Process Document for Joint Verification of the
Sorbisense Ground Water Sampler
and
Sorbisense GSW40 Passive Sampler Joint Verification Protocol for
Volatile Organic Compounds in Groundwater
and
Sorbisense GWS40 Passive Sampler Joint Test Plan for
Volatile Organic Compounds in Groundwater
June 2009
Prepared by
Amy Dindal
Anne Gregg
Zachary Willenberg
Battelle Memorial Institute
505 King Avenue
Columbus, OH 43201-2693
and
Christian Gran
Gerald Heinicke
Louise Schliitter
Mette Tjener Anders son
NOWATECH/DHI
Agern Alle 5,
DK-2970
H0rsholm, Denmark
and
John McKernan
Evelyn Hartzell
Lora Johnson
Lauren Drees
U.S. Environmental Protection Agency
26 Martin Luther King Drive
Cincinnati, OH 45268
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FOREWARD
The U.S. Environmental Protection Agency (EPA), Advanced Monitoring Systems
(AMS) Center of the Environmental Technology Verification Program (ETV) collaborated with
the NOWATECH DHI Water Monitoring Center (DHIWMC), a pilot ETV program in the
European Union, to conduct an international joint verification test of a passive ground water
sampler.
This document, which is actually a compilation of three separate documents, was used by
NOWATECH and the AMS Center to jointly verify the performance of this technology. It is
composed of a process document, a verification protocol, and a test plan for joint verification.
Combined, these three documents satisfy the requirements of an EPA ETV approved verification
test/QA plan and ensure that the requirements of both programs are met.
The verification protocol and test plan were developed by NOWATECH with input from
Battelle, EPA, and other stakeholders. Together these documents satisfy NOWATECH's
programmatic requirements. The process document was developed by the AMS Center with
input from NOWATECH and the EPA. It was developed as a supplement to the NOWATECH
documents, to ensure that all of EPA ETV programmatic requirements are met. All three
documents were reviewed and approved via the ETV process prior to the start of testing.
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TABLE OF CONTENTS
Process Document:
Section Page
1 INTRODUCTION 6
2 QUALITY SYSTEMS 11
3 VERIFICATION PLANNING 11
4 VERIFICATION TEST IMPLEMENTATION 13
5 ASSESSMENT AND RESPONSE 15
6 DOCUMENTATION AND REPORTING 19
7 REFERENCES 23
Appendix A ROLES OF KEY PERSONNEL 24
Appendix B KICK OFF MEETING CHECKLIST 25
Appendix C REVIEW REPORT FORM 28
Appendix D JOINT VERIFICATION TESTING DOCUMENT AMENDMENT AND
DEVIATIONS FORMS 29
Appendix E ASSESSMENT REPORTING FORM 32
Appendix F EXAMPLE VERIFICATION STATEMENT 34
Verification Protocol:
1 TABLE OF CONTENTS II
2 INTRODUCTION 1
2.1 Name of product 1
2.2 Name and contact of vendor 1
2.3 Name of center/verification responsible 1
2.4 Verification Test Organization 1
2.5 Expert group 2
2.6 Verification process 3
3 DESCRIPTION OF THE TECHNOLOGY 3
4 DESCRIPTION OF THE PRODUCT 4
5 APPLICATION AND PERFORMANCE PARAMETER DEFINITIONS 6
5.1 Matrix/matrices 6
5.2Target(s) 6
5.3 Effects 6
5.4 Performance parameters for verification 6
5.5 Additional parameters 8
6 EXISTING DATA 8
6.1 Summary of existing data 8
6.2 Quality of existing data 9
6.3 Accepted existing data 9
7 TEST PLAN REQUIREMENTS 9
7.1 Test design 10
-------
7.2 Reference analysis 11
7.3 Data management 11
7.4 Quality assurance 11
7.5 Test report 11
8 EVALUATION 11
8.1 Calculation of performance parameters 12
8.2 Evaluation of test data quality 13
8.3 Compilation of additional parameters 13
8.3.1 User manual 13
8.3.2 Product costs 14
8.3.3 Occupational health and environment 15
9 VERIFICATION SCHEDULE 15
10 QUALITY ASSURANCE 15
APPENDIX 1 17
Terms and definitions used in the verification protocol 17
APPENDIX 2 22
References 22
APPENDIX 3 25
Application and performance parameter definitions 25
Test Plan:
1 TABLE OF CONTENTS II
2 INTRODUCTION 1
2.1 Verification protocol reference 1
2.2 Name and contact of vendor 1
2.3 Name of center/test responsible 1
2.4 Expert group 2
3 TEST DESIGN 2
3.1 Test sites 5
3.1.1 Types 5
3.1.2 Addresses 5
3.1.3 Descriptions 5
3.2 Tests 5
3.2.1 Test methods 6
3.2.2 Test staff 8
3.2.3 Test schedule 9
3.2.4 Test equipment 9
3.2.5 Type and number of samples 9
3.2.6 Operation conditions 11
3.2.7 Operation measurements 11
3.2.8 Product maintenance 11
3.2.9 Health, safety and wastes 11
4 REFERENCE ANALYSIS 12
4.1 Analytical laboratory 12
-------
4.2 Analytical parameters 12
4.3 Analytical methods 12
4.4 Analytical performance requirements 13
4.5 Preservation and storage of reference samples 13
5 DATA MANAGEMENT 13
5.1 Data storage, transfer and control 13
6 QUALITY ASSURANCE 14
6.1 Test plan review 14
6.2 Performance control - reference analysis 14
6.3 Test system control 15
6.4 Data integrity check procedures 16
6.5 Test system audits 16
6.6 Test report review 17
7 TEST REPORT 17
7.1 Test site report 17
7.2 Test data report 17
7.3 Amendment report 17
7.4 Deviations report 17
APPENDIX 1 19
Terms and definitions used in the test plan 19
APPENDIX 2 24
Reference methods and references 24
APPENDIX 3 27
In-house test methods 27
APPENDIX 4 46
In-house analytical methods 46
APPENDIX 5 48
Data reporting forms 48
APPENDIX 6 89
Data management 89
APPENDIX 7 95
Deviations and amendments 95
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EXECUTIVE SUMMARY
The Nordic Water Technology Verification Center's (NOWATECH) DHI Water
Monitoring Center (DHI WMC), a pilot Environmental Technology Verification Program (ETV)
in the European Union, and the United States Environmental Protection Agency ETV Program's
(EPA ETV) Advanced Monitoring Systems (AMS) Center are jointly verifying the Sorbisense
(vendor) GWS40 passive ground water sampler.
Under this joint effort, NOWATECH was responsible for developing the verification
protocol, preparing the test plan including quality assurance (test/QA), testing, and generating
the verification report/verification statement in accordance with their requirements. The AMS
Center provided technical and quality assurance oversight throughout the NOWATECH process
to ensure EPA ETV requirements were also met, and facilitated reviews and audits by QA
personnel, EPA Program management, and stakeholders of the verification protocol, test plan,
testing, and verification report. The AMS center also developed a process document to
supplement the protocol and test plan developed by NOWATECH and ensure that all of EPA
ETV programmatic requirements are met. The process document, combined with the protocol
and test plan, satisfy the requirements of an EPA approved verification test/QA plan. This
document is a compilation of these three documents.
The purpose of this verification is to evaluate a passive ground water sampling
technology, which is capable of detecting 10 contaminants: mono-, di-, tri- and -
tetrachloroethenes, chloroethene, benzene, toluene, ethylbenzene, xylenes (BTEX), and
methyl-fert-butylether (MTBE). Passive sampling is based upon distribution of solutes
between the sampled medium, and a collecting medium. Flow of solute from one medium
to the other continues until equilibrium is established in the system. The amount of solute in the
sampling medium is then determined analytically and can be used to calculate the concentration
in the sampled medium. This result will then be compared to results from a standard analytical
method for the contaminants of interest, providing information on the precision, accuracy, and
range of the technology being verified. Other verification parameters will include determination
of the limit of detection, and the robustness of the monitoring technology.
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Battelle Qj NOWATECH
The Business of Innovation WATER.ENVIRONMENT- HEALTH
Environmental Technology
Verification Program
Advanced Monitoring
Systems Center
Process Document for
US EPA ETV AMS CENTER
and
NOWATECH DHI WMC
Joint Verification of the
Sorbisense Ground Water Sampler
-------
Process Document for
US EPA ETV AMS CENTER
and
NOWATECH DHI WMC
Joint Verification of the
Sorbisense Ground Water Sampler
February 10,2009
Prepared by
Battelle
505 King Avenue
Columbus, OH 43201-2693
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US ETV AMS Center and NOWATECH DHIWMC
Joint Verification Process Document
Page 3 of 3 5
Date: 2/10/2009
TABLE OF CONTENTS
Section Page
1 INTRODUCTION 6
2 QUALITY SYSTEMS 11
3 VERIFICATION PLANNING 11
4 VERIFICATION TEST IMPLEMENTATION 13
5 ASSESSMENT AND RESPONSE 15
6 DOCUMENTATION AND REPORTING 19
7 REFERENCES 23
Appendix A ROLES OF KEY PERSONNEL 24
Appendix B KICK OFF MEETING CHECKLIST 25
Appendix C REVIEW REPORT FORM 28
Appendix D JOINT VERIFICATION TESTING DOCUMENT AMENDMENT AND
DEVIATIONS FORMS 29
Appendix E ASSESSMENT REPORTING FORM 32
Appendix F EXAMPLE VERIFICATION STATEMENT 34
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US ETV AMS Center and NOWATECH DHIWMC
Joint Verification Process Document
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Date: 2/10/2009
List of Figures Page
Figure 1. Organization Chart for the Joint Verification Test of Sorbisense GWS40 Passive
Ground Water Sampler 7
List of Tables
Table 1.0 Assessments for the Joint Verification 18
Table 2.0 Document and Reporting Responsibilities for the Joint Verification 22
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Joint Verification Process Document
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Date: 2/10/2009
DISTRIBUTION LIST
John McKernan
Lauren Drees
US EPA
26 West Marin Luther King Drive
Mail Code: 208
Cincinnati, OH 45268
Christian Gran
Gerald Heinicke
Louise Schliitter
DHI
Agern Alle 5,
DK-2970
H0rsholm, Denmark.
Hubert de Jonge
Vendor- Sorbi sense
Niels Pedersens Alle 2
DK-8830
Tjele, Denmark
Amy Dindal
Anne Gregg
Zachary Willenberg
Battelle
505 King Ave.
Columbus, OH 43201
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Joint Verification Process Document
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Date: 2/10/2009
section. The names of the key personnel and their roles during this verification are presented
in Appendix A.
United States
Environmental
Protection Agency,
Environmental
Technology
Verification Program
(US EPA ETV)
Battelle, US EPA
ETV Advanced
Monitoring
Systems Center
Stakeholder
Committee
Sorbisense
(Vendor of
GWS40)
Expert
Group/External
Peer
Reviewers
Nordic Water
Technology
Verification Centers
Project
(NOWATECH)
DHI,
NOWATECH
Water Monitoring
Center
DHI
Testing Staff
Figure 1. Organization Chart for the Joint Verification Test of Sorbisense GWS40
Passive Ground Water Sampler
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Date: 2/10/2009
1.1 Sorbisense Involvement
Sorbisense, the technology vendor, has entered into agreements with both Battelle and
DHI for this joint ETV verification. The vendor will provide the following support during
joint verification of the vendor's technology:
»»» A person from the vendor's organization to be Battelle's and DHI's point of
contact and to lead vendor's participation in joint verification of the vendor's
technology;
*»* Review and comment on the joint verification testing documents, including
Verification Protocol, Test Plan, Verification Report, Verification Statement,
and other documents pertaining to joint verification of the vendor's technology
as requested by Battelle and/or DHI;
»»» Permission to post/cite information about the vendor's technology, including
the Verification Protocol, Test Plan, Verification Report, and Joint
Verification Statement, on the US ETV website (http://www.epa.gov/etv/) and
in other program publications;
*»* Equipment/materials for testing, appropriate training in its operation, and on-
site support on an as needed basis;
»»» At no cost to DHI or Battelle or US EPA, the vendor's technology and
associated equipment/materials for testing, appropriate training in its
operation, and on-site support on an as needed basis; and
»»» Written descriptions, diagrams, and/or photographs of the vendor's
technology, as input for the Verification Protocol, Test Plan and Verification
Report.
1.2 DHI Involvement
During the verification of vendor's technology, DHI will:
»»» Provide a person from DHI's organization to be Battelle's and the vendor's
point of contact and to lead DHI's participation in verification of the vendor's
technology;
*»* Prepare and revise the Verification Protocol, Test Plan, Verification Report,
Verification Statement, and other documents pertaining to the verification of
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Joint Verification Process Document
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Date: 2/10/2009
the vendor's technology and allow Battelle, US EPA, and the Expert Group
the opportunity to review and comment on these documents;
»»» Assemble a team of qualified technical staff to conduct the verification test in
accordance with the Verification Protocol, Test Plan, and this document;
»»» Ensure that all quality procedures specified in the Verification Protocol, Test
Plan, NOWATECH Center Quality Manual Template1, and this document are
followed;
*»* Conduct a (virtual) j oint kick-off meeting with Battelle prior to test initiation;
»»» Provide a summary of the QA activities performed by the DHI WMC Internal
Auditor during the verification testing; and
»»» Provide permission to post/cite information about DHI's involvement in the
joint verification, including the Joint Verification Protocol, Test Plan,
Verification Report, and Verification Statement, on the US ETV website on
the US ETV website and in other program publications.
1.3 Battelle Involvement
During the ETV verification of the vendor's technology, Battelle will:
»»» Provide a person from Battelle's organization to be DHI's and the vendor's
point of contact;
»»» Prepare a procedural document outlining the process of the vendor's
technology verification for acceptance by the US EPA (this document);
»»» Provide input, review, and comment on the Verification Protocol, Test Plan,
Verification Report, Verification Statement, and other documents pertaining to
verification of the vendor's technology;
*»* Conduct a (virtual) j oint kick-off meeting with DHI (using checklist in
Appendix B) prior to test initiation;
»»» Strive to obtain US EPA approval for the final Verification Protocol, Test
Plan, Verification Report, including a Verification Statement; and
»»» Comply with all quality procedures and program requirements specified in the
Test/QA Plan, Quality Management Plan for the ETV AMS Center (ETV
AMS Center QMP)2, and in the U.S "Environmental Technology Verification
Program Quality Management Plan" (US ETV QMP)3, as follows:
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o Prepare and get US EPA ETV approval of an audit checklist and
provide the checklist to DHI prior to the audit;
o Conduct a technical systems audit once during the verification test;
o Audit at least 10% of the verification data;
o Prepare and distribute an assessment report for each audit;
o Verify implementation of any necessary corrective action; and
o Provide a summary of the quality assurance/quality control (QA/QC)
activities and results for the verification reports.
1.4 NOWATECH Involvement
NOWATECH responsibilities are based on the requirements stated in the
NOWATECH Center Quality Manual Template.1
1.5 US EPA Involvement
A complete list of US EPA's responsibilities in the AMS Center are based on the
requirements stated in the AMS Center ETV QMP.2 The US EPA will provide technical and
quality oversight of all ETV AMS Center activities to ensure compliance with the US ETV
program requirements.
1.6 Stakeholder Committee and Expert Group Involvement
The AMS Center's Water Stakeholder Committee is made up of buyers and users of
such technologies. This committee assists in prioritizing the types of technologies to be
verified and in specific cases, provides testing support. It also has representatives that assist
in review of the Test/QA plans, Verification Reports, and Verification Statements. The AMS
Center Water Stakeholder Committee provided concurrence for the Center to proceed with
testing in this area. The stakeholders have been kept apprised of progress throughout the
planning process for this test and have provided input during progress meetings on the test
design.
In addition, the US ETV AMS Center obtains the peer review of two external peer
reviewers and one EPA peer reviewer who are not directly involved with the verification test.
The NOWATECH ETV program uses an Expert Group to perform the external peer review
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of the documents and give input on the verification. For this test, the Expert Group is made
up of three individuals to fulfill the requirements of both programs. These individuals are
named with their affiliations in the Verification Protocol6 and Test Plan7.
2 QUALITY SYSTEMS
The Battelle and DHI quality systems to be implemented for this joint verification
will conform with the specifications listed in:
• ANSI/ASQ E4-2004, " Specifications and Guidelines for Quality
Systems for Environmental Data Collection and Environmental
Technology Programs"4 or the comparable International Standards
Organization (ISO) 90015.
Per the US EPA ETV QMP3' verification organization quality systems, such as DHFs
quality systems, are to be reviewed and approved by verification organization management,
the AMS Center Manager, and the AMS Center Quality Manager. Since not all of the
NOWATECH/DHI quality documents have been finalized, this process document will serve
to define the specific quality activities that will be performed by Battelle and DHI for this
joint verification.
3 VERIFICATION PLANNING
In performing the verification test, DHI and Battelle will follow the technical and QA
procedures specified in the NOWATECH Verification Protocol6, NOWATECH Test Plan7,
and this process document. Because DHI is preparing the Verification Protocol, Test Plan,
conducting the testing activities, and preparing the Verification Report and Verification
Statement, the procedure and expectations of the US EPA ETV program need to be clarified
in a document that explains the process and requirements (this document).
3.1 Planning the Test Design
Initially, the verification test design process produced a Verification Protocol6
and Test Plan7 based upon the NOWATECH and US EPA ETV processes. These two
documents together represent the equivalent of a US ETV AMS Center Test/QA plan.
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The protocol includes an Application and Performance Parameter Definition
Document (Appendix 3 in the Verification Protocol6) that developed relevant
parameters and ranges hereof for verification considering the vendor stated
performance, government standards, and other technologies and methods in the
market. It also evaluated existing data that has been collected to decide whether it
could be used as part of the verification or whether it could be used as the vendor
stated claims to help decide on relevant performance parameters to test during the
verification. The Application and Performance Parameter Definition Appendix was
not jointly produced and is a specific process within the NOWATECH program;
therefore, it was not reviewed by the US EPA ETV program. In designing this
verification test, DHI staff used consensus-accepted test design and a previously peer
reviewed US EPA ETV Test/QA Plan8. The design also takes into account
constraints of time, scheduling, and resources. All relevant activities pertaining to
environmental data operations have been identified, as well as performance
specifications and the appropriate controls. Finally, a process document (this
document) was produced by Battelle to address the process and differences between
the programs to ensure a successful joint verification. Collectively, these three
documents (the NOWATECH Verification Protocol6, NOWATECH Test Plan7, and
Process Document for the US EPA ETV AMS Center and NOWATECH DHI WMC
Joint Verification of the Sorbisense Ground Water Sampler) are referred to as the
"testing documents".
The US EPA ETV process utilized its Water Stakeholder Committee to guide
the test design process. It provided concurrence for the Center to proceed with testing
in this area. The stakeholders have been kept apprise of progress throughout the
planning process for this test and have provided input during progress meetings on the
test design. The committee also identified potential peer reviewers to perform a
formal technical review of the testing documents. The NOWATECH ETV program
uses an Expert Group to perform the external peer review of the documents and give
input on the verification. For this test, the Expert Group is made up of individuals to
fulfill the requirements of both programs. It includes three individuals that have
extensive experience in the field of ground water monitoring, one EPA reviewer and
two non-EPA reviewers. These reviewers have no direct involvement in the
verification test beyond providing their reviews. The comments from the reviews
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performed by the Expert Group of the testing documents and the Verification Report
and Verification Statement will be reconciled by DHI. The review process will utilize
the Review Report Form produced by the NOWATECH and is included in Appendix
C.
4 VERIFICATION TEST IMPLEMENTATION
This technology performance verification will be implemented according to the
Verification Protocol6 and the Test Plan7 (including technical procedural documents)
prepared during planning. Generation of verification test data will not be initiated until the
approved Verification Protocol and Test Plan are in place. Any data generated before the
required documents are approved will have to be repeated. In performing the verification test,
DHI will perform an internal audit of the data collection and handling that follows the
technical and QA procedures specified in these documents, as well as, the NOWATECH
Center Quality Manual Template1. The Battelle AMS Center will perform a technical
systems audit (TSA) to be sure that these requirements are being met.
A virtual joint kick-off meeting will be held prior to the start of the verification test to
review procedures for the test with all verification testing staff. The joint kick-off meeting
checklist is provided in Appendix B.
