Guide Compendium of Analytical Methods (CAM)

The guide to MassDEP's Compendium of Quality Control Requirements and Performance Standards for Selected Analytical Protocols (WSC #10-320) took effect July 1, 2010 and is periodically updated. The guide is also referred to as the "Compendium of Analytical Methods", or "CAM" for short.

Overview

The Compendium provides the regulated community with a compilation of recommended laboratory protocols, for the generation of analytical data used in support of assessment and evaluation decisions at disposal sites regulated under M.G.L.c. 21E and the Massachusetts Contingency Plan (MCP). These laboratory protocols include recommended analytical methods, reporting limit requirements, method-specific QC requirements and performance standards.

Compliance with the QC requirements and performance standards for these protocols will result in analytical data that are presumed to meet the performance standards of the MCP. Analytical data with "Presumptive Certainty" status are data for which the MassDEP stipulates the precision, accuracy, and sensitivity have been adequately determined. Depending on the nature and use of the analytical data, a separate evaluation may be necessary to confirm that the quality and representativeness of data are sufficient for its intended use in support of a response action decision. Data that achieve "Presumptive Certainty" status must still be assessed for usability and representativeness in comparison to project objectives as specified in 310 CMR 40.1056(2)(k) and further described in the MassDEP Policy #WSC-07-350, MCP Representativeness Evaluations and Data Usability Assessments.

Adherence to this approach will promote inter-laboratory consistency and provide the regulated community with a greater degree of certainty regarding the quality of data used for MCP decision-making. MassDEP's issuance of these CAM requirements and performance standards is in no way intended to preempt the exercise of professional judgment by the data user in regards to the selection of analytical methods and associated QC requirements. However, it must be clearly understood that if an alternative analytical method is chosen to support MCP decisions, the data user is responsible for independently demonstrating the accuracy, precision, sensitivity, representativeness and overall usability for all analytical data pursuant to the requirements of 310 CMR 40.0017, 40.0191(2), and 40.1056(2)(k).

It should be noted that this document does not provide any specific guidance regarding proper sampling procedures, approaches to achieve representative sampling nor the type and frequency of field QC samples required to evaluate overall data representativeness or usability.

Documents are presented in the Adobe Acrobat format, including sectional bookmarks for the protocol status, analytical method overview, quality control requirements and performance standards table, and target analyte list.

Comments and recommendations on these procedures should be directed to:
bwsc.cam@state.ma.us

Additional Resources

Effective Date

The effective date for Cleanup of Sites & Spills: WSC #10-320: Compendium of Quality Control Requirements and Performance Standards for Selected Analytical Protocols is July 1, 2010. For the purpose of meeting the requirements for "Presumptive Certainty," these protocols must be used on analyses conducted on or after July 1, 2010

Sampling, Data Evaluation and Reporting Procedures for MCP Activities

This section of the CAM (Section VII) provides the regulated community with quality assurance (QA) and quality control (QC) guidance regarding the acquisition and reporting of analytical data submitted in support of response actions conducted at disposal sites.

Additional Resources

Gas Chromatography/Mass Spectrometry (GC/MS) Methods

MassDEP has developed 2 CAM protocols for GC/MS methods:

  • WSC-CAM-IIA - Volatile Organic Compounds (VOCs), based on USEPA Method SW-846 8260B 

    and
     
  • WSC-CAM-IIB - Semivolatile Organic Compounds (SVOCs), based on USEPA Method SW-846 8270D

Additional Resources

Metals Methods

There are four CAM protocols developed for metals analysis:

  • WSC-CAM-IIIA - Trace Metals by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES),
    based on USEPA Method SW846 6010C,
     
  • WSC-CAM-IIIB - Mercury by Cold Vapor Atomic Absorption (CVAA) Spectrometry,
    based on USEPA Method SW-846 7470A & 7471B,
     
  • WSC-CAM-IIIC - Trace Metals by Graphite Furnace Atomic Absorption (GFAA) Spectrometry,
    based on USEPA Method SW-846 7010,

    and
     
  • WSC-CAM-IIID - Trace Metals by Inuctively Couple Plasma-Mass Spectrometry (ICP-MS),
    based on USEPA Method SW-846 6020A.

