohio 45268. Available at 

http://water.epa.gov/scitech/drinkingwater/labcert/analyticalmethods_ogwdw.cfm

EPA QA/R-2. EPA Requirements for Quality Management Plans (QA/R-2). EPA Document 

#EPA/240/B-01/002. Office of Environmental Information (OEI), EPA, Washington, DC 20460. 

Available at http://www.epa.gov/quality/qmps.html
Page 41 of 41

EPA QA/R-5. EPA Requirements for Quality Assurance Project Plans (QA/R-5) EPA Document 

#EPA/240/B-01/003. OEI, EPA, Washington, DC 20460. Available for download from 

http://www.epa.gov/quality/qs-doc/r5-final.pdf

Statistical Protocol for the Determination of the Single-Laboratory Lowest Concentration 

Minimum Reporting Level (LCMRL) and Validation of the Minimum Reporting Level (MRL), 

November 2004. TSC, OGWDW, EPA, Cincinnati, Ohio 45268. Available for download from 

http://water.epa.gov/scitech/drinkingwater/labcert/analyticalmethods_ogwdw.cfm

SM Method 3125. Metals by Inductively Coupled Plasma/Mass Spectrometry (1997). Available 

for purchase at http://www.standardmethods.org/store/ProductView.cfm?ProductID=211

SM Method 4110D. Ion Chromatographic Determination of Oxyhalides and Bromide (2000). 

Available for purchase at http://www.standardmethods.org/store/ProductView.cfm?ProductID=31