Test personnel will have access to the approved testing documents, approved changes
to testing documents, and all referenced documents. When a prescribed sequence for the
work is defined in the testing documents, work performed shall follow that sequence.
Changes to that sequence need to be documented by either amendment (planned changes) or
deviation (unplanned changes). All verification test activities will be documented. Suitable
documents are bound notebooks (e.g. laboratory record books, or LRBs), field and laboratory
data sheets, spreadsheets, computer records, and output from instruments (both electronic and
hardcopy). All documentation is implemented as described in the testing documents. All
implementation activities are traceable to the testing documents and to the test personnel. The
responsibilities of specific test personnel listed in these testing documents that leave the
project before it is completed will be reassigned.
When work cannot be implemented according to the approved testing documents, DHI
shall be responsible for providing a written amendment or a deviation report for the test
records. Amendments are produced for changes that are made to the testing document before
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the proposed change will be made. Amendments must be approved by the DHI WMC
Verification Responsible, the DHI WMC Internal Auditor, Battelle AMS Center Manager,
and the Battelle AMS Center Quality Manager. Following approval, the amendment will be
distributed to all internal personnel holding a copy of the testing documents. A deviation
report is produced for any changes to the testing document that occurred during the test.
Deviation reports must be retained in the verification test records and summarized in the
Verification Report. Frequent deviations from established procedures should result in a
retrospective review of the written document and possible revision. Amendments and
deviations will include all the information displayed on the forms shown in Appendix D.
All persons responsible for performing verification testing and Sorbisense will receive
copies of the final versions of the Verification Protocol6 and the Test Plan7 and associated
documentation provided by DHI. Current versions of the Verification Protocol6 and the Test
Plan7 and any applicable methods and SOPs are required to be physically in place at the
technology verification testing sites. Battelle oversight and inspection of the verification test
will be provided by the Battelle AMS Center Quality Manager and will be over the course of
one week. An audit checklist will be prepared and approved by the EPA AMS Center Project
Officer and EPA AMS Center Quality Manager. The audit checklist will be provided to DHI
prior to the audit. The audit will begin with an "In Briefing" conducted by the Battelle AMS
Center Quality Manager to specify and clarify the necessary points of the audit. Testing
during laboratory, standpipe, and field activities will be observed along with viewing the
external laboratory performing the reference analyses. To verify full implementation of the
testing documents, the inspection will include the testing process and any documentation
associated with the process, such as sample chain of custody transfers, instrument
maintenance and calibration, sample preparation and analysis, and data records. At the
conclusion of the audit there will be an "Exit Briefing" held to discuss the findings and
corrective actions necessary. The Battelle AMS Center Quality Manager will also provide a
written report, verify the completion of any corrective actions needed, and retain a copy of
the report with permanent Battelle AMS Center Quality Manager records. The report will be
commented on by DHI WMC and comments addressed before it is distributed. The
Assessment Reporting Form is presented in Appendix E. The EPA AMS Center Project
Officer will be included in the routing of the inspection results and a written copy provided to
both the EPA AMS Center Project Officer and EPA AMS Center Quality Manager.
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5 ASSESSMENT AND RESPONSE
Assessments will be planned, scheduled, conducted, and reported in order to measure
the efficacy of the Battelle and DHI WMC quality procedures and verification execution.
The testing will be audited internally by the WMC Internal Auditor in accordance with the
Verification Protocol6 and Test Plan7. The WMC Document Reviewer and Internal Auditor
equate to the Battelle AMS Center Quality Manager. The WMC Document reviewer will
perform the technical review of the Test Plan and Verification Report documents. The WMC
Internal Auditor will perform an audit based upon identified critical points. The procedure
includes two main steps:
• Check that the protocol/plan is prepared and followed in accordance with the
DHI QMS and the WMC QM (horizontal audit)
• Check of verification/test parameters and data at the identified critical points, ie a
vertical audit in lab, office and/or field.
Data from the testing will be controlled by the Verification Responsible and the Test
Responsible when received. Data integrity will be controlled by the Test Responsible
(transfer of raw data to spreadsheets) and Verification Responsible (calculations as part of
evaluations) as spot checks (5% of the data).
Monitoring of the work process to be conducted by the Battelle AMS Center Quality
Manager will be done to:
• Ensure satisfactory performance based on requirements,
• Ensure required actions (as specified in implementation documents) are
performed so that routine measurements meet specifications,
• Ensure preventive maintenance is performed and documented as specified in
facility and study records,
• Ensure calibrations are performed as planned and prescribed,
• Ensure corrective actions are implemented and documented as planned in
response to items of nonconformance.
Assessment types, responsibility, and schedule for this joint verification will be as
shown in Table 1.0, and are defined as follows:
Quality Systems Audit (QSA), an on-site review of the implementation of the
WMC quality procedures. This review is used to verify the existence of, and
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evaluate the adequacy of, the internal quality system. This review will be done in
conjunction with the Technical Systems Audit.
Technical Systems Audit (TSA), a qualitative on-site evaluation of sampling
and/or measurement systems associated with a particular verification test. The
objective of the TSA is to assess and document the acceptability of all facilities,
maintenance, calibration procedures, reporting requirements, sampling, and
analytical activities, and quality control procedures in the test. Conformance
with the testing documents and associated methods and/or Standard Operating
Procedures is the basis for this assessment. The Battelle AMS Center Quality
Manager will prepare and use an audit checklist that is approved by the EPA
AMS Center Quality Manager. The checklist will be available to DHI before
the audit takes place. This review will be done in conjunction with the QSA.
Performance Evaluation Audits (PE), a quantitative evaluation of the
measurement systems used. The type and frequency of performance evaluation
self-audits are specified in the Test plan for the joint verification test. The value
or composition of reference materials must be certified or verified prior to use,
and the certification or verification must be adequately documented. The
Battelle AMS Center Quality Manager will review results of PE audits during
the TSA; however, it is most preferable for the PE results to be shared with
Battelle as soon as they are available, so that any issues can be resolved.
Audits of Data Quality, an examination of the verification data after they have
been collected and verified by project personnel. The Battelle AMS Center
Quality Manager will audit at least 10% of all verification data, including
equations and calculations.
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Table 1.0 Assessments for the Joint Verification
Assessment Subject of Minimum Reason for
Tool Assessors Responders Assessment Frequency Assessment Report Reviewed by
Quality
Systems
Audit
Technical
Systems
Audits
Performance
Evaluation
Audits
Audits of
Data Quality
Battelle AMS
Center Quality
Manager
Battelle AMS
Center Quality
Manager and DHI
Internal Auditor
Battelle AMS
Center Quality
Manager and DHI
Internal Auditor
Battelle AMS
Center Quality
Manager and DHI
Internal Auditor
DHI
DHI
DHI
DHI
NOWATECH
Quality
Manual
Template
Verification
Protocol, Test
Plan, and
Process
Document
Verification
Protocol, Test
Plan, and
Process
Document
raw data and
summary data
once
once
once
At least 10%
of the
verification
data
assess quality
management
practices of
verification
collaborators
assess
technical
quality of
verification
tests
assess
measurements
performance
assess data
calculations
and reporting
EPA directors of
quality assurance
EPA AMS Center
Project Officer
Battelle AMS Center
Manager and Test
Coordinator
NOWATECH WMC
Verification
Responsible
EPA AMS Center
Project Officer
EPA AMS Center
Quality Manager
Battelle AMS Center
Manager and Test
Coordinator
NOWATECH WMC
Verification
Responsible
EPA AMS Center
Project Officer
EPA AMS Center
Quality Manager
Battelle AMS Center
Manager and Test
Coordinator
NOWATECH WMC
Verification
Responsible
EPA AMS Center
Project Officer
EPA AMS Center
Quality Manager
Battelle AMS Center
Manager and Test
Coordinator
NOWATECH WMC
Verification
Responsible
5.1 Assessment Reports
Each assessment must be fully documented. The Battelle AMS Center
Quality Manager and the DHI WMC Verification Responsible will archive all
assessment reports generated for this verification test.
Each assessment must be responded to by the appropriate level of
management. The Battelle quality assessment reports shall require a written
response by the person performing the inspected activity, and
acknowledgment of the assessment by the Battelle AMS Center Test
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Coordinator. The Assessment Reporting Form is provided in Appendix E. An
assessment report will also be prepared by the WMC Internal Auditor and
provided to the Battelle AMS Center test coordinator for archive.
Corrective action must be documented and approved on the original
assessment report, with detailed narrative in response to the assessor's finding.
Initials and date are required for each corrective action response.
Acknowledgment of the response will be provided by the Battelle Test
Coordinator.
Implementation of corrective actions must be verified by the Battelle
AMS Center Quality Manager or the DHI Internal Auditor to ensure that
corrective actions are adequate and have been completed. This will be done in
real-time if corrective actions can be immediately performed and signed off on
the assessment report. Alternatively, should the corrective action require
additional approvals not immediately available on-site, the DHI Internal
Auditor may need to repeat the inspection, as the designee of the Battelle
AMS Center Quality Manager, in order to corroborate the implementation and
effectiveness of the corrective action.
5.2 Stop Work
Assessor responsibility and authority to stop work during a verification
test for quality considerations is delegated to DHI and Battelle. DHI must
ensure compliance with all applicable Danish federal, state, and local safety
policies during the performance of verification testing.
Should it be determined during an assessment that test objectives of
acceptable quality cannot be achieved during performance of verification
testing, the Battelle AMS Center is responsible for immediately notifying the
DHI WMC Verification Responsible of the need to consider a stop work
order. The DHI WMC Verification Responsible will then direct the staff
accordingly. The EPA AMS Center Quality Manager will notify the EPA
AMS Center Project Officer if work of inadequate quality is discovered.
Documentation is required of any stop work order and the corrective
action implemented and shall be maintained as part of the Battelle quality
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records, with a copy provided to the EPA AMS Center Project Officer and
EPA AMS Center Quality Manager.
5.3 Response
Responses to TSA adverse findings should be addressed within 10
working days after the TSA report is completed. However, it is expected that
findings that have a direct impact on the conduct of a verification test will be
corrected immediately following notification of the finding.
Responses to each adverse finding will be documented in the assessment
report. Ideally, assessment reports will provide space after each adverse
finding for a response to be recorded. The response will indicate the
corrective action taken or planned to address the adverse finding. The
response should be signed and dated by the staff responsible for implementing
the corrective action.
Any corrective action that cannot be immediately implemented will be
verified following completion by the Battelle AMS Center Quality Manager or
designee. Once all corrective action associated with an assessment report has
been taken, the Battelle AMS Center Quality Manager or designee will initial
the corrective action in the assessment report thus documenting verification of
the corrective action. Any impact that an adverse finding had on the quality of
verification test data should be addressed in the verification report.
The TSA report, with responses to adverse findings recorded within, will
be sent to EPA within 10 working days after the Battelle AMS Center Quality
Manager has verified all corrective actions.
6 DOCUMENTATION AND REPORTING
6.1 Responsibilities for these activities concerning documentation and reporting are
summarized in Table 2.0 and are detailed below.
6.1.1 Preparation
Individual case requirements and this document shall guide document
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Date: 2/10/2009
and record content and/or format. Guidance for content and/or format
are derived by the EPA ETV and NOWATECH directives and the
following documents:
• ANSI/ASQ E4-20044.
• ETV AMS Center QMP2.
• US EPA document "EPA QA/R-2, EPA Requirements for Quality
Management Plans, March 2001.
• NOWATECH Center Quality Manual Template1.
6.1.2 Review/Approval.
Record review/approval for joint verification testing documents shall be
performed by qualified technical and/or management personnel as
described in Table 2.0. The individual reviewer shall have access to all
needed references.
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Table 2.0 Document and Reporting Responsibilities for the Joint Verification*
Preparation/
Record Type Updating Review Approval Finals Distributed to:
Verification Protocol
and Test Plan
(including SOPs,
amendments and
deviations)
Raw data
Verification Report
ETV Verification
Statement
Audit Reports
Audit Reports
DHI
DHI
DHI
DHI
DHI Internal
Auditor
Battelle AMS
Center
Quality
Manager
Battelle AMS Center Manager
Battelle AMS Center Qualify
Manager
EPA AMS Center Quality Manager
EPA AMS Center Project Officer
NOWATECH WMC Verification
Responsible
DHI Document Reviewer
Stakeholders/Expert Group
Vendor
WMC Internal Auditor
Battelle AMS Center Manager
Battelle AMS Center Qualify
Manager
EPA AMS Center Quality Manager
NOWATECH WMC Verification
Responsible
Vendor
Stakeholders/Expert Group
Battelle AMS Center Manager
Battelle AMS Center Qualify
Manager
EPA AMS Center Project Officer
EPA AMS Center Quality Manager
NOWATECH WMC Verification
Responsible
WMC Document Reviewer
Vendor
ETV Program Director
Stakeholders/Expert Group
DHI Test Responsible
NOWATECH WMC Verification
Responsible
Battelle AMS Center Manager
Battelle Verification Test
Coordinator
NOWATECH WMC Verification
Responsible
WMC Test Responsible
EPA AMS Center Project
Officer
EPA AMS Center Quality
Manager
NOWATECH WMC
Verification Responsible
N/A
EPA AMS Center Project
Officer
EPA AMS Center Quality
Manager
NOWATECH WMC
Verification Responsible
EPA Laboratory Director
Battelle Management
EPA AMS Center Project
Officer
EPA AMS Center Quality
Manager
DHI Director RDI and
Quality Management
NOWATECH Steering
Committee Head
N/A
N/A
Testing Staff
Vendor
EPA AMS Center Project Officer
EPA AMS Center Quality Manager
NOWATECH WMC Verification
Responsible
EPA can request copies
ETV Program Director
EPA AMS Center Project Officer
ETV Webmaster
Vendor
NOWATECH WMC Verification
Responsible
ETV Program Director
EPA AMS Center Project Officer
Battelle AMS Center Manager
NOWATECH WMC Verification
Responsible
ETV Webmaster
Vendor
NOWATECH WMC Verification
Responsible
Battelle AMS Center Quality
Manager
Battelle AMS Center Manager
Battelle Verification Test
Coordinator
EPA AMS Center Project Officer
EPA AMS Center Quality Manager
EPA AMS Center Project Officer
EPA AMS Center Quality Manager
Battelle AMS Center Manager
Battelle Verification Test
Coordinator
NOWATECH WMC Verification
Responsible
*See Appendix A for the roles and names of the individuals filling these roles.
A6.2 Reporting
The end result of the joint verification process will be a Verification
Report and Verification Statement for the Sorbisense GWS40. The review
and approval procedures for the verification report and statement for US EPA
ETV program purposes are given in Table 2.0. The Verification Report will be
peer-reviewed by external reviewers in the Expert Group and the Verification
Statement will be signed by an EPA laboratory director, Battelle management,
the DHI Director of Research and Quality Management and the NOWATECH
Steering Committee Head. Appendix F presents a preliminary template for a
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Verification Statement. This document will be expanded and organized to
meet US EPA ETV and NOWATECH program requirements.
All logos will appear on the Verification Statement. These will
include: US ETV, Battelle, NOWATECH, DHI, and US EPA logos. All logos
except the US EPA logo will appear on the cover page of all other joint testing
documents (Test Plan, Verification Protocol, Verification Report). All of
these testing documents will be made publicly available on the US EPA ETV
Web site (www.epa.gov/etv) regardless of the technology's performance.
The vendor will comply with both the NOWATECH and US EPA
ETV policies on referencing the verification documents of their technology.
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REFERENCES
1. NOWATECH. ETV Test Center and Test Organization: Center Quality Manual
Template. December 2008.
2. Battelle. Quality Management Plan for the ETV Advanced Monitoring Systems
Center. Version 7.0. 11-17-2008.
3. United States Environmental Protection Agency. Environmental Technology
Verification Program Quality Management Plan. Version 3.0. January 2008.
4. American Society for Quality. ANSI/ASQ E4-2004. Quality systems for
environmental data and technology programs - Requirements with guidance for use.
1-4-2004.
5. International Standardization Organization. ISO 9001. Quality management systems
-Requirements. 11-15-2008.
6. DHI. Sorbisense GWS40 Passive Sampler, Joint Verification Protocol. January
2009.
7. DHI. Sorbisense GWS40 Passive Sampler, Joint Test Plan. January 2009.
8. Sandia National Laboratories. Groundwater Sampling Technologies Verification Test
Plan. Environmental Technology Verification Program. Version 2.0. July 1999.
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APPENDIX A
ROLES OF KEY PERSONNEL
NOWATECH Role:
NOWATECH person who signs the Verification Statement: NOWATECH Steering
Committee Head - Christian Gran
DHI Water Monitoring Center (DHI WMC) Roles:
DHI person who signs the Verification Statement: Director of Research and Quality -
J0rn Rasmussen
WMC Verification Responsible: Christian Gran
WMC Test Responsible: Gerald Heinicke
WMC Document Reviewer: Anders Lynggaard Jensen
WMC Internal Auditor: Louise Schliitter
WMC Verification and Test staff: several - see protocol and plan
US EPA ETV Roles:
EPA person who signs the Verification Statement: National Risk Management
Research Laboratory (NRMRL) Director - Sally Gutierrez
EPA AMS Center Project Officer: John McKernan
EPA AMS Center Quality Manager: Lauren Drees, EPA NRMRL Director for
Quality Assurance
Battelle Advanced Monitoring Systems (AMS) Center Roles:
Battelle person who signs the Verification Statement: Chemical, Environmental and
Materials Operations Manager - Lisa McCauley
AMS Center Manager: Amy Dindal
AMS Center Quality Manager: Zach Willenberg
AMS Center Test Coordinator: Anne Gregg
Parallel Roles between the NOWATECH and US EPA ETV programs:
Verification Responsible = Center Manager
Test Responsible = Center Test Coordinator
Internal Auditor + Document Reviewer = Center Quality Manager
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APPENDIX B
KICK OFF MEETING CHECKLIST
ETV JOINT VERIFICATION TEST KICK-OFF MEETING
PURPOSE
To prepare verification testing staff for the NOWATECH and US EPA ETV AMS Center
joint verification test and review critical logistical, technical, and administrative aspects of
the test. The kick-off meeting will be scheduled prior to the start of testing. It should be near
the start of the test but allow time for the test coordinator to address any lingering issues.
FORM
The kick off meeting will be virtual, i.e. based upon phone and WebEx sharing of documents.
STAFF TO ATTEND
• Verification test coordinator/responsible (DHI and Battelle)
• ETV program manager (Battelle)
• QA manager (Battelle)
• US EPA ETV program staff and NOWATECH (invited but optional)
All testing staff involved in all. phases of test will subsequently have a kick-off meeting on-
site with the DHI WMC verification Responsible. The external laboratory is informed
through requisitions of analyses only.
PROJECT MANAGEMENT
• Review roles/responsibilities of all staff attending meeting
• Stakeholders, EPA/ETV program manager, and EPA/QA staff pre-notified of testing
schedule and start date?
• Review test schedule
• Formal distribution of final, signed hard-copy Test/QA plan made to all staff
involved.
• Documentation of all pertinent forms.
o Peer review forms on Protocol document and Test plan. Must include one
EPA reviewer/two non-EPA peer reviewers.
o Final Test/QA plan approved by vendor.
o Vendor-Collaborator agreement signed and stored in project files?
o Documentation that the vendor is satisfied that the staff operating the
technology are proficient in its use.
QUALITY ASSURANCE
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• Copies of all standard methods cited or included in the Test plan available to testing
staff and in laboratory where test will be performed?
• EPA QA staff pre-notified of test start date?
• Remind testing staff to sign and date everything.
• If samples are to be transported between labs, field sites, and DHI bring chain-of-
custody form to meeting, review how to complete, and where to obtain form.
• Review deviation/amendment procedures at meeting - what to do in the middle of a
test if testing document cannot be followed - who to notify/what forms to file.
• Review testing document at meeting - identify key testing procedures and critical
steps to ensure no ambiguity or questions.
• Are or will there be copies of the certificates of analysis in the verification test
records?
• When will PE audit be performed? Who will perform? Has materials/equipment
been purchased or obtained for the PE audit? What are QC limits? What to do if QC
limits are not met? Who to contact?
• Will regular communication between DHI and Battelle be maintained? If so, how?