Additional Resources

Petroleum Hydrocarbon Methods

Mass DEP has developed three CAM protocols for analyzing petroleum hydrocarbons based on the MassDEP VPH/EPH Methods:

  • WSC-CAM-IVA - Volatile Petroleum Hydrocarbons (VPH) by GC/PID/FID,
    based on the MassDEP VPH Method  by GC/PID/FID
     
  • WSC-CAM-IVC - Volatile Petroleum Hydrocarbons (VPH) by GC/MS,
    based on the MassDEP VPH by GC/MS Method,

    and
     
  • WSC-CAM-IVB - Extractable Petroleum Hydrocarbons (EPH),
    based on the MassDEP EPH Method. 

Additional Resources

Gas Chromatography Methods

MassDEP has developed three CAM protocols for gas chromatography methods used to analyze for PCBs, chlorinated pesticides and chlorinated herbicides:

  • WSC-CAM-VA - Polychlorinated Biphenyls (PCBs),
    based on USEPA Method SW-846 8082A,
     
  • WSC-CAM-VB - Chlorinated Pesticides, 
    based on USEPA Method SW-846 8081B,

    and
     
  • WSC-CAM-VC - Chlorinated Herbicides, 
    based on USEPA Method SW-846 8151A

Additional Resources

Miscellaneous Wet Chemical methods

MassDEP has developed CAM protocols for two wet chemistry methods:

  • WSC-CAM-VIA - Total Cyanide and Physiologically Available Cyanide (PAC)
    based on USEPA Method SW-846 9014, 9012B and others

    and
     
  • WSC-CAM-VIB - Hexavalent Chromium (Cr VI) by UV-Visible Spectrophotometry
    based on USEPA Method SW-846 7196A

Additional Resources

High Performance Liquid Chromatography (HPLC) and Ion Chromatography Methods

MassDEP has prepared two CAM protocols for HPLC and ion chromatography methods:

  • WSC-CAM-VIIIA - Nitroaromatics and Nitramine by HPLC,
    based on USEPA Method SW-846 8330A,

    and
     
  • WSC-CAM-VIIIB - Perchlorate by Ion Chromotography,
    based on USEPA Methods  SW-846 331.0 / 332 and SW-846 6850 / SW-846 6860

Additional Resources

Air Sampling Methods

MassDEP has developed two CAM protocols for analyzing air samples:

  • WSC-CAM-IXA - Air-Phase Petroleum Hydrocarbons (APH) by GC/MS,
    based on the MassDEP Method for the Determination of Air-Phase Petroleum Hydrocarbons (APH)

    and
     
  • WSC-CAM-IXB - Volatile Organic Compounds (VOCs) in Air Samples (TO-15) by GC/MS

Additional Resources

Reporting Forms

MassDEP has developed a number of forms associated with using the CAM, including:

  • MassDEP Analytical Protocol Certification Form 
     
  • MCP Analytical Services Request Form  
     

Results Reporting Forms

  • VPH Analytical Results Form 
  • EPH Analytical Results Form
  • TPH Analytical Results Form 
  • Required APH Data Reporting Information 

Additional Resources

APH Method Worksheets

Both nominal concentration- and on-column-mass-based APH Analytical Method Calculation Worksheets utilizing the analytical information presented in Final Method for the Determination of Air- phase Petroleum Hydrocarbons (APH) Appendix 5, Tables 8 - 11 have been developed using a Microsoft Office Excel platform.  These worksheets are intended to be used by laboratories for individual sample calculations or to "proof" Laboratory Information Management System (LIMS) calculations for range and target analyte concentrations using the APH Method.

Nominal Concentration-Based Calculation Worksheet 

This Worksheet (link below) provides (1) an example nominal concentration based RRF calculations for APH aliphatic and aromatic ranges and the target analytes based on multi-point calibration data and (2) example calculations of sample concentrations for APH aliphatic and aromatic ranges and the target analytes based on the calculated RRFs, simulated area counts and other sample-specific data. The relevant analytical data for the target analytes are extracted from Table 6-8 of the aforementioned Appendix 5.

Note: Some minor differences in calculated values as compared to Appendix 5 may be observed due to the Microsoft Excel calculation algorithms.