Daily/weekly email updates?
TECHNICAL
• Emphasize to testing staff to document anything and everything that is observed about
the technologies, particularly if there are unusual sample results (e.g., sample color).
• Are provisions made to handle daily preparation of solutions/standards, if necessary?
• Take digital photos of all test activities.
DATA/REPORTING
• Review data recording forms or sheets at meeting or discuss how/where will data be
recorded for each testing activity
• How are data going to be converted electronically? Are data saved in technology
undergoing verification and then exported to Excel? Or will data be recorded
manually by the operators? If so, how will transcription errors be avoided?
• Data review - who will be doing two week review for each data set collected? If
Battelle staff not on-site, how will data be transmitted to Battelle?
• Distribute and review report schedule. Reporting should begin at the same time as
testing.
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APPENDIX C
REVIEW REPORT FORM
Review report
Document title:
Reviewer
name:
Name:
Organization:
Address:
Telephone:
E-mail
Document date: November
2008
Review date:
Review results
Rate items
Contents
Scope
Organization
Data quality
Method validity
Conclusions
Other (specify)
Satisfactory
Unsatisfactory
Overall recommendation
Acceptable as is
Minor revisions
Major revisions
Not acceptable
Reason
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Joint Verification Process Document
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Date: 2/10/2009
Revision details
Topic
Report chapter,
section, page
Revision
required
Reason
Revision action(to be filled in by
document owner during revision
after review)
Add additional rows, if pertinent.
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APPENDIX D
JOINT VERIFICATION TESTING DOCUMENT
AMENDMENT AND DEVIATIONS FORMS
AMENDMENT
TESTING DOCUMENT TITLE AND DATE:
AMENDMENT NUMBER:
EFFECTIVE DATE:
PART TO BE CHANGED/REVISED:
CHANGE/REVISION:
REASON FOR CHANGE:
ORIGINATED BY:
Battelle AMS Center Test Coordinator or DHI WMC Test Responsible
DATE
APPROVED BY:
DHI WMC Internal Auditor DHI WMC Verification Responsible
DATE DATE
Battelle AMS Center Quality Manager Battelle AMS Center Manager
DATE DATE
Required Distribution with documentation - All individuals/organizations listed on distribution for
the applicable Test/QA Plan, including but not limited to:
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Date: 2/10/2009
Battelle AMS Center Manager
NOWATECH WMC Verification Responsible
Testing Staff
Battelle Quality Manager
WMC Internal Auditor
Subcontractors (if any)
EPA/ETV AMS Center Project Officer
EPA/ETV AMS Center Quality Manager
Vendor
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DEVIATION REPORT
TESTING DOCUMENT TITLE AND DATE:
DEVIATION NUMBER:
DATE OF DEVIATION:
DESCRIPTION OF DEVIATION:
CAUSE OF DEVIATION:
IMPACT OF DEVIATION ON THE TEST:
CORRECTIVE ACTION:
ORIGINATED BY:
Battelle AMS Center Test Coordinator or DHI WMC Test Responsible
DATE
ACKNOWLEDGED BY:
DHI WMC Quality Manager Battelle AMS Center Quality Manager
DATE DATE
Required Distribution with documentation - All individuals/organizations listed below:
Battelle AMS Center Manager
NOWATECH WMC Verification Responsible
Battelle AMS Center Quality Manager
WMC Internal Auditor
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APPENDIX E
ASSESSMENT REPORTING FORM
Quality Assurance Routing Sheet
Verification Test:
Audit Type:
Test Coordinator:
Vendor:
Auditor: Date:
Test Coordinator, please complete the attached form indicating CORRECTIVE
ACTION TAKEN (IF NEEDED), sign and date this Routing Sheet in the space
provided beside your name, and return the entire set when completed to the Battelle
AMS Center Quality Manager no later than .
Route To Signature Date
WMC Test
Responsible
AMS Center Test
Coordinator
Approval
Battelle AMS Center
Manager
Battelle AMS Center
Quality Manager
NOWATECH WMC
Verification
Responsible
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Audit Comment Sheet
Instructions: The Battelle AMS Center Quality Manager will fill out the first column for the audit indicated above. The Verification Test Coordinator (or
assigned responder) will respond to the comments and initial and date the response in column three. The Battelle AMS Center Quality Manager will verify
and document that the response/corrective action has been completed by initialing and dating the final column.
QA Comment
Testing Coordinator
Response/Corrective Actions
Responder
Initials/ Date
QA Initials/
Date
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APPENDIX F
EXAMPLE JOINT VERIFICATION STATEMENT
THE ENVIRONMENTAL TECHNOLOGY VERIFICATION
PROGRAM
This is a preliminary template of a Verification Statement that may be expanded
and organized to meet NOWATECH and US EPA ETV program requirements.
NOWATECH and DHI logos will be added.
U.S. Environmental Protection .Agency
Batreiie
UK Business of Innovation
TECHNOLOGY TYPE:
APPLICATION:
TECHNOLOGY NAME:
COMPANY:
ADDRESS:
WEB SITE:
E-MAIL:
PHONE:
FAX:
ETV Joint Verification Statement
• Description of EV and the organizations involved in this joint verification.
• Name technology category and technology (product) that was jointly verified.
VERIFICATION TEST DESCRIPTION
• Describe the verification test- when, how
• Describe the performance parameters
• Describe the QA performed
TECHNOLOGY DESCRIPTION
Describe the technology (product)
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VERIFICATION RESULTS
• Summary of results by performance parameters
Signature blocks for:
NOWATECH Steering Committee Head - Christian Gran
DHI Director of Research and Quality - J0rn Rasmussen
Battelle Chemical, Environmental and Materials Operations Manager - Lisa McCauley
US EPA National Risk Management Research Office of Research and Development -
Sally Gutierrez
NOTICE: ETV verifications are based on an evaluation of technology performance under specific,
predetermined criteria and the appropriate quality assurance procedures. EPA and Battelle make no expressed or
implied warranties as to the performance of the technology and do not certify that a technology will always
operate as verified. The end user is solely responsible for complying with any and all applicable federal, state,
and local requirements. Mention of commercial product names does not imply endorsement.
-------
NOWATECH
Hnrdir Innnvjtinn f cntf»
Baireiie
I'll.* I kii>Liiuif ^ Innovation
Sorbisense GSW40 Passive Sampler
Joint verification protocol
Volatile organic compounds in groundwater
January 2009
Version approved
-------
Sorbisense GSW40 Passive Sampler
Joint verification protocol
Agern Alle 5
DK-2970 H0rsholm
Denmark
Tel: +4545169200
Fax: +4545169292
dhi@dhigroup.com
www.dhigroup.com
Vendor
Sorbisense ApS
Vendors representative
Hubert deJonge
Project
Nordic Water Technology Verification Centers
Authors
Christian Gran
Revision
Joint verification protocol
Description
Key words
Environmental technology verification, passive
sampler, groundwater
Project No
80144
Date
January 2009
Approved by
CHG ALJ ALJ
By Checked Approved Date
Classification
£3 Open
CD Internal
CD Proprietary
Distribution
Sorbisense
DHI
UBA-A
Battelle
US EPA
HdJ
CHG, GHE, MTA
DM
AMG, ZJW
LD
No of copies
File distribution
only
-------
TABLE OF CONTENTS
TABLE OF CONTENTS
2 INTRODUCTION 1
2.1 Name of product 1
2.2 Name and contact of vendor 1
2.3 Name of center/verification responsible 1
2.4 Verification Test Organization 1
2.5 Expert group 2
2.6 Verification process 3
3 DESCRIPTION OF THE TECHNOLOGY 3
4 DESCRIPTION OF THE PRODUCT 4
5 APPLICATION AND PERFORMANCE PARAMETER DEFINITIONS 6
5.1 Matrix/matrices 6
5.2 Target(s) 6
5.3 Effects 6
5.4 Performance parameters for verification 6
5.5 Additional parameters 8
6 EXISTING DATA 8
6.1 Summary of existing data 8
6.2 Quality of existing data 9
6.3 Accepted existing data 9
7 TEST PLAN REQUIREMENTS 9
7.1 Test design 10
7.2 Reference analysis 11
7.3 Data management 11
7.4 Quality assurance 11
7.5 Test report 11
8 EVALUATION 11
8.1 Calculation of performance parameters 12
8.2 Evaluation of test data quality 13
8.3 Compilation of additional parameters 13
8.3.1 User manual 13
8.3.2 Product costs 14
8.3.3 Occupational health and environment 15
9 VERIFICATION SCHEDULE 15
10 QUALITY ASSURANCE 15
-------
APPENDIX 1 17
Terms and definitions used in the verification protocol 17
APPENDIX 2 22
References 22
APPENDIX 3 25
Application and performance parameter definitions 25
-------
2 INTRODUCTION
Environmental technology verification (ETV) is an independent (third party)
assessment of the performance of a technology or a product for a specified
application, under defined conditions and quality assurance.
This verification is a joint verification with the US EPA ETV scheme and the
Advanced Monitoring Systems Centre, Battelle, see the verification protocol
III for details on organization and implications. The compliance of the test with
both scheme's requirements is ensured through a process document 111.
2.1 Name of product
The product is the Sorbisense GWS40 passive sampling system (106-012-11)
with samplers (cartridges) for analysis of volatile organic compounds (VOCs)
(no. 043-0091-12, 043-0101-12, 043-0102-12). The analysis of the samplers is
performed by AlControl under ISO 17025 accreditation. The passive samplers
and the subsequent analysis of the cartridges constitute the product.
2.2 Name and contact of vendor
Sorbisense A/S, Niels Pedersens Alle 2, DK-8830 Tjele, Denmark, phone +45
8999 2505, +45 8999 2599.
Contact: Hubert de Jonge, e-mail hubert@sorbisense.com.
The laboratory responsible for the analysis of samples (subcontractor to the
vendor) is: ALcontrol Laboratories, Steenhouwerstraat 15, 3194 AGHoogvliet,
Netherlands,
Contact: Jaap Willem Hutter, e-mail j.hutter@alcontrol.nl
2.3 Name of center/verification responsible
NOWATECH Water Monitoring ETV Center, DHI, Agern Alle 5, DK-2970
H0rsholm, Denmark.
Verification responsible: Christian Gran, e-mail chg@dhigroup.com, phone
+45 95 16 95 70, mobile +45 29 65 34 47.
US EPA Advanced Monitoring System Center, Battelle Memorial Institute,
505 King Avenue, Columbus, Ohio 43201-2693, US.
Verification responsible: Anne M. Gregg (AMG), e-mail gregga@battelle.org,
phone+1 614-424-7419
2.4 Verification Test Organization
The verification will be conducted as a joint verification between the Nordic
Water Technology Verification Centers (NOWATECH ETV) and the U.S.
-------
Environmental Technology verification (US ETV) Program. The verification is
planned and conducted to satisfy the requirements of the ETV scheme
currently being established by the European Union (EU ETV) and the US ETV
program. Verification and tests will be performed by DHI as NOWATECH
Water Monitoring Center (DHI WMC) under contract with Nordic Innovation
Centre, Nordic Council of Ministers. Battelle will be participating as the
manager of the ETV Advanced Monitoring Systems (AMS) Center through a
cooperative agreement with the U.S. Environmental Protection Agency (EPA).
The day to day operations of the verification and tests will be coordinated and
supervised by DHI personnel, with the participation of the vendor, Sorbisense.
The testing will be conducted in the DHI laboratories, H0rsholm, Denmark and
in the field in the Copenhagen area, Denmark. DHI will operate the samplers
during the verification. Sorbisense will provide the sampling systems, the
samplers and the analysis of samplers for the test. Furthermore, Sorbisense will
provide user manuals and operation instructions, and will participate in
development of protocol and plans with DHI. Battelle will ensure that the
verification and tests is planned and conducted to satisfy the requirements of
the US ETV program, including obtaining input and concurrence from its
stakeholder group, as described in the process document 111. Battelle will also
participate in the development of the plan document for the verification and
tests and perform quality assurance of the verification and tests. EPA will
participate in quality assurance of the verification and tests.
An expert group is established to provide independent expert review of the
planning, conducting and reporting of the verification and tests.
The organization chart in Figure 1 identifies the relationships of the
organization associated with this verification and tests.
Figure 1 Organization of the verification and tests
us EPA ETV
NOWATECH ETV
Battelle AMS
Verifications
DHI WMC
Tests
Sorbisense
Battelle AMS
stakeholders
2.5 Expert group
The expert group assigned to this verification and responsible for review of the
verification plan and report documents includes:
-------
Dietmar Miiller (DM), e-mail dietmar.mueller@umweltbundesamt.at,
Contaminated Sites, Umweltbundesamt, Spittelauer Lande 5, 1090 Wien,
Austria, phone +43-(0)1 -313 04/5913
Mike Sherrier (MS), e-mail michael.p.sherrier@usa.dupont.com, DuPont,
Barley Mill Plaza, Bldg 19-1132, 4417 Lancaster Pike, Wilmington, DE
19805, US, phone +1 302-892-1168
Cynthia Paul (CP), e-mail paul.cindy@epa.gov, U.S. Environmental Protection
Agency, 919 Kerr Research Drive, P.O. Box 1198. Ada, OK 74820, US,
phone: +1 580-436-8556.
2.6 Verification process
Verification and tests will be conducted in two separate steps, as required by
the EU ETV. The steps in the verification are shown in Figure 2.
Figure 2 Verification steps
References for the verification process are the Quality Management Plan for
the Battelle AMS /3/ and the Quality Manual for the ETV operations at DHI
following the NOWATECH Quality Manual Template /4/.
A joint US EPA ETV and NOWATECH ETV verification statement will be
issued after completion of the verification. Ensuring the compliance of the
verification with the US ETV requirements is done following a process
document developed by Battelle AMS.
This verification protocol, the test plan and the process document shall be seen
as one consolidated verification description.
DESCRIPTION OF THE TECHNOLOGY
The technology product to be verified is applying the technology of passive
sampling.
-------
Passive sampling is based upon distribution of solutes between the sampled
medium, e.g. a water body, and a collecting medium, the sampler or sampling
medium. Flow of solute from one medium to the other continues until
equilibrium is established in the system, or until the sampling session is
terminated by the user. The amount of solute in the sampling medium is then
determined analytically and can be used to calculate the concentration in the
sampled medium. With exposure until equilibrium, the sampled medium
concentration can be calculated based on the solute distribution between the
two media involved as obtained by e.g. experimental calibration of the device.
With exposure until the sampling session is terminated by the user (before
achieving equilibrium), the time-weighted average solute concentration in the
sampled medium can be determined from the exposure time and the sampling
rate for the solute in question.
A wide range of products are available for passive sampling (equilibrium based
and rate controlled) of solutes (inorganic and organic) from waters.
4 DESCRIPTION OF THE PRODUCT
The Sorbisense passive sampler combines the principle of passive sampling
with a patented tracer based calculation of the amount of water that the sampler
has been exposed to. The sampler consists of a polypropylene cartridge
containing, see Figure 3:
• A sorbent that absorbs solutes from water passing the sampler.
• Tracer salt that dissolves proportionally with the volume of water
passing the cartridge.
• Filters between sorbent and tracer salt compartments.
Figure 3 Principle of the Sorbisense sampler
. Sorbent
Filter -——___
i
__^ , Tracer salt
Rlter
Tracer salt
i ^ \ I
Rlter
When the sampling period is over, the Sorbisense sampler is sent to a
laboratory for extraction and analyses whereupon time-weighted average solute
concentration is reported.
For analysis, the cartridge is cut and the sorbent taken for batch extraction with
acetone followed by quantification of sorbed compounds by headspace GC-
-------
MS. The tracer salt (calcium citrate) is taken for extraction with 0.2 M HC1 and
quantification of extracted calcium with ICP.
The sampled water volume is calculated from:
V =
start ,tracersalt lab ,tracersalt
~K
The solute water concentration is calculated from:
C=MsoluJV =
Msolute*K
start,tracersalt start ,tracersalt
V= water volume in L; Mstart: tracersalt = weighed amount of salt in production as
mg Ca; Miab, tracersalt = extracted amount of salt in laboratory as mg Ca; C =
VOC concentration in ug/L; Msoiute = mass of VOC detected in ug; K =
solubility of the salt with the standard calibration value as 184 mg Ca/L.
The product to be verified here is the Sorbisense GWS40 sampling system
intended for sampling of shallow groundwater and equipped with samplers for
volatile organic compounds.
Figure 4 Mounting of the GWS40 sampling system
The GWS40 is mounted with air hose, safety string and Sorbisense samplers
(can be mounted in top and bottom of the GWS40) and is subsequently
lowered to the desired measuring depth, see Figure 4. The water pressure will
push water through the sampler slowly filling the GWS40. The air hose enables
the air inside the GWS40 to escape to the atmosphere. When the measuring
period is over, the samplers are removed and sent to the laboratory for analysis.
-------
APPLICATION AND PERFORMANCE PARAMETER
DEFINITIONS
The application is defined as detailed in the application definition appendix,
Appendix 3, in terms of matrix/matrices for use, targets of monitoring and
effects.
The passive sampler is supplied by the vendor as combined sampling and
analysis, and the verification shall accordingly see these two steps as one.
5.1 Matrix/matrices
The matrix of the application is groundwater and the field of application is
investigations of (potentially) contaminated groundwater (groundwater
investigations).
5.2 Target(s)
The targets of the product are volatile organic contaminants (VOC), here
mono-, di-, tri- and -tetrachloroethenes, benzene, toluene, ethylbenzene and
xylenes (BTEX) and methyl-fert-butylether (MTBE), see Table 1.
Table 1 Targets of the Sorbisense GSW40 VOC sampler
Target compounds
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
5.3 Effects
The effects for the application are set in terms of limit of detection (LoD),
precision, trueness, range of application and robustness.
5.4 Performance parameters for verification
The ranges of performance relevant for the application, as derived in Appendix
3, are presented in Table 2. These ranges are used for planning the verification
and testing only. For Sorbisense VOC sampling, concentrations above 2,000
|ig/L are not likely to be measurable (vendor information) and are not included
in the verification. The calculation of the performance parameters explaining
their principle is given in Table 5.
-------
Table 2 Ranges of performance parameters relevant for groundwater investigations
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
Limit of
detection
M9/L
0.02-0.05
0.1-1
0.1-1
0.1-1
0.1-1
0.1-1
0.5-5
0.5-5
0.5-5
0.2-2
Precision
%
<25
<25
<25
<25
<25
<25
<25
<25
<25
<25
Trueness
%
75-125
75-125
75-125
75-125
75-125
75-125
75-125
75-125
75-125
75-125
Range of
application
M9/L
LoD-1*10b
LoD-1*10b
LoD-1*10b
LoD-1*10b
LoD-0.1*10b
LoD-1*10b
LoD-0.1*10b
LoD-0.1*10b
LoD-0.1*10b
LoD-1*10b
Robustness
%
100±15
100±25
100±25
100±25
100±25
100±25
100±25
100±25
100±25
100±25
Limit of detection shall be evaluated from the standard deviation of replicate
measurements at less than 5 times the detection limit evaluated and will reflect
a less than 5% risk of false blanks.
Precision shall be evaluated under repeatability and reproducibility conditions.
Repeatability is obtained as the standard deviation of measurements done with
the same measurement procedure, same operators, same measuring system,
same operating conditions and same location, and replicate measurements on
the same or similar objects over a short period of time. Reproducibility is
obtained as the standard deviation of measurements that includes different
locations, operators, measuring systems, and replicate measurements on the
same or similar objects. In laboratory terminology, repeatability is the within
series precision and the reproducibility the between series precision.
Trueness is the correspondence between (mean) concentrations found in
measurements and corresponding true concentrations.
In addition to conventional trueness, the trueness of time-weighted averages
obtained with the sampler shall be verified.
The range of application is the range from the LoD to the highest concentration
with linear response.
The parameters of robustness to be verified are sampling depth, sampling time,
sampling concentration and groundwater ionic strength. Robustness is basically
the trueness as found for different values of the robustness parameters.
The version of the product to be verified is designed for sampling shallow
aquifers, i.e. with sampling depths from 0.5 to 5 m below groundwater table
(mbgw). The pressure on samplers will vary with depth to the sampling
positions, and pressure variations in the range of 1.05-1.5 atmosphere shall
accordingly be verified.
Sampling time variations from 3 to 9 days shall be verified covering the
different sampling times recommended by the vendor, as the exposure time
may impact the performance.
-------
In investigations of contaminated groundwater, both uncontaminated and
strongly contaminated groundwater will be included. The concentrations
verified shall therefore reflect the range from uncontaminated groundwater to
highly contaminated groundwater, with at the least 3 concentrations distributed
over a relevant range.
In order to reflect the varying ionic strength of groundwaters, groundwater
ionic strengths within the range 10-100 mS/m shall be verified, corresponding
to the 5-95 percentile of Danish groundwaters 151.
Information on the analytical performance for the sampler analysis will be
obtained from the responsible laboratory for comparison.
Impact of other factors such as groundwater flow, well construction or
presence of other contaminants than the targets can not be ruled out and should
be considered in planning the tests for the verification.
5.5 A dditional parameters
Besides the performance parameters to be obtained by testing, compilation of
parameters describing users manual, product costs and occupational health &
safety issues of the product are required as part of the verification.
6 EXISTING DATA
A test of Sorbisense samplers, similar but earlier product version, for volatile
organic contaminants in groundwater wells has been conducted by the
laboratory used by the vendor for sampler analysis.
6.1 Summary of existing data
The summarized data as provided by the manufacturer is presented in Figure 5.
The test was set up with polyvinylchloride (PVC) pipes simulating
groundwater wells (standpipes), filled with spiked water and equipped with
Sorbisense samplers inserted directly into the water using a pipe adaptor
("pipe"), Sorbisense samplers mounted in GWS samplers ("GWS") and water
samples taken directly from the pipe ("water samples").
-------
Figure 5 Summarized data on sampler test for selected VOC as provided by the manufacturer
Test parameter
VOC Spike level:
(average of results)
VOC measuring range:
VOC recovery:
(average of results)
VOC detection limit
VOC concentration
precision:
Sotbtsense
Water Samples
0, 6, 36, 120, 3000 ug/L
GWS: 0 - 1980 ug/L
Pipe: 0 - I860 uq/L
GWS: 85 % of spiked level
Pipe: 91% of spiked level
0.2ug/V
(V= volume sampled';
GWS: 13 ,7% of mean
Pipe: 8, 9% of mean
Catulafted *wn 44 dujfcates
each
0-2160 ug/L
75% of spiked levd
0.2 ug/L
30, 5% of mean
caoi&ted Dram 44
trttfcates
3000,0
2500.0 -H
2000,0
GWS
Rpe
1:1 relation
0 500 1000 1500 2000 2500 3000
Wilier samples (ug/L)
6.2 Quality of existing data
It is not stated whether the testing and analysis were done under the
laboratory's ISO 17025 accreditation 161, the test laboratory can not be
considered independent, and the documentation made available for the
verification is not sufficient to allow for an assessment of the data quality.
6.3 Accepted existing data
It was decided that the existing data shall not be used as part of the verification
due to the data quality issues, see Section 6.2. The data will be used as an
indication of the performance range to be expected during planning.
TEST PLAN REQUIREMENTS
Based upon the application and performance parameter identification, Section
0, the requirements for test design have been set, see below. The detailed test
-------
plan is prepared separately based upon the specification of test requirements
presented below.
7.1 Test design
The outline of the required tests is shown in Table 3. The principle behind the
design is that three test scales are used: laboratory tests, standpipe tests and
field tests. Each scale is further described below and provides information on
specified performance parameters, with the smallest scale chosen for each
parameter in order to maintain simplicity and controlled conditions in the test.
Table 3 Test design scales and associated performance parameters
Laboratory
Limit of detection: best
possible
Precision and trueness: best
possible
Robustness, sampling time
and groundwater ionic
strength
Trueness of time-weighted
average concentration
Stand pipe
Limit of detection: realistic
Precision (repeatability), true-
ness and range of application
Robustness, sampling depth
None
Field
None
Precision (reproducibility)
General robustness
None
As an example of the application of the scale principle, consider the test for
evaluation of trueness and robustness. Trueness as best possible estimate is
evaluated from direct application at the laboratory scale (chloroethene only).
Trueness as realistic estimate is evaluated from the stand pipe scale simulating
a groundwater well (all but chloroethene), and the variation in trueness
between groundwater wells (robustness) is evaluated at the field scale.
Combining the scales thus provides the best possible estimates of real
conditions performance.
The laboratory tests shall apply direct application of standard solution to the
samplers (best possible) or exposure of samplers to spiked water from a sample
dispenser (robustness and trueness). The laboratory tests provides information
on the response of the samplers to carefully controlled parameters and best
possible information on the performance of the samplers with chloroethene, a
compound that can not be included in standpipe tests due to practical and
health and safety considerations.
The standpipe test is intended to simulate ground water movement through a
well established in the laboratory and to enable full control of solute
concentrations. The standpipe test provides more realistic information on the
performance of the samplers, while minimizing the variability of the test
system as compared to field systems.
The field tests shall provide information on the robustness of the sampling
system under the real conditions of groundwater investigations. In planning the
field tests, varying aquifer and well conditions should be aimed at in order to
allow for consideration of any impact of factors such as groundwater flow, well
10
-------
construction or presence of other contaminants than the targets, as well as the
impact of combined variation of robustness parameters.
7.2 Reference analysis
Reference analysis must be done under ISO 17025 accreditation 161 using a
GC-MS-SIM P&T method (EPA 624.2 or equivalent 111) and must be
documented to satisfy the analytical requirements set for groundwater
investigations in Denmark, see Table 4 and the application and performance
parameter definitions, Appendix 3.
Table 4 Required analytical quality for reference analysis
Compound
All
Limit of
detection
ug/L
0.03
Precision
5
Trueness
90-110
Range of
application
ug/L
0.03-2000
7.3 Data management
Data storage, transfer and control must be done in accordance with the
requirements of ISO 9001 /8/ enabling full control and retrieval of documents
and records. The filing and archiving requirements of the DHI Quality Manual
must be followed (10 years archiving).
7.4 Quality assurance
The quality assurance of the tests must include control of the reference system,
control of the test system and control of the data quality and integrity.
The test plan and the test report will be subject to review by the expert group as
part of the review of this verification protocol and the verification report, see
Figure 2.
As this verification is a joint verification with the US EPA ETV, auditing from
Battelle AMS Center is to be included in the test quality assurance.
7.5 Test report
The test report must follow the principles of template of the DHI NOWATECH
verification center quality manual template /4/ with data and records from the
tests presented. For this joint verification, the principles (contents) of the US
ETV format must be complied with as well.
8 EVALUATION
The evaluation includes calculation of the performance parameters, see Section
5.4 for definition, evaluation of the data quality based upon the test quality
assurance, see Section 7.4 for requirements, and compilation of the additional
parameters as specified in Section 5.5.
11
-------
8.1 Calculation of performance parameters
Calculations are done according to generally accepted statistical principles
such as those described in 191 and as described in Table 5, referring also to the
test design shown in Table 3.
Table 5 Calculations used for the test results
Parameter
Calculation
Explanations
Limit of
detection, LoD
is the Student's t factor for
f = n, - 1 degrees of freedom, n
being the number of
measurements.
2r is the standard deviation of the
measurements under repeatability
conditions
Precision
(repeatability or
reproducibility),
as relative
standard
deviation, RSD
imox imin
d = •
m
1.693
DJ is the range at level i
Xjmin and Xjmax are the lowest and
highest measurements at level i
dj is the relative range at level i
d is the mean relative range for
all m levels
Trueness, T
Tt -
T =
y
FJ^
m
x. is the mean of Sorbisense
measurements at level i, Xj
y i is the mean of reference
measurements at level i, y\
Ti is the trueness at level i
y is the true value of the analyte
T is the mean true value for all
levels
Range of
application
Visual identification of linear range,
linear regression of results within linear
range to yield slope, intercept and
coefficient of regression (r2).
Robustness
See trueness, trueness reported for
each specific parameter studied.
Robustness,
concentration
integration
'/T =
yT is the true, mean concentration
over the exposure period
q and tj are the concentrations and
exposure times for each
concentrations steps
Test of mean
against true
value
IT- e| xtfT
is Student's t-factor for
two-sided test at 95% confidence
level, n is number of
measurements and c is the true
concentration.
12
-------
Parameter
Test of mean
against mean
value
Calculation
P7-yTI_ «. ^
4
15?I
n +• ffi _ HA' - £>s + SF - y)s
nxm" n+m-2
Explanations
The test requires that the
variances are equal, v is n+m-2,
and sd is the standard deviation of
the difference between the two
means.
For field measurements, the reference measurements will be used as the true
values.
For laboratory and standpipe measurements, concentrations obtained from
preparation of the matrices are checked against the reference measurements
(reference samples). If preparation based concentrations match the reference
measurements, mean trueness within 100% ± 2 x RSD (relative standard
deviation), these are used as true values for the test measurements. If not, the
reference measurements are used as the true values.
Calculations will be performed in Excel 2007 set up for the purpose with the
equations required.
8.2 Evaluation of test data quality
The information of the test report on the reference system, the test system and
data quality and integrity control will be evaluated against the requirements set
in this protocol and the objectives set in the test plan.
The spreadsheet used for the calculations will subject to control on a sample
basis (spot validation).
The external audit reports prepared by Battelle AMS Center, see Section 7.4,
will be evaluated and major findings compiled and reported.
8.3 Compilation of additional parameters
8.3.1 User manual
The verification criterion for the users manual is that it describes the use of the
samplers adequately and understandable for the typical sampler and sampling
planner. This criterion is evaluated through evaluation of a number of specific
points of importance, see Table 6 for the parameters to include.
A description is complete, if all essential steps are described, if they are
illustrated with a figure or a photo, where relevant, and if the descriptions are
understandable without reference to other guidance.
13
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Table 6 Criteria for user manual evaluation
Parameter
Product
Principle of operation
Intended use
Performance expected
Limitations
Preparations
Unpacking
Transport
Assembly
Installation
Function test
Operation
Steps of operation
Points of caution
Accessories
Maintenance
Trouble shooting
Safety
Chemicals
Power
Complete
description
Summary
description
No
description
Not relevant
V
V
8.3.2 Product costs
The capital investment costs and the operation and maintenance cost will be
itemized based upon a determined design basis /10/, see Table 7 for the items
that will be included.
Table 7 List of capital cost items and operation and maintenance cost items per product unit
(sample)
Item type
Capital
Site preparation
Buildings and land
Equipment
Utility connections
Installation
Start up/training
Permits
Operation and maintenance
Materials, including chemicals
Utilities, including water and energy
Labor
Waste management
Permit compliance
Item
Number
None
14
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The design basis will be described and the cost items relevant for the
Sorbisense sampler listed. Note that the actual costs for each item is not
compiled and reported.
8.3.3 Occupational health and environment
The risks for occupational health and safety and for the environment associated
with the use of the product will be compiled. The compilation will list
chemicals used during product operation and classified as toxic, T, or very
toxic, Tx, for human health and/or very environmentally hazardous (N)
according to /I I/. The information will be given as amount used per product
unit (sample), see Table 8 for format.
Table 8 Compilation of classified chemicals used during product operation
Compound
CAS number
Classification
Amount used per product
unit
Additional risks from installing, operating and maintaining the product will be
evaluated, compiled and reported, if relevant. In particular, risks for human
health associated with power supply and danger of infections will be
considered.
VERIFICATION SCHEDULE
The verification is planned for 2008-9. The overall schedule is given in Table
9.
Table 9 Verification schedule
Task
Application definition document
Verification protocol with test plan
Test
Test reporting
Verification
Verification report
Report document review
Verification statement
Timing
May 2008
November 2008 to January
2009
January to March 2009
March 2009
March 2009
March 2009
April 2009
April 2009
10 QUALITY ASSURANCE
The quality assurance of the verification is described in Table 10 and Figure 2,
and the quality assurance of the tests in the test plan but summarized here, as
well as in the process document 111.
15
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Table 10QA plan for the verification
Initials
Tasks
Plan document
with verification
protocol and test
plan
Test system
Report
document with
test report and
verification
report
DHI
ALJ
Review
-
Review
LSC
Audit
Battelle AMS
Center
ZW
Audit
US EPA
ETV
LD, JMK,
EH
Review
-
Review
Expert
Group
CP, DM,
MS
Review
-
Review
Internal review of plan and report documents is done by chief engineer Anders
Lynggaard Jensen (ALJ), and test system audit (see test plan) is done following
the GLP audit procedure by a trained auditor: head of laboratory products
Louise Schluter (LSC).
The Battelle quality manager, Zachary Willenberg (ZW), will perform a
technical systems audit (TSA) during this verification and test.
EPA QA staff, Lauren Drees (LD), John McKernan (JMK) and Evelyn Hartzell
(EH) will do review of the plan and report documents.
The expert group will do review of the plan and report documents.
Reviews will be done using the NOWATECH review report template.
16
-------
APPENDIX 1
Terms and definitions used in the verification protocol
17
-------
The abbreviations and definitions used in the verification protocol and the test
plan are summarized below.
Where discrepancies exist between NOWATECH and US EPA ETV
terminology, definitions from both schemes are given.
Word
ADQ
AMS Center
Analysis
Analytical
laboratory
Application
A-UBA
BTEX
CEN
CWA
DHI WMC
Direct
application
DOC
Drinking water
control
DS
Effect
EN
ETV
EU
Evaluation
NOWATECH
Audit of data quality: An examination
of a set of data after is has been
collected and 1 00% verified by
project personnel, consisting of
tracing at least 1 0% of the test data
from original recording through
transferring, calculating, summarizing
and reporting.
Advanced Monitoring Systems
Center at Battelle
Analysis of Sorbisense samplers at
the vendor identified laboratory
Independent analytical laboratory
used to analyze reference samples
The use of a product specified with
respect to matrix, target, effect and
limitations
Umweltbundesamt Austria
Benzene, toluene, ethylbenzene and
xylenes
European Committee for
Standardization
CEN Workshop agreement
(ETV) Water Monitoring Center at
DHI
A test design where a standard
solution is applied directly to the
Sorbisense samplers
Dissolved organic carbon
Control of drinking water quality
against drinking water maximum
concentrations.
Danish Standard
The way the target is affected, in this
verification the way the target
compounds are measured
European standard
Environmental technology verification
(ETV) is an independent (third party)
assessment of the performance of a
technology or a product for a
specified application, under defined
conditions and adequate quality
assurance.
European Union
Evaluation of test data for a
US ETV
EPA program that develops generic
verification protocols and verifies the
performance of innovative
environmental technologies that have
the potential to improve protection of
human health and the environment
An examination of the efficiency of a
18
-------
Word
Experts
GC
Groundwater
investigation
Groundwater
monitoring
GWS
ISO
Laboratory
sample
dispenser
Limit of
detection
LoD
Limit of
quantification
LoQ
Matrix
mbgv
mbs
Method
MS
MTBE
NOWATECH
ETV
P&T
PE
Performance
claim
Performance
parameters
Precision
NOWATECH
technology product for performance
and data quality
Independent persons qualified on a
technology in verification or on
verification as a process
Gas chromatography
Investigation of groundwater
contamination with measurements
controlled against groundwater
maximum concentrations.
Baseline monitoring of groundwater
quality.
Groundwater sampler
International Standardization
Organization
Test device designed for controlled
exposure of Sorbisense samplers to
test solutions.
Calculated from the standard
deviation of replicate measurements
at less than 5 times the detection
limit evaluated. Corresponding to
less than 5% risk of false blanks.
Calculated from the detection limit,
typically 3 times the LoD, the
concentration, where the blank
variation impacts the precision 20%.
The type of material that the product
is intended for
m below groundwater table
m below surface
Generic document that provides
rules, guidelines or characteristics for
tests or analysis
Mass spectrometry
Methyl-fe/f-butylether
Nordic Water Technology Verification
Centers
Purge and trap
Performance evaluation: A
quantitative evaluation of a
measurement system, usually
involving the measurement or
analysis of a reference material of
known value or composition
The effects foreseen by the vendor
on the target (s) in the matrix of
intended use
Parameters that can be documented
quantitatively in tests and that
provide the relevant information on
the performance of an environmental
technology product
The standard deviation obtained from
replicate measurements, here
measured under repeatability or
US ETV
technology
Peer reviewers appointed for a
verification
19
-------
Word
(Environmen-
tal) product
PVC
QA
Range of
application
Reference
analyses
Reference
samples
Repeatability
Reproducibility
Robustness
RSD
Sampler
Samples
Sampling
system
SIM
SM
Stakeholder
Standard
NOWATECH
reproducibility conditions.
Ready to market or prototype stage
product, process, system or service
based upon an environmental
technology
Polyvinylchloride
Quality assurance
The range from the LoD to the
highest concentration with linear
response,
Analysis by a specified reference
method in an accredited (ISO 17025)
laboratory.
Samples taken for and analyzed by a
specified reference method in an
accredited (ISO 17025) laboratory.
The precision obtained under
repeatability conditions, that is with
the same measurement procedure,
same operators, same measuring
system, same operating conditions
and same location, and replicate
measurements on the same
or similar objects over a short period
of time
The precision obtained under
reproducibility conditions, that is with
measurements that includes different
locations, operators, measuring
systems, and replicate
measurements on the same or
similar objects
% variation in measurements
resulting from defined changes in
matrix properties.
Relative standard deviation in %.
Sorbisense sorbent cartridge
Samples taken with and analyzed
after the Sorbisense method.
The sampling reservoir and venting
system used to operate the
Sorbisense samplers
Selected ion monitoring
Standard Methods for the
Examination of Water and
Wastewater, latest edition
Generic document established by
US ETV
(Environmental) technology
Buyers and users of technology,
technology developers/vendors, the
consulting engineers, the finance and
export communities, government
permitters, regulators, first
responders, emergency response,
disaster planners, public interest
groups, and other groups interested
in the performance of innovative
environmental technologies.
20
-------
Word
Stand pipe
Target
(Environmenta
1) technology
Test/testing
Trueness
ISA
US EPA
Vendor
Verification
VOC
VOX
WS
NOWATECH
consensus and approved by a
recognized standardization body that
provides rules, guidelines or
characteristics for tests or analysis
Test device designed to simulate a
groundwaterwell
The property that is affected by the
product, in this verification the target
compounds measured.
The practical application of
knowledge in the environmental area
Determination of the performance of
a product by parameters defined for
the application
The % recovery of true value
obtained either from knowledge on
the preparation of test solutions or
from measurements with reference
methods.
Technical system audit
United States Environmental
Protection Agency
The party delivering the product or
service to the customer
Evaluation of product performance
parameters for a specified application
under defined conditions and
adequate quality assurance
Volatile organic compounds, here the
compounds listed as target
compounds/analytical parameters
Volatile halogenated organic
compounds, here the halogenated
compounds listed as target
compounds/analytical parameters
Workshop (under CEN)
US ETV
An all-inclusive term used to describe
pollution control devices and
systems, waste treatment processes
and storage facilities, and site
remediation technologies and their
components that may be utilized to
remove pollutants or contaminants
from, or to prevent them from
entering, the environment.
The technology developer, owner, or
licensee seeking verification
Establishing or proving the truth of
the performance of a technology
under specific, predetermined
criteria, test plans and adequate data
QA procedures
21
-------
A P P E N D IX 2
References
22
-------
1. Gran, C. Sorbisense GWS40 Passive Sampler. Verification protocol. 2009.
2. Battelle. Process Document for US EPA ETV AMS Center and NOWATECH DHI WMC Joint
Verification of the Sorbisense Ground Water Sampler. 2009.
3. Battelle. Quality management plan (QMP) for the ETV Advanced Monitoring Systems Center.
Version 7.0. 17-11-2008.
4. NOWATECH. Verification test center quality manual. 2008.
5. Leerke Thorling. Data extract from the Danish Groundwater Monitoring Programme. 21-5-2008.
6. ISO. General requirements for the competence of testing and calibration laboratories. ISO 17025.
2005.
7. US EPA. Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas
Chromatography/Mass Spectrometry. Method 624.2. 1995.
8. International Standardization Organisation. EN ISO 9001. Quality management systems -
Requirements. 15-11-2008.
9. ISO. Accuracy (trueness and precision) of measurement methods and results - Part 1. ISO 5725-1.
2004.