On-Column Mass-Based Calculation Worksheet

This Worksheet (link below) provides (1) an example on-column-mass-based RRF calculations for APH aliphatic and aromatic ranges and the target analytes based on multi-point calibration data and (2) example calculations of sample concentrations for APH aliphatic and aromatic ranges and the target analytes based on the calculated RRFs, simulated area counts and other sample-specific data. The relevant analytical data for the target analytes are extracted from Table 6-8 of the aforementioned Appendix 5.

Note: Some minor differences in calculated values as compared to Appendix 5 may be observed due to the Microsoft Excel calculation algorithms.

Additional Resources

USEPA SW-846 Methods

The US EPA publication SW-846, entitled Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, is the Office of Solid Waste's (OSW's) official compendium of analytical and sampling methods that have been evaluated and approved for use in complying with the RCRA regulations. SW-846 functions primarily as a guidance document setting forth acceptable, although not required, methods for the regulated and regulatory communities to use in responding to RCRA-related sampling and analysis requirements.

SW-846 is a multi-volume document that changes over time as new information and data are developed. It has been issued by EPA since 1980 and is currently in its third edition. Advances in analytical instrumentation and techniques are continually reviewed by OSW and incorporated into periodic updates to SW-846 to support changes in the regulatory program and to improve method performance and cost effectiveness. To date, EPA has finalized Updates I, II, IIA, IIB, III and IIIA to the SW-846 manual, and the updated and fully integrated manual contains approximately 3500 pages. The Methods Team of OSW has also made Draft Updates IVA and IVB for public use. 

Glossary of Quality Assurance Terminology

The analytical chemistry and environmental sampling techniques used to assess sites under the MCP use specialized vocabulary that may be unfamiliar to those reading this material for the first time. MassDEP has but together a glossary of terms to help you understand these terms.

Combined Target Analyte List

Each analytical method described above is used to evaluate a specific set of contaminants.  This combined list was developed to provide a single reference source for analytes that are commonly encountered at disposal sites with a cross-reference to the appropriate MCP Analytical Protocol(s). 

Frequently Asked Questions

The CAM Protocols: Questions & Answers provides responses to questions submitted to MassDEP on the implementation of the revised CAM Protocols, effective July 1, 2010.

Questions on the CAM protocols may be sent to BWSC.CAM@state.ma.us

Additional Resources

Double-Blind Laboratory Evaluation Program

During 2004 and 2005, the Massachusetts Department of Environmental Protection (MassDEP) conducted a large double-blind laboratory evaluation study, involving 19 commercial laboratories that provide the majority of analytical support services to parties assessing and cleaning up hazardous waste sites in Massachusetts. A "double-blind" study is one in which a laboratory is unaware that they have been sent samples that contain known concentrations of contaminants. The study was undertaken by MassDEP as part of a multi-year/multi-component data enhancement effort, in order to obtain a direct, real world sense of data quality and reliability in its waste site cleanup program.

MassDEP contracted with a well-known laboratory Proficiency Testing company to prepare test samples. To maintain the confidentiality of the study, the company set up mock consulting firms to send out samples and pay for analyses. Each laboratory was shipped a soil sample and groundwater sample spiked with measured concentrations of 5 common Volatile Organic Compounds (VOCs). This procedure was repeated on 3 different occasions -- in July, September, and November of 2004 -- at identical spiking concentrations.

In addition to these 19 commercial laboratories, double-blind samples were also delivered to the MassDEP state analytical laboratory (the Wall Experiment Station), by an agency employee, under the pretense of being samples from a confidential enforcement case.

MassDEP believes the results of this study are very encouraging. The vast majority of the laboratories evaluated were able to consistently quantify most analytes within 20% of the actual value. This excellent result is well within the most stringent acceptance criteria in use by the industry.

In a few cases, false positive or false negative results were reported, particularly with respect to vinyl chloride in water, which is known to be a problematic analyte. MassDEP is conducting further review of analytical data generated by the study to attempt to determine the reasons for these results.

Given these findings, MassDEP believes the public can have confidence in the integrity of the commercial laboratory community, and in the accuracy of the analytical data used to confirm cleanup of sites contaminated with Volatile Organic Compounds (VOCs), which are among the most pervasive and problematic pollutants at hazardous waste sites.

Additional Resources

Image credits:  (Paul Locke)

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