10. Gavaskar, A. and Gumming, L. Cost Evaluation Strategies for Technologies Tested under the
Environmental Technology Verification Program. 2001. Battelle.
11. European Commission. Commission Directive on classification, packaging and labelling of
dangerous substances. 2001/59/EC. 2001.
12. The Environment Agency's Monitoring Certification Scheme. Performance standards and test
procedures for portable water monitoring equipment. 2008.
13. ISO. Water Quality - On-line sensors/analysing equipment for water - Specifications and
prerformance tests. ISO 15839. 2006.
14. International Standardization Organisation. Water quality - Guide to analytical quality control for
water analysis. ISO 13530. 1998.
15. Battelle Advanced Monitoring Systems Center. Test/QA Plan for Verification of Enzymatic Test
Kits. Environmental Technology Verification Program . 21-9-2005.
16. Sandia National Laboratories. Ground Water Sampling Technologies Verification Test Plan.
U.S.Environmental Protection Agency.
Environmental Technology Verification Program . 1999.
17. EU Kommisionen. Commission directive laying down, pursuant to Directive 2000/60/EC of the
European Parliament and of the Council, technical specifications for chemical analysis and
monitoring of water status. Draft. 2008.
23
-------
18. International Standardization Organisation. Water quality — Vocabulary — Part 2. ISO 6107-2.
1-5-2006.
19. European Parliament and Council. Directive 2006/118/EC of the European Parliament and of the
Council of 12 December 2006 on the protection of groundwater against pollution and deterioration.
12-12-2006.
20. European Council of Ministers. Council Directive 98/83/EC of 3 November 1998 on the quality of
water intended for human consumption. Council Directive 98/83/EC. 3-11-1998.
21. Miljeministeriet. Bekendtgorelse om kvalitetskrav til miljomalingerudfert af akkrediterede
laboratorier, certificerede personer m.v. Bekendtgerelse 1353. 2006.
22. Jergensen, C., Boyd, H. B., Fawell, I, and Hydes, O. Establishment of a list of chemical
parameters for the revision of the Drinking Water Directiv. 2008.
23. Miljestyrelsen. Liste over kvalitetskriterier i relation til forurenet jord. 1-12-2005.
24. Danmarks Miljeundersegelser. Liste over miljefremmede staffer i NOVANA.
http://www.dmu.dk/NR/rdonlvres/A1758992-D52E-4C73-8701-
BC1C8D25791D/0/MFS stofliste20070807.pdf. 7-8-2007.
25. Sandia National Laboratories. ETV joint verification statement - GORE-SORBER water quality
monitoring. 2000. US EPA.
26. Parker, L. V. and Clark, C. H. Study of Five Discrete Interval-Type Groundwater Sampling
Devices. 2002. US Army Corps of Engineers.
27. US Geological Survey, Naval Facilities Engineering Service Center, and Battelle. Demonstration
and validation of a regenerated cellulose dialysis membrane diffusion sampler for monitoring
groundwater quality and remediation progress at DoD sites. 18-4-2006.
24
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A P P E N D IX 3
Application and performance parameter definitions
25
-------
This appendix defines the application and the relevant performance parameters
application as input for verification and test of an environmental technology
following the NOWATECH ETV method.
1 Applications
The intended application of the product for verification is defined in terms of
the matrix, the targets and the effects of the product.
The Sorbisense GWS40 passive sampling system with samplers (cartridges)
and analysis of the samplers is provided by the vendor as one product, and the
verification shall accordingly see these two investigation steps as one.
1.1 Matrix/matrices
The matrix of the application is groundwater and the field of application is
investigations on (potentially) contaminated groundwater (groundwater
investigations). In groundwater investigations, the groundwater composition
generally varies considerably, and the pressure on samplers will vary with
depth to the sampling positions. The varying ionic strength, contaminant
concentration and water pressure may impact the performance and this impact
shall be evaluated as part of the verification.
1.2 Target(s)
The targets of the application are volatile organic contaminants, here mono-,
di-, tri- and -tetrachloroethenes, BTEX and MTBE. Investigations of
contaminated groundwater generally include both uncontaminated and strongly
contaminated groundwater. The concentrations verified shall accordingly
reflect the range from uncontaminated groundwater to highly contaminated
groundwater. With the claimed application at sampling depths from 0.5 mbs to
5 mbs (m below surface), pressure variation in the range 1-1.5 atmosphere shall
be verified. Furthermore, with the claimed application, groundwater ionic
strengths within the range 10-100 mS/m shall be verified, corresponding to the
5-95 percentile of Danish groundwaters 151.
1.3 Effects
The effects for the application are generally reported in terms of limit of
detection (LoD), precision, trueness, range of application and robustness. The
effects claimed by the vendor are given in Appendix table 1 for all target
compounds.
The robustness is the change in trueness within the range of application for
defined variations in water pressure, contaminant concentration, groundwater
ionic strength and sampling time.
26
-------
Appendix table 1 Vendor claim of performance, general terms
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
Limit of
detection
M9/L
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
1
Precision
%
<20
<20
<20
<20
<20
<20
<20
<20
<20
<20
Trueness
%
>80
>80
>80
>80
>80
>80
>80
>80
>80
>80
Range of
application
ljg/L
LoD-2000
LoD-2000
LoD-2000
LoD-2000
LoD-2000
LoD-2000
LoD-2000
LoD-2000
LoD-2000
LoD-2000
Robustness
%
100±30
100±30
100±30
100±30
100±30
100±30
100±30
100±30
100±30
100±30
1.4
Exclusions
Passive sampling at waste disposal sites is excluded from the defined
application and is thus not covered by the verification, as the conditions with
respect to ionic strength and DOC are outside the ranges covered by the
verification conditions. Groundwater baseline monitoring and drinking water
control are excluded as well, as the passive sampler will not satisfy the
detection limit requirements for this purpose, see Chapter 0.
2 General performance Requirements
No formal performance requirements for the application have been identified in
the European Union or the US.
The conventional performance parameters of analytical and monitoring
methods and equipment are limit of detection (LoD), precision (repeatability
and reproducibility), trueness, specificity, linearity and matrix sensitivity. The
uncertainty of measurements may be used to summarize the performance.
Parameters may be added to characterize e.g. on-line or on-site monitoring
instruments. The listed parameters cover the requirements set or implemented
in international standards and by testing and verification operators 112-161.
2.1 Regulatory requirements
The general requirement for analytical quality in water monitoring in Europe
will be established with the adoption of the Commission Directive on technical
specifications for chemical analysis and monitoring of water status 111/
requiring not more than 25% relative standard deviation at the level of the
relevant water quality standards. The limit of quantification, LoQ, must be at or
below 30% of the relevant water quality standard (WQS), corresponding to a
limit of detection at or below 10% of the WQS. The LoQ is as defined in ISO
6107-2: 2006 /18/. The Groundwater Directive 1191 only sets an absolute
requirement for monitoring of tri- and tetrachloroethene during groundwater
27
-------
monitoring without stating the water quality standard and the quality
requirement.
The European Directive on drinking water /20/ defines performance
requirements for methods used for control of drinking water quality for the
VOCs benzene, tri- and tetrachloroethene, among others. These values cover
the chemical analysis only, and quality requirements for drinking water control
would mostly be seen as stricter than for groundwater investigations. The
drinking water based performance requirements for analysis only should
therefore be seen as strict compared to groundwater monitoring including also
sampling, see Appendix table 2.
Appendix table 2 Regulatory requirements from the European drinking water directive
Compound
Trichloroethene
Tetrachloroethene
Benzene
Limit of
detection
M9/L
1
1
0.25
Precision
%
25
25
25
Trueness
%
75-125
75-125
75-125
Range of
application
ug/L
1
-
-
Robustness
%
-
-
-
The Monitoring Certification Scheme of the British Environment Agency does
not provide performance standards for groundwater or drinking water
monitoring/127.
Danish statute on quality requirements for environmental control 1211 specifies
the requirements for control and monitoring of mono-, di-, tri- and -
tetrachloroethenes and benzene in groundwater as shown in Appendix table 3.
The detection limits stated are not justified by the maximum concentrations for
groundwater, except for for chloroethene, see Section 2.2.
Again, it should be noted that the requirements cover analysis only and must
thus be seen as stricter than required for methods including sampling.
Appendix table 3 Regulatory requirements for groundwater monitoring and control from the
Danish analytical quality requirement statute
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Limit of
detection
M9/L
0.03
0.03
0.03
0.03
0.03
0.03
Precision
%
5
5
5
5
5
5
Trueness
%
100±10"
100±10
100±10
100±10
100±10
100±10
Range of
application
M9/L
-
-
-
-
-
-
Robustness
%
-
-
-
-
-
-
2.2 Application based requirements
The application of the samplers in groundwater investigations further defines
performance requirements in terms of the contaminant concentrations
1 -: no requirement
2 Assuming a 5% relative standard deviation
28
-------
monitored and controlled during investigations in general. The lower limit of
concentrations to be monitored will in most cases be defined by the
groundwater maximum concentrations (and as a lower limit the drinking water
maximum concentrations) for the compounds in question, see Appendix table
4.
Appendix table 4 Summary of groundwater and drinking water maximum concentrations, as
summarized in /22/ and /23/
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
Groundwater
Denmark
ug/L
0.2
1
1
1
1
1
5
-
5
2-5
EU
ug/L
0.5
-
-
10
10
1
-
-
-
-
Drinking water
US
ug/L
2
7
70-100
5
5
5
1000
100
10*10J
20-40
WHO
ug/L
0.3
30
50
70
40
10
700
300
500
-
A general requirement for the limit of detection of 1/10 of the maximum
concentration is applied widely, and the derived limits of detection are
compiled in Appendix table 5. Required detection limits for both drinking
water and groundwater control are in the same ranges in Austria.
For the Danish groundwater monitoring program (GRUMO), requirements for
detection limits are as given in Appendix table 5 7247. It should be noted, that
the detection limits required here for groundwater monitoring do not comply
with those required in Danish statute on quality requirements for environmental
control 7217 covering also monitoring of the compounds in groundwater as
shown in Appendix table 5.
Appendix table 5 Summary of detection limit requirements derived from the groundwater and
drinking water maximum concentrations and for the Danish groundwater
monitoring programme, 2003
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
Groundwater
maximum
concentration
based
Denmark
ug/L
0.02
0.1
0.1
0.1
0.1
0.1
0.5
-
0.5
0.2
Drink
CO
EU
ug/L
0.05
-
-
1
1
0.1
-
-
-
-
[ing water ma.
ncentration be
US
ug/L
0.2
0.7
7
0.5
0.5
0.5
100
10
1000
2
Kimum
ised
WHO
ug/L
0.03
3
5
7
4
1
70
30
50
-
Groundwate
r monitoring
based
Denmark
ug/L
0.05
-
-
0.02
0.02
0.04
0.04
-
0.02
-
29
-------
Application based requirements for trueness and precision have generally not
been stated to the same degree as for the limits of detection, mainly because
regulatory compliance rules in most cases do not consider the uncertainty of
control results.
No requirements for range of application and robustness have been identified.
In practical performance of site investigations, the dissolved concentrations
range from below detection limit to the limit of solubility. The upper limit of
concentrations to be monitored will thus in most cases be defined by the
solubilities of the target compounds are summarized in Appendix table 6.
Appendix table 6 Summary of target compound solubilities
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
Water solubility
M9/L
2.8*10b
3.3*1 Ob
3.5-6.3*1 Ob
1.4*10b
0.24*1 Ob
1.8*10b
0.55*1 Ob
0.1 7*1 Ob
0.1 6-0.20*1 Ob
1.8*10b
3 State of the art performance
Whereas a broad range of studies on the performance of analytical methods and
sampling methods for VOC in groundwater have been published, independent
and comparative studies of passive samplers used for VOC monitoring in
groundwater are scarce. Examples of reported performances (sampling and
analysis) are compiled in Appendix table 7.
Appendix table 7 Summary of state of the art performance for passive samplers
Sampler
GORE-
SORBER
USGS PDB
Dialysis
membrane
sampler
USGS PDB
Limit of
detection
ugTL
-
-
0.1-5
Precision
%
14-21
0.9-4.3
17
21
Trueness
%
-
86-118
100%
Range of
applicatio
n3
ug/L
5-2000
2-500
0.2-25*1 03
Robustne
ss
%
-
-
-
Reference
/25/
7267
1211
Reported performance (sampling and analysis) as obtained with reference sampling is given in
Appendix table 8.
Verified range of application, practical range may differ
30
-------
Appendix table 8 Summary of state of the art performance for reference samplers
Sampler
Grab sampling
Grab sampling
Low purge
pump sampling
Limit of
detection
ug/L
-
-
-
Precision
%
12%
1.1-9.8
15
Trueness
%
-
-
-
Range of
applicatio
n
ug/L
5-2000
2-500
0.2-25*1 03
Robustne
ss
%
-
-
-
Reference
1251
I2&I
1211
The precision results obtained with the passive samplers do not greatly differ
from the precision values obtained with reference sampling methods. As the
precision data obtained with the reference methods will generally be accepted
for groundwater monitoring and control, the precision data obtained with the
passive samplers should also be considered acceptable.
4 Performance parameter definitions
The statement of regulatory and application based requirements in terms of the
analytical quality rather than the combined quality of analysis and sampling, as
relevant for passive samplers, makes the identification of relevant criteria
difficult for passive samplers.
Only a limited number of studies on the contributions of sampling and analysis,
respectively, to the limit of detection, precision and trueness of groundwater
monitoring and control have been published. Therefore, the regulatory and
application based requirements needs identified for analytical performance can
not be directly translated into the combined sampling and analysis performance
requirements relevant for passive samplers.
The discrepancies between requirements based upon different approaches when
comparing Appendix table 2, Appendix table 3 and Appendix table 5, further
hampers the identification of relevant criteria.
Therefore, relevant performance parameters for the application are set in
Appendix table 9 based upon regulatory and application based requirements
and state of the art performance.
In order to address the general definition of performance parameters in terms of
analytical quality only, information on this using the sampler should be
obtained from the responsible laboratory for comparison, if possible.
In addition to the straight forward performance parameters of limit of
detection, precision, trueness and range of application, the robustness shall be
31
-------
tested for the critical parameters identified here: variations in water pressure,
contaminant concentration, groundwater ionic strength and sampling time.
Appendix table 9 Relevant ranges of performance parameters for groundwater investigations
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
Limit of
detection
M9/L
0.02-0.05
0.1-1
0.1-1
0.1-1
0.1-1
0.1-1
0.5-5
0.5-5
0.5-5
0.2-2
Precision
%
<25
<25
<25
<25
<25
<25
<25
<25
<25
<25
Trueness
%
75-125
75-125
75-125
75-125
75-125
75-125
75-125
75-125
75-125
75-125
Range of
application
M9/L
LoD-1*10b
LoD-1*10b
LoD-1*10b
LoD-1*10b
LoD-0.1*10b
LoD-1*10b
LoD-0.1*10b
LoD-0.1*10b
LoD-0.1*10b
LoD-1*10b
Robustness
%
85-115
100±25
100±25
100±25
100±25
100±25
100±25
100±25
100±25
100±25
32
-------
NOWATECH
Nordk Innovation Ccntie
Baflelie
\\M il'.iiiinmr ^ Eanordtii
Sorbisense GWS40 Passive Sampler
Joint test plan
Volatile organic compounds in groundwater
-r
January 2009
Version approved
-------
Sorbisense GWS40 Passive Sampler
Joint test plan
Agern Alle 5
DK-2970 H0rsholm
Denmark
Tel: +4545169200
Fax: +4545169292
dhi@dhigroup.com
www.dhigroup.com
Vendor
Sorbisense ApS
Vendors representative
Hubert de Jonge
Project
Nordic Water Technology Verification Centers
Authors
Gerald Heinicke
Mette Tjener Andersson
Revision
Joint test plan
Description
Key words
Environmental technology verification, passive
sampler, groundwater
Project No
80144
Date
January 2009
Approved by
GHE CHG CHG
By Checked Approved Date
Classification
£3 Open
n Internal
n Proprietary
Distribution
Sorbisense
DHI
UBA-A
Battelle
US EPA
HdJ
CHG, GHE, MTA
DM
AMG, ZJW
LD
No of copies
File distribution
only
-------
1 TABLE OF CONTENTS
1 TABLE OF CONTENTS
2 INTRODUCTION 1
2.1 Verification protocol reference 1
2.2 Name and contact of vendor 1
2.3 Name of center/test responsible 1
2.4 Expert group 2
3 TEST DESIGN 2
3.1 Test sites 5
3.1.1 Types 5
3.1.2 Addresses 5
3.1.3 Descriptions 5
3.2 Tests 5
3.2.1 Test methods 6
3.2.2 Test staff 8
3.2.3 Test schedule 9
3.2.4 Test equipment 9
3.2.5 Type and number of samples 9
3.2.6 Operation conditions 11
3.2.7 Operation measurements 11
3.2.8 Product maintenance 11
3.2.9 Health, safety and wastes 11
4 REFERENCE ANALYSIS 12
4.1 Analytical laboratory 12
4.2 Analytical parameters 12
4.3 Analytical methods 12
4.4 Analytical performance requirements 13
4.5 Preservation and storage of reference samples 13
5 DATA MANAGEMENT 13
5.1 Data storage, transfer and control 13
6 QUALITY ASSURANCE 14
6.1 Test plan review 14
6.2 Performance control - reference analysis 14
6.3 Test system control 15
6.4 Data integrity check procedures 16
6.5 Test system audits 16
6.6 Test report review 17
7 TEST REPORT 17
7.1 Test site report 17
7.2 Test data report 17
7.3 Amendment report 17
7.4 Deviations report 17
-------
APPENDIX 1 19
Terms and definitions used in the test plan 19
APPENDIX 2 24
Reference methods and references 24
APPENDIX 3 27
In-house test methods 27
APPENDIX 4 46
In-house analytical methods 46
APPENDIX 5 48
Data reporting forms 48
APPENDIX 6 89
Data management 89
APPENDIX 7 95
Deviations and amendments 95
-------
2 INTRODUCTION
This joint test plan is the implementation of a test design de-
veloped for verification of the performance of an environ-
mental technology following the NOWATECH ETV method.
The verification is a joint verification with the US EPA ETV
scheme and the Advanced Monitoring Systems Centre, Bat-
telle, see the verification protocol III for details on organiza-
tion and implications. The compliance of the test with both
scheme's requirements is ensured through a process docu-
ment 111.
2.1 Verification protocol reference
This test plan is prepared in response to the test design estab-
lished in the Sorbisense GWS40 Passive Sampler, verifica-
tion protocol, Volatile organic compounds in groundwater,
Version final draft, December 2008 III.
2.2 Name and contact of vendor
Sorbisense A/S, Niels Pedersens Alle 2, DK-8830 Tjele,
Denmark, phone +45 8999 2505, +45 8999 2599.
Contact: Hubert de Jonge, e-mail hubert@sorbisense.com.
The laboratory responsible for the analysis of samples (sub-
contractor to the vendor) is: ALcontrol Laboratories, Steen-
houwerstraat 15, 3194 AGHoogvliet, Netherlands,
Contact: Jaap Willem Hutter, e-mail j.hutter@alcontrol.nl
2.3 Name of center/test responsible
NOWATECH Water Monitoring ETV Center , DHI, Agern
Alle 5, DK-2970 H0rsholm, Denmark.
Test responsible: Gerald Heinicke, e-mail
ghe@dhigroup.com, phone +45 95 16 92 68, mobile +45 29
91 07 15.
US EPA Advanced Monitoring System Center, Battelle Me-
morial Institute, 505 King Avenue, Columbus, Ohio 43201-
2693, US.
Test responsible: Anne M. Gregg (AMG), e-mail
gregga@battelle.org, phone +1 614-424-7419
-------
2.4 Expert group
The expert group assigned to this test and responsible for re-
view of test plan and test report includes:
Dietmar Miiller (DM), e-mail
dietmar.mueller@umweltbundesamt.at Contaminated Sites,
Umweltbundesamt, Spittelauer Lande 5, 1090 Wien, Austria,
phone+43-(0)1-313 04/5913
Mike Sherrier (MS), e-mail
michael.p.sherrier@usa.dupont.com, DuPont, Barley Mill
Plaza, Bldg 19-1132, 4417 Lancaster Pike, Wilmington, DE
19805, US, phone +1 302-892-1168
Cynthia Paul (CP), e-mail paul.cindy@epa.gov, U.S. Envi-
ronmental Protection Agency, 919 Kerr Research Drive, P.O.
Box 1198. Ada, OK 74820, US, phone: +1 580-436-8556.
TEST DESIGN
The test design outlined in the test protocol is summarized in
Table 1. The term "samples" is used for samples taken with
the Sorbisense sampler, whereas the term "reference sam-
ples" is used for water samples taken for reference analysis.
Acronyms are explained in Appendix 1.
If nothing else is stated below, the standard conditions for the
stand pipe include mid range ionic strength (30-70 mS/m
conductivity), a sampling period of 6 days and a sampling
depth of 0.5 m (0.05 atm overpressure).
In Table 1, labels are given for each experiment and for ex-
periments with different levels, a new label is given for each
level.
-------
Table 1 Test design
Performance parameters
Limit of detection (LoD)
Precision (repeatability
and reproducibility)
Range of application
Trueness
Robustness, general
Robustness, specific
Reference for the robust-
ness test levels
Sampling depth
Ionic strength
Laboratory1
Direct application to samplers of VOX
standard dilution in 7 replicates in the
range LoD-5 x LoD.
Triplicate analysis of VOX standard dilu-
tion.
Exp. H
Direct application in 7 replicates to
samplers of VOX standard at 1 0% of
range.
Exp. L
Triplicate samples at 1 spiked 50%
range VOC concentration4, 1 mid range
ionic strength (35 mS/m) and 1 mid
range sampling time (6 days) from the
sample dispenser. Three reference
samples distributed over the sampling
period.
Exp. BA
n.a.
Triplicate samples at 1 spiked mid
range VOC concentration, 2 ionic
strengths (10 and 100 mS/m), (6 days),
Stand pipe2
7 replicate samples in the range
LoD-5 x LoD, spiked cone.
7 reference samples distributed
over the sampling period.
Exp. J
Triplicate samples and three ref-
erence samples, the later distrib-
uted over the sampling period,
each at 5 spiked VOC cone.
10,25,50,75, 100% of range
Exp. N, P, R, T, V
Precision test above.
Triplicate samples at 1 spiked
VOC mid range concentration,
0.5 atm. overpressure.
Three reference samples distrib-
uted over the sampling period.
Exp. CA
n.a.
Field
n.a.3
Single samples and reference
samples at three (Sorbisense) or
four (reference) times from a total
of 5 wells at 1-3 sites, inherent
concentrations.
Exp. AA, AB, AC, AD, AE
n.a.
n.a.
n.a.
1 Direct application is done with chloroethene and the other chlorinated compounds, but without the BTEX and MTBE in the standard, other ex-
periments are done with the full VOC set without chloroethene
2 Standpipe experiments are done with the full VOC set without chloroethene
3 n.a.: not applicable
4 from pure chemicals, without chloroethene
-------
Performance parameters
Laboratory1
Stand pipe
Field
from the sample dispenser.
Three reference samples distributed
over the sampling period for each ionic
strength.
Exp. DA, EA
Sampling time
Triplicate samples at 1 spiked VOC mid
range concentration, mid range ionic
strength and 2 sampling times (3 and 9
days), from the sample dispenser.
Three reference samples distributed
over the sampling period for each sam-
pling time.
Exp. FA, GA
n.a.
n.a.
Concentration integration
Triplicate samples at a step VOC con-
centration, 3 concentrations (20, 50 and
80 % of range), each at 1/3 of 6 days
sampling period, from the sample dis-
penser.
Three reference samples distributed
over the sampling period.
Exp. HA
n.a.
n.a.
-------
3.1 Test sites
Both the laboratory tests and the standpipe tests will be conducted in the DHI labora-
tory buildings, H0rsholm, Denmark.
The field tests will be carried out on contaminated groundwater sites in the Copenha-
gen area.
3.1.1 Types
The test sites are summarized in Table 2.
Table 2 Summary of test sites
Scale
Laboratory
Standpipe
Field
Address/site
DHI premises
DHI premises
S0borg hovedgade, S0borg
S0borg hovedgade, S0borg
S0borg hovedgade, S0borg
Farum Bytorv, Farum
R0de Vejrm0lle, Roskildevej, Al-
bertslund
Site de-
tails
None
None
AFV6
AFV4
B109
AFV1
K4
VOC profile for test
All target compounds
All target compounds
All target compounds
All target compounds, low cone.
Chlorinated solvents
BTEX + MTBE, high concentrations
BTEX + MTBE, intermediary concen-
trations
Please, note that the field test sites are preliminary and may change after site data
compilation and inspections. Changes will be documented by an amendment to this
document.
3.1.2 Addresses
See Table 2.
3.1.3 Descriptions
See Table 2.
3.2 Tests
The test program has been prepared to provide the information and to apply the ap-
proaches presented for analytical quality control for water analysis (ISO 13530) /3/
and for performance test of on-line sensors/analysing equipment (ISO 15839) /4/. The
field tests have been prepared to comply with the test requirements in the Cost Agree-
ment (pre-standard) on verification of monitoring technologies for groundwater site
characterization (CEN/WS 32:2008) 151.
The test design, as described in Table 1, includes three test scales: laboratory, stand
pipe and field.
For chloroethene (vinyl chloride), the performance is only tested in a simplified labo-
ratory design (direct application, best possible LoD, repeatability precision and true-
ness) and in the field (worst realistic reproducibility precision and robustness) due to
difficulties preparing, obtaining and handling chloroethene solutions.
-------
3.2.1 Test methods
No standard methods exist for testing of passive samplers for groundwater monitoring.
The test methods have accordingly been prepared for the purpose (see Appendix 3),
with reference to the Ground Water Sampling Technologies Verification Test Plan
prepared for the US EPA ETV program 161. Preparation of test solutions, reagents and
chemicals are described in Appendix 3 as well. It should be noted that the methods in
Appendix 3 are described at the detailed level of a work instruction for direct imple-
mentation in the laboratory.
For standpipe tests, groundwater, see Appendix 3.7, was used for preparing test solu-
tions, and for laboratory tests, (clean) water, also see Appendix 3.7, was used. All dilu-
tions were prepared in water.
For the laboratory and standpipe tests, custom-made stainless steel test devices have
been being prepared, see below.
For direct application laboratory tests, a standard solution with chlorinated compounds
only is applied to the samplers directly with a syringe, followed by equilibration and
flushing with water using the sample dispenser, see Appendix 3.1 for method descrip-
tion (no illustration).
For the laboratory tests, a sample dispenser device, Figure 1, is designed as a closed
system that enables direct exposure of samplers to test solutions with known and sta-
ble VOC concentrations by conveying the test solution from a closed container by
gravity, see Appendix 3.2. The container is equipped with spiking port, sampling port
and magnetic stirrer to maintain homogeneous conditions in the sample container.
Figure 1 Sample dispenser
£
Samplinq oort
'«*: 11 h _5 ~™ w o y valve
and ver t' c GI r o 2 zi e
Magnetic siirbar
oo
-------
The standpipe test device, Figure 2, is designed with a closed container filled with test
solution where the sampling system with samplers can be suspended from the top, see
Appendix 3.3. Air from the sample reservoir is vented through an air hose. The con-
tainer is equipped with sampling ports and mixing is ensured through continuous
pumping from top to bottom.
For both the sample dispenser and the standpipe, the air entering the container to re-
place dispensed liquid is saturated with VOCs at the same concentration as in the con-
tainer, by using an air wash bottle.
Figure 2 Standpipe
Air exchange tube
Steel pipe
reci'rculation loop
Sampling port with
3-way valve and nozzl
end10Q811800378-3
The field sampling. Figure 3, is done by suspending the sampling systems with sam-
plers in the screened intervals in depth with the pump of established wells with con-
-------
tinuous pumping (monitoring wells or pump-and-treat wells), see Appendix 3.4. Ref-
erence samples are taken from the pumped streams (pump depth sampling strategy).
Figure 3 Field sampling
Air hose
Ground
String .
Groundwater
table
Sampler
Reservoir-
Reference sample
| Pump, stationary, continuous
pumping
Screened interval
and100811800378-2
3.2.2
In cases, where the pump is deeper than the maximum sampling depth or the installa-
tions do not allow for positioning the sampler in pump depth, a position above is cho-
sen (above pump sampling strategy). The sampler position is always within the
screened interval and within the same aquifer unit as the pump. In such cases, a low
volume reference sampling pump is positioned at the same depth as the sampler in-
take.
In all cases, a low purge sampling strategy is followed, allowing only for flushing of
sampling equipment.
Test staff
The test staff is test responsible Ph.D. Gerald Heinicke (GHE), field responsible Mette
T. Andersson (MTA) and test technician Susanne Klem (SEK).
-------
3.2.3 Test schedule
The test schedule is given in Table 3, see Table 1 for identification of experiment la-
bels.
Table 3 Test schedule
Task
Test plan
Pre-testing dispenser
Test using dispenser
Direct application
Set up standpipe
Test using standpipe
Test field
Test report draft
Test report QA
Test report
Week number 2008
47
X
X
H, L
48
X
49
X
X
50
X
X
51
X
X
52
X
Week no. 2009
1
X
2
3
BA
J
Task
Test plan
Pre-testing dispenser
Test using dispenser
Direct application
Set up standpipe
Test using standpipe
Test field
Test report draft
Test report QA
Test report
Week number 2009
4
DA
N
5
EA
P
6
7
FA, GA
R
T
8
HA
V
AA, AB, AC, AD, AE
9
CA
X
10
X
11
X
12
X
13
X
3.2.4 Test equipment
The test equipment includes (working procedures):
Laboratory sample dispenser (Appendix 3.2)
Stand pipe (Appendix 3.3)
Field sampling (Appendix 3.4)
The laboratory and stand pipe equipment has been designed and produced for the pur-
pose. Equipment test procedures are described in Appendix 3.5.
General laboratory equipment procedures including cleaning and calibration are those
described and ISO 17025 accredited 111 for the DHI laboratories under the laboratory
services manual of the DHI Quality Management System /8/.
3.2.5 Type and number of samples
The types and number of samples are summarized in Table 4.
-------
Table 4 Summary of type and number of samples
Limit of detection
Precision
Range of application
Trueness
Robustness, general
Robustness, specific
Reference for the ro-
bustness test levels
Sampling depth
Ionic strength
Sampling time
Concentration inte-
gration
Samples per test
scale
Samples totally5
Laboratory
7 analyses
3 reference analyses
7 analyses
3 samples
3 reference samples
1 reference analysis
6 samples
6 reference samples
2 reference analysis
6 samples
6 reference samples
2 reference analysis
3 samples
3 reference samples
3 reference analysis
32 samples
29 reference sam-
ples/analyses
Stand pipe
7 samples
7 reference samples
3 reference analysis
15 samples
15 reference samples
5 reference analysis
3 samples
3 reference samples
1 reference analysis
25 samples
34 reference sam-
ples/analyses
Field
15 samples
20 reference samples
15 samples
20 reference samples
72 samples
107 reference samples/analyses
The term analysis covers analysis of Sorbisense samplers that have been exposed to
standard solutions by direct application. The term "samples" is used for samples taken
with the Sorbisense sampler and analyzed accordingly.
The term reference analyses covers analysis of standards and standard dilutions after a
reference method in an accredited (ISO 17025) laboratory. The term reference samples
covers sampling of water and analysis after a reference method in an accredited (ISO
17025) laboratory.
The analytical program shown above includes 26 reference analyses of standard and
stock solutions, as well as of dilutions. If the stability of the solutions and the analyti-
cal precision proves satisfactory in the initial part of the program, the number of repli-
cate reference analysis may be reduced.
The water and the groundwater used in laboratory tests will be controlled for blanks,
and the groundwater further characterized for general groundwater parameters, see
Appendices 2 and 3.7.
Includes also pretesting samples and analyses not in the above rows
10
-------
In addition to the number of test samples, samples controlling the test systems will be
required as described in Appendix 3.5. The total number of samples for this purpose is
18 reference samples. The samples will include test system blank samples.
3.2.6 Operation conditions
The operation conditions applied during the verification of the product are:
• Sampling temperature: ambient 5-25°C
• Sampling depth: 0.5-5 m below the water surface
• Sample volume: up to 600 mL
• Sampling period: up to 9 days
• Sampling replicates: one sampler per sampling event
3.2.7 Operation measurements
During operation, the following operation conditions are recorded, as relevant, see
Appendix 5 for data recording and reporting forms:
• Sampling temperature
• Depth of sample intake
• Sample volume
• Sampling period
3.2.8 Product maintenance
Samplers are kept in sealed bags as delivered from the vendor at ambient temperature
until used. Opened bags with unused samplers are resealed until used.
No further maintenance is prescribed for the equipment.
3.2.9 Health, safety and wastes
The use of the product does not imply special health, safety and waste issues.
Laboratory work during testing will be done according to the DHI Safety Rules that
are compliant with the extensive Danish rules for safe occupational health and the
European regulations of work with chemicals. Work with VOC spiked solutions will
be done using nitrile rubber gloves.
Field work will be done according to the DHI rules for safe field work included in the
DHI Safety Rules.
Chemicals and test solutions are discarded according to Danish regulations for chemi-
cal waste by collection and destruction, in casu by collection in drums followed by
controlled destruction.
11
-------
4
REFERENCE ANALYSIS
The reference analysis applies to an aliquot of the test solutions that will be submitted
to an analytical laboratory for analysis. These samples will verify the actual concen-
trations of the test solutions and the results will be compared to the results of the prod-
uct in this verification.
4.1 Analytical laboratory
Reference analyses are done by Eurofms Danmark A/S, Smedeskovvej 38, DK-8464
Galten, Denmark.
Contact Rita Splidt Pedersen, Eurofms Milj0 A/S, +45 70 22 42 66.
4.2 Analytical parameters
The analytical parameters and the target VOC are given in Table 5.
Table 5 Analytical parameters
Analytical parameters
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
4.3 Analytical methods
The analysis are done using purge and trap gas chromatography with mass spectrome-
try detection in the selected ion monitoring mode (P&T GC-MS-SIM) according to the
packages given in Table 6.
Table 6 Analytical packages, parameters and performance expectations from the contracted laboratory
Analytical
package
DR124 chlorinated solvents
and degradation projects
DR102BTEX
231 45 MTBE
Parameter
Trichlorethene
Tetrachlorethene
1,1-Dichlorethene
trans-1 ,2-dichlorethene
cis-1,2-dichlorethene
Chloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Limit of
detection
ug/l
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,1
Uncertainty
%
7,5
9,2
8,5
8,2
14
7,7
7,4
8,9
9,4
7,4
7,3
7,0
12
-------
The analytical method is based upon EPA Method 624 191 and ISO 15680 /10/ (see
Appendix 2 for details).
4.4 Analytical performance requirements
The analytical performance requirements are given in Table 7.
It should be noted that the uncertainties stated by the laboratory, Table 6, includes both
the random error under reproducibility conditions (requirements set here for the preci-
sion under repeatability conditions) and the systematic errors (requirements set here
for the trueness).
For MTBE, concern may be raised whether the laboratory will be able to satisfy the
required limit of detection.
Table 7 Required analytical performances
Compound
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Xylenes
MTBE
Limit of
detection
M9/L
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
Precision
%
5
5
5
5
5
5
5
5
5
5
Trueness
%
90-110
90-110
90-110
90-110
90-110
90-110
90-110
90-110
90-110
90-110
Range of
application
ug/L
0.03-2000
0.03-2000
0.03-2000
0.03-2000
0.03-2000
0.03-2000
0.03-2000
0.03-2000
0.03-2000
0.03-2000
4.5 Preservation and storage of reference samples
All water samples for VOC reference analysis are taken in 3 x 40 mL autosampler vi-
als with Teflon lined screw caps as delivered from the laboratory contracted for refer-
ence sample analysis. The samples are not preserved but stored cold (1-5°C) and dark
until delivered to the laboratory within a maximum of 3 days.
5 DATA MANAGEMENT
In general, the data filing and archiving procedures of the DHI Quality Management
System will be followed.
5.1 Data storage, transfer and control
The data to be compiled and stored are summarized in Table 8.
Analytical raw data will be filed and archived according to the specifications of the
laboratories quality management systems under their ISO 17025 accreditation, Eu-
rofins for reference analysis and AlControl for sample analysis (Sorbisense sampler
analysis).
13
-------
Table 8 Data compilation and storage summary
Data type
Test plan and
report
Test details in
laboratory and
field
Calculations
Analytical re-
ports
Data media
Protected PDF
files
Log book and
pre-pre pared
forms
Excel files
Paper
Data recorder
Test responsi-
ble, DHI
Technician,
DHI
Test responsi-
ble, DHI
Test responsi-
ble, DHI
Data re-
cording tim-
ing
When ap-
proved
During collec-
tion
During calcula-
tions
When received
Data storage
Files and ar-
chives at DHI
Files and ar-
chives at DHI
Files and ar-
chives DHI
Files and ar-
chives DHI
Forms for data recording are given in Appendix 5.
6 QUALITY ASSURANCE
The tests are performed under the quality management system of DHI which is ISO
9001 compliant /I I/, but not certified. The DHI laboratories have ISO 17025 accredi-
tations 111 and OECD GLP approvals 1121 for a range of tests and ISO 17025 for sam-
pling of drinking water. As part of the ISO 17025 and GLP inspections, the procedures
for general laboratory processes, quality assurance and documentation/archiving are
assessed.
6.1 Test plan review
The test plan will be subject to internal review by the verification responsible from
DHI WMC Verifications: senior chemist Christian Gran. Additionally, the test plan
will be subject to review by the Battelle Advanced Monitoring Center quality manager
(Zachary Willenberg, respectively), as well as by the US EPA ETV AMS project offi-
cer, quality manager and ETV coordinator (John McKerna, Lauren Drees and Evelyn
Hazell, respectively).
External review of the test plan will be done by the expert group assigned to this veri-
fication.
6.2 Performance control - reference analysis
General chemistry, reference sample analyses and reference analyses are done under
the ISO 17025 accreditation of Eurofins.
The performance of Eurofins for the reference analysis will be evaluated (performance
evaluation audit) from laboratory quality control data for the relevant period (precision
under repeatability conditions, trueness). Data for the analytical quality control of the
laboratory will include duplicate control samples at two concentrations (acceptance
within 100%±10%) in each series and at the least one blank sample per 5 samples. The
data from participation in a proficiency test arranged by Analytical Products Inc Sep-
14
-------
tember 2008 will be evaluated for the demonstrated precision and traceability for the
compounds in question for relevant matrices.
The detection limits and risks of false positives of the laboratory are controlled by
submitting blank samples and low concentration samples as described in the test pro-
gram.
The precision and trueness of the laboratory is further evaluated by analysis of stock,
standard and spike solutions used for the test (26 reference analyses). The reference
analysis includes analysis of a standard with analytical certificate and of solutions pre-
pared from pure chemicals at DHL
The analytical reference performance control is summarized in Table 9, with reference
to Appendix 3.6 and 3.7 for information on water, standard solution (purchased stan-
dard with analytical certificate) and VOC solutions (prepared by DHI from pure
chemicals).
Table 9 Summary of analytical reference performance control
Control type
VOX standard solution
VOC solutions
Water
Laboratory quality control
Proficiency test
Limit of detection
-
-
X
-
-
Precision
-
X
-
X
X
Trueness
X
X
-
X
X
6.3 Test system control
The laboratory test design includes test solutions of known concentrations, traceable
back to added chemicals of p.a. quality or standards with analytical certificate, see
Appendix 3.7 for specifications of purity etc.
The known concentrations will be used to pre-test the test design, see Appendix 3.5.
The water used for preparation of solutions will be controlled for contents of the target
VOC as blanks by reference analysis.
The stability of the test concentrations will be controlled continuously during the tests
by taking and analyzing reference samples distributed over the sampling periods, con-
sidering the "true concentrations" based upon added amounts and the reference analy-
ses.
The control of the field test system is done using analysis of reference samples and
field blank samples.
The analytical reference performance control is summarized in Table 10. Laboratory
blanks/spiked samples are water, in some cases with ionic strength controlled by add-
ing KC1, and the standpipe blanks/stand pipe samples are groundwater (matrix).
15
-------
Table 10 Summary of test system control
Information/control type
System contamination/blank
sample reference analysis
System contamination/field
blank sample reference
analysis
System trueness/spiked
sample reference analysis
System variability/spiked
sample reference analysis
System trueness/natural
sample reference analysis
System variability/natural
sample reference analysis
Laboratory
X
-
X
X
-
-
Standpipe
X
-
X
X
-
-
Field
-
X
-
-
X
X
6.4 Data integrity check procedures
All transfer of data from printed media to digital form and between digital media are
checked by spot check of not less than 5% of the data (test or field responsible). If er-
rors are found in a spot check, all data from the transfer are checked.
6.5 Test system audits
Internal audit from DHI following the GLP audit procedure by a trained auditor is
done, see the verification protocol for details.
The Battelle quality manager, Zachary Willenberg, will perform a technical systems
audit (ISA) at least once during this verification and test. The purpose of this audit is
to ensure that the verification test is being performed in accordance with the AMS
quality management plan /13/, this test plan, published reference methods and any
methods used in the tests. In the ISA, the Battelle quality manager, or designee, may
review the reference methods used, and compare actual test procedures to those speci-
fied or referenced in this plan. In the TSA, the Battelle quality manager will observe
testing in progress, observe the reference method sample preparation and analysis
(when available), inspect documentation, and review technology-specific record
books. He will also check standard certifications and may confer with other Battelle
staff. A TSA report will be prepared, including a statement of findings and the actions
taken to address any adverse findings. The AMS quality manager and the
NOWATECH WMC verification responsible will receive a copy of Battelle's TSA re-
port. The TSA findings will be communicated to technical staff at the time of the audit
and documented in a TSA report.
The Battelle Quality Manager will perform an audit of data quality (ADQ). This will
be a review of data acquisition and handling procedures and an audit of at least 10% of
the data acquired in the test and verification. The Battelle Quality Manager will trace
the data from initial acquisition, through reduction and statistical comparisons, to final
reporting. All calculations performed on the data undergoing the audit will be checked.
16
-------
6.6 Test report review
The test report will be subject to internal review by the verification responsible from
DHIWMC Verifications: senior chemist Christian Gran.
External review of the test report will be done by the expert group as part of the re-
view of the verification report, that will include the full test report as an appendix.
7 TEST REPORT
The test report will follow the template of the DHI NOWATECH verification center
quality manual /14/ and will be included as an appendix in the verification report. The
test report will contain the test plan, except for this Chapter 7 on test report format,
with the data and records from the tests to be inserted as new Chapter 7. For this joint
verification, the principles (contents) of the US ETV format will be complied with as
well.
7.1 Test site report
The test site report will include: well design drawing, well and pump data, operation
data as outlined in Section 3.2.7 (forms in Appendix 5).
7.2 Test data report
The test data will include all data recorded during the test and the data reported by the
analytical laboratories, see Appendix 5 for data forms.
7.3 Amendment report
The report section on deviations will compile all changes of this test plan occurring
before testing with justification of deviations and evaluation of any consequences for
the test data quality.
7.4 Deviations report
The report section on deviations will compile all deviations from this test plan occur-
ring during testing with justification of deviations and evaluation of any consequences
for the test data quality.
17
-------
18
-------
A P P E N D I X 1
Terms and definitions used in the test plan
19
-------
The abbreviations and definitions used in the verification protocol and the test plan are
summarized below.
Where discrepancies exist between NOWATECH and US EPA ETV terminology,
definitions from both schemes are given.
Word
ADQ
AMS Center
Analysis
Analytical
laboratory
Application
A-UBA
BTEX
CEN
CWA
DHI WMC
Direct applica-
tion
DOC
Drinking water
control
DS
Effect
EN
ETV
EU
Evaluation
NOWATECH
Audit of data quality: An examination
of a set of data after is has been col-
lected and 1 00% verified by project
personnel, consisting of tracing at
least 10% of the test data from origi-
nal recording through transferring,
calculating, summarizing and report-
ing.
Advanced Monitoring Systems Cen-
ter at Battelle
Analysis of Sorbisense samplers at
the vendor identified laboratory
Independent analytical laboratory
used to analyze reference samples
The use of a product specified with
respect to matrix, target, effect and
limitations
Umweltbundesamt Austria
Benzene, toluene, ethylbenzene and
xylenes
European Committee for Standardi-
zation
CEN Workshop agreement
(ETV) Water Monitoring Center at
DHI
A test design where a standard solu-
tion is applied directly to the Sorbi-
sense samplers
Dissolved organic carbon
Control of drinking water quality
against drinking water maximum
concentrations.
Danish Standard
The way the target is affected, in this
verification the way the target com-
pounds are measured
European standard
Environmental technology verification
(ETV) is an independent (third party)
assessment of the performance of a
technology or a product for a speci-
fied application, under defined condi-
tions and adequate quality assur-
ance.
European Union
Evaluation of test data for a technol-
ogy product for performance and
data quality
US ETV
EPA program that develops generic
verification protocols and verifies the
performance of innovative environ-
mental technologies that have the
potential to improve protection of
human health and the environment
An examination of the efficiency of a
technology
20
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Word
Experts
GC
Groundwater
investigation
Groundwater
monitoring
GWS
ISO
Laboratory
sample dis-
penser
Limit of detec-
tion
LoD
Limit of quanti-
fication
LoQ
Matrix
mbgv
mbs
Method
MS
MTBE
NOWATECH
ETV
P&T
PE
Performance
claim
Performance
parameters
Precision
(Environmen-
NOWATECH
Independent persons qualified on a
technology in verification or on verifi-
cation as a process
Gas chromatography
Investigation of groundwater con-
tamination with measurements con-
trolled against groundwater maxi-
mum concentrations.
Baseline monitoring of groundwater
quality.
Groundwater sampler
International Standardization Organi-
zation
Test device designed for controlled
exposure of Sorbisense samplers to
test solutions.
Calculated from the standard devia-
tion of replicate measurements at
less than 5 times the detection limit
evaluated. Corresponding to less
than 5% risk of false blanks.
Calculated from the detection limit,
typically 3 times the LoD, the concen-
tration, where the blank variation im-
pacts the precision 20%.
The type of material that the product
is intended for
m below groundwater table
m below surface
Generic document that provides
rules, guidelines or characteristics for
tests or analysis
Mass spectrometry
Methyl-fe/f-butylether
Nordic Water Technology Verification
Centers
Purge and trap
Performance evaluation: A quantita-
tive evaluation of a measurement
system, usually involving the meas-
urement or analysis of a reference
material of known value or composi-
tion
The effects foreseen by the vendor
on the target (s) in the matrix of in-
tended use
Parameters that can be documented
quantitatively in tests and that pro-
vide the relevant information on the
performance of an environmental
technology product
The standard deviation obtained from
replicate measurements, here meas-
ured under repeatability or repro-
ducibility conditions.
Ready to market or prototype stage
US ETV
Peer reviewers appointed for a verifi-
cation
(Environmental) technology
21
-------
Word
tal) product
PVC
QA
Range of ap-
plication
Reference
analyses
Reference
samples
Repeatability
Reproducibility
Robustness
RSD
Sampler
Samples
Sampling sys-
tem
SIM
SM
Stakeholder
Standard
NOWATECH
product, process, system or service
based upon an environmental tech-
nology
Polyvinylchloride
Quality assurance
The range from the LoD to the high-
est concentration with linear re-
sponse,
Analysis by a specified reference
method in an accredited (ISO 17025)
laboratory.
Samples taken for and analyzed by a
specified reference method in an ac-
credited (ISO 17025) laboratory.
The precision obtained under repeat-
ability conditions, that is with the
same measurement procedure, same
operators, same measuring
system, same operating conditions
and same location, and replicate
measurements on the same
or similar objects over a short period
of time
The precision obtained under repro-
ducibility conditions, that is with
measurements that includes different
locations, operators, measuring sys-
tems, and replicate measurements
on the same or similar objects
% variation in measurements result-
ing from defined changes in matrix
properties.
Relative standard deviation in %.
Sorbisense sorbent cartridge
Samples taken with and analyzed
after the Sorbisense method.
The sampling reservoir and venting
system used to operate the Sorbi-
sense samplers
Selected ion monitoring
Standard Methods for the Examina-
tion of Water and Wastewater, latest
edition
Generic document established by
consensus and approved by a rec-
ognized standardization body that
provides rules, guidelines or charac-
USETV
Buyers and users of technology,
technology developers/vendors, the
consulting engineers, the finance and
export communities, government
permitters, regulators, first respond-
ers, emergency response, disaster
planners, public interest groups, and
other groups interested in the per-
formance of innovative environmental
technologies.
22
-------
Word
Standpipe
Target
(Environ-
mental) tech-
nology
Test/testing
Trueness
ISA
US EPA
Vendor
Verification
VOC
VOX
WS
NOWATECH
teristics for tests or analysis
Test device designed to simulate a
groundwaterwell
The property that is affected by the
product, in this verification the target
compounds measured.
The practical application of knowl-
edge in the environmental area
Determination of the performance of
a product by parameters defined for
the application
The % recovery of true value ob-
tained either from knowledge on the
preparation of test solutions or from
measurements with reference meth-
ods.
Technical system audit
United States Environmental Protec-
tion Agency
The party delivering the product or
service to the customer
Evaluation of product performance
parameters for a specified application
under defined conditions and ade-
quate quality assurance
Volatile organic compounds, here the
compounds listed as target com-
pounds/analytical parameters
Volatile halogenated organic com-
pounds, here the halogenated com-
pounds listed as target com-
pounds/analytical parameters
Workshop (under CEN)
USETV
An all-inclusive term used to describe
pollution control devices and sys-
tems, waste treatment processes and
storage facilities, and site remedia-
tion technologies and their compo-
nents that may be utilized to remove
pollutants or contaminants from, or to
prevent them from entering, the envi-
ronment.
The technology developer, owner, or
licensee seeking verification
Establishing or proving the truth of
the performance of a technology un-
der specific, predetermined criteria,
test plans and adequate data QA
procedures
23
-------
A P P E N D IX 2
Reference methods and references
24
-------
Reference analysis, VOC
Water samples are taken as 40 mL samples in autosampler vials filled completely from
the bottom and allow to overflow.
A precise volume of subsample is transferred from the sampler vial to the airsparger
via a sample loop and using helium as the pressure gas. The subsample is purged with
helium and the purged compounds trapped on a VOCARB 3000 adsorbent, followed
by thermal desorption at 240°C and transfer of desorbed compounds to the gas chro-
matograph (GC). GC separation is followed by selected ion monitoring and quantifica-
tion against external standard.
Selectivity is ensured by applying a maximum limit of 20% deviation of mass ratios
for the selected masses from reference run.
The equipment used is Tekmar Aquatek 70/Velocity XPT and Agilent 6890 GC/5973
or 5975 MS
Standard method references are EPA Method 624.2 191 and ISO 15680 /10/.
2 General chemistry
Groundwater from wells in the field test will be characterized for general chemistry
parameters using the below given methods. Analysis for pH and conductivity is done
on-line in the field.
Parameter
PH
Conductivity
Nitrate
Fluoride
Chloride
Bicarbonate
Sulphate
Method
DS287
DS288
EN 10304
EN 10304
EN 10304
DS256
EN 10304
Parameter
DOC
Iron
Ammonium
Sodium
Potassium
Calcium
Magnesium
Method
EN 1484
SM3500C
DS224
SM3500C
SM3500C
SM3500C
SM3500C
General chemistry data for groundwater for the laboratory tests, see Appendix 3.7, will
be obtained from the water work delivering the water.
25
-------
2 References
1. Gran, C. Sorbisense GWS40 Passive Sampler. Joint verification protocol. 2008.
2. Battelle. Process Document for US EPA ETV AMS Center and NOWATECH DHI WMC Joint Verifica-
tion of the Sorbisense Ground Water Sampler. 2009.
3. ISO. Guidance on Quality assurance of environmental water sampling and handling. 5667-14. 1998.
4. ISO. Water Quality - On-line sensors/analysing equipment for water - Specifications and prerformance
tests. ISO 15839. 2006.
5. CEN. Environmental technology verification - Soil and groundwater site characterization, monitoring and
remediation Technologies. CEN/WS CWA 32. 2008.
6. Sandia National Laboratories. Ground Water Sampling Technologies Verification Test Plan. U.S. Environ-
mental Protection Agency.
Environmental Technology Verification Program . 1999.
7. ISO. General requirements for the competence of testing and calibration laboratories. ISO 17025. 2005.
8. DHI. DHI Quality Manual. 2008.
9. US EPA. Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatog-
raphy/Mass Spectrometry. Method 624.2. 1995.
10. ISO. Water quality ~ Gas-chromatographic determination of a number of monocyclic aromatic hydrocar-
bons, naphthalene and several chlorinated compounds using purge-and-trap and thermal desorption. ISO
15680. 2003.
11. International Standardization Organisation. EN ISO 9001. Quality management systems - Requirements.
15-11-2008.
12. OECD. OECD Principles of Good Laboratory Practice. OECD GLP Document No. 1. 21-1-1998.
13. Battelle. Quality Management Plan (QMP) for the ETV Advanced Monitoring Systems Center. Version 7.0.
17-11-2005.
14. NOWATECH. Verification test center quality manual. 2008.
26
-------
A P P E N D IX 3
In-house test methods
27
-------
The in-house test methods are the detailed specifications (work instructions) of the tests to be
performed including specific information on the practical work planned, Appendices 3.1 to 3.4.
The pre-testing is described in Appendix 3.5 and the check of solutions used in Appendix 3.6.
Reagents are described in Appendix 3.7 and apparatus in Appendix 3.8.
The volumes of solutions used for different experiments are summarized in Appendix 3.9.
The storage and shipping of samples is described in Appendix 3.10.
28
-------
Appendix 3.1
Direct application of halogenated hydrocarbons standard to samplers.
For personal safety and to avoid contamination, wear nitrile gloves for all handling of equip-
ment.
a) Place 7 samplers in the fume cupboard in a vial stand.
b) Add the spike (50 jiL of 24.7 |ig/mL VOX standard dilution for SxLoD, 50 jiL standard
solution for 10 % of range) directly into the adsorber resin of the sampler using a 50 jiL
gas tight syringe.
c) Place each sampler into a separate 100 mL glass bottle with PTFE-lined screw cap.
d) Place 3-4 of the 100 mL bottles into a 2 L wide-neck glass bottle with Teflon-lined
screw cap.
e) Let the samplers equilibrate at 4°C for 24 hours at least.
f) Remove the samplers from the glass bottles.
g) Connect 3 of the samplers to the sample dispenser using new 1/16" capillaries.
h) Convey 300 ml (collect in 500 mL graduated cylinders) of water through each sampler
during ca. 4 hours. This is done in batches of 2-3 samplers, before the sample dispenser
has been used with VOCs, but after the blank test of the sample dispenser.
i) Prepare the samplers for shipping.
29
-------
Appendix 3.2
Laboratory sample dispenser.
For personal safety and to avoid contamination, wear nitrile gloves for all handling of equip-
ment.
1 Preparations
a) Start with the clean, empty dispenser, lid attached, air exchange pipe detached from the
wash bottle. Make sure the stir bar in the dispenser is positioned in the middle of the
dispenser bottom and rotating when stirrer is switched on.
b) Connect the sampler capillaries to the 1/16 inch fittings. Place the ends of the capillaries
above the lid of the lab dispenser to avoid leakage.
c) Add 35 mL potassium chloride stock solution to the dispenser through the spiking port,
using a 100 mL syringe with Luer lock. For the tests with different ionic strength add
10 mL for 10 mS/m or 100 mL for 100 mS/m). Rinse with 100 mL of water
d) Fill the dispenser with water (see separate instruction below)
e) Add the VOC spike to the dispenser (see separate instruction below).
f) Fill the wash bottle with water up to the 5.5 L-mark, using the PTFE tubing.
g) Add the adequate spike directly to the wash bottle (under the water surface) and close
the wash bottle.
h) Connect the exchange pipe and tighten the fittings.
i) Start the magnetic stirrers in the wash bottle.
j) Take down the end of the capillaries from the dispenser. Let at least 1 mL go to drain.
k) Make sure that 30 minutes have passed since the magnetic stirrers have been started;
then, connect a sampler to each capillary.
1) Start the magnetic valve timer.
m) Note the time and possible deviations
2 Filling the dispenser with water
a) Attach one end of the PTFE tube to the vertical nozzle of the sampling port. Attach the
other end to the water tap (MilliQ).
b) Open the two-way valve in the lid of the dispenser.
c) Open the sampling port valve. Open the water tap to fill the dispenser until water over-
flows from the open two-way valve.
d) Close the water tap. Close the spiking port valve.
e) Remove the PTFE tube and close the open ends with tinfoil.
f) Drain 200 mL of water from the dispenser through the sampling port. Measure conduc-
tivity and temperature in the drained water.
g) Continue with step le
3 Addition of spike to the lab dispenser
a) Start the dispenser's magnetic stirrer
b) Open a stock solution vial with appropriate volume.
c) Fill the appropriate amount into the suitable gaslight syringe with Luer lock, with nee-
dle attached.
30
-------
d) Remove the needle from the syringe and connect the syringe to the dispenser's spiking
port.
e) Open the spiking port valve and add the contents to dispenser.
f) Close the spiking port valve and remove the syringe.
g) Attach the needle and fill syringe with methanol. Detach the needle and add also the
methanol to the dispenser.
h) Close the spiking valve, and remove the syringe.
i) Fill a 100 mL syringe with Luer lock with water. Add the water to the dispenser. Close
the spiking port valve and remove the syringe.
j) Close the two-way valve in the lid of the dispenser.
k) Continue with step If
4 During exposure
a) Control the amount of liquid that has passed through each sampler after /^ the sampling
time and full sampling time by collecting in pre-weighed 1000 mL bottles.
b) Take water phase sample from the dispenser after 2 hours, 1A the sampling time and full
sampling time, following the sampling instruction.
5 Reference sampling instructions
a) Wipe the vertical nozzle of the sample tap with acetone-soaked paper tissue. Rinse the
nozzle with water from a bottle, dry with paper tissue.
b) Set the magnetic valves to open.
c) Open the sample tap and drain 25 mL to waste.
d) Place the nozzle in a 40 mL P&T vial, open the sample valve by ca. 45 degrees and fill
the vial slowly from below. Let the sample overflow for at least 3 seconds. Close the
sample tap, and close the vial.
e) Repeat c) for the 2 following P&T vials.
f) Start the magnetic valve timer.
g) Repeat a) to clean the nozzle after sampling.
h) Store cold 1-5°C and dark for no more than 3 days and transfer to laboratory.
5 End of exposure
a) Stop both magnetic stirrers.
b) Open the two-way valve in the lid of the dispenser.
c) Drain the dispenser through the sample tap, into containers for disposal.
d) Remove the samplers and send them for analysis.
e) Detach the air exchange pipe from the wash bottle6 and tilt the container towards the
sample tap to empty completely.
f) Detach the magnetic valve from the other side of the wash bottle.
g) Empty the wash bottle. Attach the air exchange pipe lightly until next use.
6 Whenever detaching the connections of the wash bottle, detach the nut on the steel side of
the fitting, not on the glass side.
31
-------
Appendix 3.3
Standpipe
1 Preparations
Wear nitrile gloves for all handling of equipment.
a) Mount the needed number of samplers with samplers into the empty Standpipe. Tighten
with the provided strings
b) Connect the air exchange pipes to the lid.
c) Close the Standpipe.
d) Open the two-way valve in the lid of the Standpipe.
e) Fill the Standpipe from the bottom with ground water, using PTFE tubing, until water
overflows from the open two-way valve.
f) Stop the water flow, close the sampling port valve and remove the PTFE tubing.
g) Drain 200 mL from the Standpipe. Measure conductivity and temperature in the drained
water.
h) Start the circulation pump.
i) Add the spike to the Standpipe (see separate instruction).
j) Fill the wash bottle with water up to the 5.5 L-mark, using the PTFE tubing.
k) Add an adequate spike directly to the wash bottle (under the water surface) and close
the wash bottle.
1) Connect the air exchange pipe.
m) Start the magnetic stirrer in the wash bottle. Start the magnetic valve timer.
n) Note the time and possible deviations
2 Addition of spike to the Standpipe
a) Make sure the magnetic valves are closed.
b) Open a stock solution vial with appropriate volume.
c) Fill the appropriate amount into the suitable gaslight syringe with Luer lock, with nee-
dle attached.
d) Remove the needle from the syringe and connect the syringe to the Standpipe's spiking
port.
e) Open the spiking port valve and add the contents to Standpipe.
f) Close the spiking port valve and remove the syringe.
g) Fill a 100 mL syringe with Luer lock with water. Add the water to the dispenser. Close
the spiking port valve and remove the syringe.
h) Close the two-way valve in the lid of the Standpipe.
i) Continue with step Ih
3 During the exposure
Take water phase sample from the dispenser after 2 hours, /^ the sampling time and full
sampling time, following the sampling instruction.
32
-------
4 Reference sampling instructions
a) Wipe the vertical nozzle of the sample tap with acetone-soaked paper tissue. Rinse the
nozzle with water from a bottle, dry with paper tissue.
b) Set the magnetic valves to open.
c) Open the sample tap and drain 25 mL to waste.
d) Place the nozzle in a 40 mL P&T vial, open the sample valve by ca. 45 degrees and fill
the vial slowly from below. Let the sample overflows for at least 3 seconds. Close the
sample tap, and close the vial.
e) Repeat c) for the 2 following P&T vials.
f) Start the magnetic valve timer.
g) Repeat a) to clean the nozzle after sampling.
h) Store cold 1-5°C and dark for no more than 3 days and transfer to laboratory.
4 End of exposure
a) Stop the magnetic stirrer in the air wash bottle.
b) Stop the recirculation pump.
c) Open the two-way valve in the lid of the standpipe.
d) Remove the air exchange pipe.
e) Drain the standpipe into containers for disposal, using the sample tap.
f) Open the standpipe and take up the sampler
g) Remove the samplers and send them for analysis
h) Measure the sampled water volume by collecting in 1000 mL pre-weighed glass bottles
and weighing
i) Tilt the container towards the sample tap to empty completely.
j) Empty the wash bottle. Attach the air exchange pipe lightly.
33
-------
Appendix 3.4
Field sampling
1
Data compilation
First planning step includes data compilation in order to allow for the detailed plan-
ning:
Full Address
S0borg hovedgade
23, S0borg
S0borg hovedgade
17-19, S0borg
S0borg hovedgade
189, S0borg
Fa rum Bytorv 36,
Farum
Roskildevej 2-4, Al-
bertslund
Well iden-
tification
AFV6
AFV4
B109
AFV1
K4
Well regis-
tration
number
201.5751
201.5749
201.5743
193.2283
200.5185
Contact, name, phone,
e-mail
Region Hovedstaden,
Jens Lerche Mortensen,
+45 48 20 53 33,
jens.lerche.mortensen@
regionh.dk
Region Hovedstaden,
Jens Lerche Mortensen,
+45 48 20 53 33,
jens.lerche.mortensen@
regionh.dk
Region Hovedstaden,
Jens Lerche Mortensen,
+45 48 20 53 33,
jens.lerche.mortensen@
regionh.dk
Jord»Milj0, Charlotte
Juhl S0egaard, +45 35
82 04 02,
cjs@jordmil.dk
Jord»Milj0, Charlotte
Juhl S0egaard, +45 35
82 04 02,
cjs@jordmil.dk
Well iden-
tification
AFV6
AFV4
B109
AFV1
K4
Filter
(mbs) 7
5-13.3
9.5-14.5
13.5-46.5
8-15
7.5-9.5
Diameter
(mm)
125
160
165
160
160
Groundwa-
ter table
(mbs)
7.7
11.5
22
7.3
5.3
Geology
Sand
Sand
Sand
Sand
Limestone
Well iden-
tification
AFV6
Pump
(mbs)
13
Yield
(m3/hour)
0.2
Pumping
pattern
Start at water
level < 12
mbs, stop at
13 mbs
Access for
samplers
Should be
possible to
place next to
pump
mbs: meter below surface
34
-------
Well iden-
tification
AFV4
B109
AFV1
K4
Pump
(mbs)
14
37
12
8.5
Yield
(m3/hour)
1.5-2.5
2-2.5
1.5-2
2.5
Pumping
pattern
Start at water
level < 8.5
mbs, stop at
9.5 mbs
Continuously,
stop for
cleaning 15
min/day
Continuously
3 min
pumping, 5
min stop, etc.
Access for
samplers
Should be
possible to
place next to
pump
Good access
Should be
possible to
place next to
pump
Should be
possible to
place next to
pump
2 Reference sampling strategy
The second planning step is to select the reference sampling strategy (pump depth or
above pump) and to select the sampling (0.5-5 mbgvt8) and reference sampling posi-
tions. The pump depth sampling strategy applies sampling of the pumped stream. In
cases where the pump is positioned deeper than the maximum sampler depth, a posi-
tion above the pump is chosen, the above pump strategy.
Well iden-
tification
AFV6
AFV4
B109
AFV1
K4
Sampler
position
(mbs)
13
14
27
12
8.5
Sampler posi-
tion to in well
groundwater
table distance
(m)
1-2
3.5-4.5
4
1
0.5-3.5
Reference
sampling
position
(mbs)
13
14
27
12
8.5
Sampling
strategy
Pump depth
Pump depth
Above pump
Pump depth
Pump depth
3 Sampling
The sampling is done as follows:
a) Mount a sampling system with a sampler in the well at the selected depth
b) Secure the position with the provided string
c) Leave the sampler in position for 6 days
d) Take up the sampler
e) Remove the sampler and send it for analysis
f) Repeat twice
mbgv: m below groundwater table
35
-------
The reference sampling is done as follows, for the pump depth strategy:
a) Mount sampling tube upon pump exit sampling tap
b) Flush tap and tube 5-10 minutes with lowest flow filling the tube
c) Fill sample containers from the bottom and allow to overflow 2-3 times
d) Store and preserve samples as prescribed and send to the laboratory
The reference sampling is done as follows, for the above pump strategy:
a) Ensure that well pump is running at routine yield
b) Lower the pump into the well to the selected depth
c) Purge with the lowest flow filling the tube for 5-10 minutes, max 5% of stationary
pump yield
d) Ensure stability (within 10%) of indicator parameters (pH, dissolved oxygen, con-
ductivity)
e) Fill sample containers from the bottom and allow to overflow 2-3 times ensuring
no head space in the containers
e) Store and preserve samples as prescribed and send to the laboratory
Reference sampling is done before, between and after each sampling, totally 4 times.
Field blanks are prepared during the first reference sampling at each site. Water is
transferred to sample bottles on site and the samples at stored, transported and ana-
lyzed as reference samples.
Sampling is done using a Grundfos MP1 pump equipped with 10 mm Teflon tubes,
leaving the tubes in each well. Indicator parameters (pH, dissolved oxygen, conductiv-
ity, temperature) are measured in a flow through on-line cell.
36
-------
Appendix 3.5
Pre-testing
Laboratory sample dispenser
Objective
Test design
Samples
Blank test
Dispenser filled with water.
Triplicate reference sam-
ples 1) of water, 2) from
dispenser directly 30 min
after addition, and 3) from
dispenser after 6 days.
VOC stability in dispenser
Dispenser filled with water,
spiked to SxLoD.
Triplicate samples 1) of 0.1
g/L VOC solution, 2) from
dispenser 30 minutes after
addition, and 3) from dis-
penser after 6 days.
37
-------
Appendix 3.6
Preparation of solutions for reference analysis
1 10 g/L VOC stock solution
Check of concentrations is done initially and each time a subsample is taken out for
use.
Initial testing is done by filling a 1,5 mL capped vial with stock solution at -20 °C, us-
ing a low-flow pipette. Close vial. Produce triplicate vials in this way. Place each of
the 1 mL capped vials in a larger capped vial. Store cold 1-5°C and dark for no more
than 3 days and transfer to laboratory with information of concentration range.
Check during use: after using part the stock solution in the vial for spiking, fill one 1,5
mL capped vials with the solution using a gas-tight syringe. Close the vial and place it
in a larger capped vial. Store cold 1-5°C and dark for no more than 3 days and transfer
to laboratory with information on concentration range. Produce 2 more vials and keep
at -20 °C for possible future reference
2 0.1 g/L VOC solution
Check during use is done after using part the solution in the vial for spiking by trans-
ferring 1 mL to a cap vial using a low-flow pipette. Close vial, shake well. Produce
triplicate vials in this way. Close the vials and place each in a larger capped vial. Store
cold 1-5°C and dark for no more than 3 days and transfer to laboratory with informa-
tion of concentration range.
3 VOX Standard dilution
Check during use is done after using part the stock solution in the 6 mL vial with VOX
standard dilution for spiking. Fill three 1.5 mL capped vials with the solution using a
gas-tight syringe. Close the vials and place them in a P&T vial. Store cold 1-5°C and
dark for no more than 3 days and transfer to laboratory with information of concentra-
tion range
38
-------
Appendix 3.7
Reagents
1 Water
Laboratory grade water from Millipore system with electrical conductivity below 10
MQ/cm. Dissolved organic carbon below 0.1 mg/L and target VOC below the limit of
detection 0.02 |ig/L is expected and verified in first blank test series.
2 Groundwater
Potable water as obtained from the supply network at DHL Groundwater characteris-
tics are as follows:
Parameter
PH
Conductivity
Nitrate
Fluoride
Chloride
Bicarbonate
Sulphate
Value
7.6
71 mS/m
2.4 mg/L
0.62 mg/L
44 mg/L
340 mg/L
21 mg/L
Parameter
DOC
Iron
Ammonium
Sodium
Potassium
Calcium
Magnesium
Value
1 .5 mg C/L
0.02 mg/L
0.058 mg/L
30 mg/L
3.8 mg/L
85 mg/L
22 mg/L
Target VOC is below the limit of detection 0.02 |ig/L.
3 VOX standard
Standard solution "QTM Volatile Halocarbons Mix" produced by Supelco, purchased
from Sigma-Aldrich, product number 48001, lot number LB59726, with analytical
certificate, MFG date July 2008, nominal concentrations as follows (among other
VOCs):
Compound
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Nominal concentration
ug/L
1998
2000
2000
1951
2000
2000
Chemicals
Compound
1,1-Dichloroethene
trans-1 ,2-
Dichloroethene
Pro-
ducer
Supelco
Supelco
Quality
Analytical
standard
Analytical
standard
Purity
99.9%
99.9%
Batch
LB56468
LB57511
39
-------
Compound
cis- 1 ,2-
Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
m-Xylene
o-Xylene
MTBE
Methanol
Potassium chloride
Pro-
ducer
Fluka
Fluka
Supelco
Fluka
Fluka
Fluka
Fluka
Fluka
Fluka
Fluka
Fluka
Quality
Analytical
standard
Puriss. p. a.
Analytical
standard
Puriss. p. a.
Puriss. p. a.
Puriss. p. a.
Puriss. p. a.
Puriss. p. a.
Puriss. p. a.
Puriss. p. a.
For trace
analysis of
chlorinated
hydrocar-
bons
Puriss. p. a.
Purity
99.7%
>99.5%
99.9%
99.9%
>99.7%
>99.0%
>99.0%
>99.0%
>99.5%
>99.8%
>99.5%
Batch
7333X
1368013
LB56979
1369911
1392028
1388758
1399073
1406896
1399802
1379978
80150
5 10 g/L VOC stock solution
Prepare a 10 g/L solution of each target VOC as follows:
a) Fill a 250 mL volumetric flask (with glass stopper) with methanol, refrigerate
to -20°C and mark the level.
b) Keep 210 mL methanol in the volumetric flask, place on ice in fume cup-
board.
c) Add the volume indicated below of each chemical using low flow pipettes,
starting with the highest boiling compound and keeping the pipette below the
methanol surface while emptying. Close the flask after each addition.
d) Refrigerate flask to -20°C
e) Fill the volumetric flask to the new mark with methanol refrigerated to -20°C.
f) Shake by hand until no phase difference is visible.
g) Distribute the stock solution into 1.5, 3.5 and 10 ml capped vials using a low
flow pipette. Check cap tightness (tight when cannot be twisted), wrap with
aluminum foil and place in freezer, -20°C.
Compound
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m-Xylene
uL pipetted
-
2000
2000
1 500
1 750
1 500
2750
2750
2750
2750
3000
Density
9/L
-
1.218
1 .2565
1.2837
1 .4642
1 .6227
0.87865
0.8669
0.867
0.8802
0.8642
ug pipetted
-
2 436 000
2513000
1 925 550
2 562 350
2 434 050
2416288
2 383 975
2 384 250
2 420 550
2 592 600
Concentration g/L
-
9.74
10.05
7.70
10.25
9.74
9.67
9.54
9.54
9.68
10.37
40
-------
Compound
MTBE
uL pipetted
3250
Density
9/L
0.74
ug pipetted
2 405 000
Concentration g/L
9.62
6 0.1 g/L VOC solution
Prepare a 0.1 g/L solution from the lOg/L solution as follows, directly before use.
a) Open a 1.5 mL vial of 10 g/L stock solution
b) Fill a 10 mL capped vial with 10 mL of methanol using a low flow pipette at
20°C±2°C
c) Add 100 jiL of 10 g/L stock solution using a gas tight syringe with cemented
needle, keep needle under methanol surface while emptying.
d) Close the vial, check for tightness.
e) Shake by hand.
f) Use after letting the solution equilibrate at room temperature for 1 hour.
7 24.7 ug/L VOX standard dilution for direct application
Prepare a 24.7 |ig/mL stock solution of halogenated hydrocarbons as follows:
a) Add 6 mL of methanol to a 6 mL cap vial using a low flow pipette.
b) Transfer 75 jil of the 2000 |ig/mL volatile hydrocarbon standard to the cap
vial using a 50 jiL gas tight syringe, keeping the needle below the methanol
surface while emptying.
c) Close the vial, check for tightness.
d) Shake by hand.
e) Use after letting the solution equilibrate at room temperature for 1 hour.
8 205 g/L KC1 stock solution
Prepare a 205 g/1 stock solution of potassium chloride:
a) Place a 1000 mL volumetric flask with 200 mL of water
b) Weigh the flask with water
c) Add portions of KC1 dried at 105°C overnight and shake well
d) When all 205 g of KC1 is dissolved, allow the solution to equilibrate to room
temperature.
e) Fill the flask to the mark.
f) Transfer to a 1000 mL glass bottle and close with a blue cap screw lid.
41
-------
Appendix 3.8
Apparatus
1 Glass syringes and adapters
a) 1 gas tight glass syringe with stainless steel Luer-lock, 2.5 mL
b) 1 gas tight glass syringe with stainless steel Luer-lock, 5 mL
c) 1 gas tight glass syringe with stainless steel Luer-lock, 10 mL
d) 1 stainless steel Luer/Luer adapter with valve, each for lab dispenser and
standpipe.
e) 6 needles with Luer adapter, 22 ga (0.394 mm ID)
f) 1 gas tight syringes with fixed needle, 25 jiL
g) 2 gas tight syringes with fixed needle, 50 jiL
h) 1 gas tight syringe with fixed needle, 100 jiL
i) 1 gas tight syringe with fixed needle, 500 jiL
j) 1 gas tight syringe with fixed needle, 1000 jiL
k) Glass syringe with Luer lock, 100 mL
2 Glassware
a) Volumetric flasks 250 mL and 1000 mL with glass stopper
b) Low flow glass pipettes at 250, 500, 7500, 1000, 1250, 1500, 2000 and 2500
,iL
c) 3 stir bars, glass coated
d) Capped vials for 1.5, 3.5, and 10 mL, caps with PTFE seals.
e) 25 mL Erlenmeyer flask with mark
f) 200 mL Erlenmeyer flask with mark
g) 1000 mL bottle with blue screw cap
h) 1000 mL bottles with red screw cap
i) 500 mL graduated cylinders
3 Miscellaneous
a) Micropipettes with tips at 100 jiL, 1 mL and 5 mL
b) Dedicated, water flushed PTFE tubes, 8x6 mm diameter
c) Nitrile gloves
3 Field
a) GrundfosMPl pump
b) Transformer box
c) 220 V generator
d) Dedicated, water flushed 10 mm PTFE tubes
e) On-line flow through devices (WTW) for monitoring of indicator parameters
(pH, dissolved oxygen, conductivity)
42
-------
Appendix 3.9
Spike volumes and solutions
Experiment
H
L
BA
DA
EA
FA
GA
HA
HA
HA
J
N
P
R
T
V
CA
Lab dispenser or
standpipe (mL)
0.050
0.050
4.00
4.00
4.00
4.00
4.00
1.50
4.00
6.00
2.50
2.00
5.00
10.00
15.00
20.00
10.00
Wash bottle
(mL)
—
—
0.55
0.55
0.55
0.55
0.55
0.2
0.55
0.85
0.125
0.10
0.25
0.50
0.80
1.00
0.50
Solution
VOX standard dilution
VOX standard
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
0.1 g/L VOC solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
1 0 g/L VOC stock solution
43
-------
Appendix 3.10
Managing, storing and shipping of samples/samplers
1 Managing samples
a) Prior to each individual test, the sampling responsible (test technician or field
responsible) labels the correct type and number of sample vials, according to
information in the test plan and the data forms. For cap vials, only the labels
are prepared, to avoid contamination.
b) The test responsible checks the array of labeled sample bottles and labels
against the test plan and the data forms.
c) After sampling, the sampling responsible takes a photo of the sample vials and
sends the photo to the test responsible immediately.
d) The sampling responsible stores the sample vials.
e) The test responsible prepares a requisition for analysis, and sends it to the sam-
pling responsible.
f) The sampling responsible ships the samples, and making sure that they are sent
within the maximum stated storage time.
g) The sampling responsible informs the test responsible immediately when the
samples have been sent.
h) The sampling responsible keeps a copy of the requisition with a note of the
date of shipping.
2 Sample storing, reference samples
Water samples are taken in 40 mL P&T vials. Samples are stored cold 1-5°C and dark
for no more than 3 days prior to transfer to the laboratory.
3 Sample storing, samplers
Samplers are equipped with protective caps in both ends, placed in transportation
tubes and stored cold 1-5°C and dark for no more than 7 days prior to transfer to the
laboratory.
4 Sample shipping, reference samples
Water samples (P&T vials) are sent in cooling boxes with cooling elements. Cap vials
with stock solution or stock dilution are placed individually into a P&T vial and may
be sent in a non-isolated package, with one cooling element.
44
-------
5 Sample shipping, samplers
Samplers are packed in the transport tubes in a cardboard box at ambient temperature.
45
-------
A P P E N D IX 4
In-house analytical methods
46
-------
None
47
-------
A P P E N D I X 5
Data reporting forms
48
-------
A Check of 10 g/L VOC stock solution, reference analyses, unopened vial
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Dec.1,2008
A1
Not taken
A2
Cone
Not taken
A3
entration mg/L
Jan. 8, 2009
A4
Jan. 8, 2009
A5
Jan. 8, 2009
A6
aA Check of 10 g/L VOC stock solution, reference analyses, used in test BA. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
aA1
Concen
Spare
Vial
aA2
tration g/L
Spare
Vial
aA3
49
-------
bA Check of 10 g/L VOC stock solution, reference analyses, used in test DA. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
bA1
Concen
Spare
Vial
bA2
tration g/L
Spare
Vial
bA3
50
-------
cA Check of 10 g/L VOC stock solution, reference analyses, used in test EA. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
cA1
Concen
Spare
Vial
cA2
tration g/L
Spare
Vial
cA3
o!A Check of 10 g/L VOC stock solution, reference analyses, used in test FA. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
dA1
Concen
Spare
Vial
dA2
tration g/L
Spare
Vial
dA3
51
-------
eA Check of 10 g/L VOC stock solution, reference analyses, used in test GA. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
eA1
Concen
Spare
Vial
eA2
tration g/L
Spare
Vial
eA3
fA Check of 10 g/L VOC stock solution, reference analyses, used in test HA for 20 % of range. Spare vials are not sent for analysis, but kept in
the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
fA1
Concen
Spare
Vial
fA2
tration g/L
Spare
Vial
fA3
52
-------
gA Check of 10 g/L VOC stock solution, reference analyses, used in test HA for 50 % of range. Spare vials are not sent for analysis, but kept in
the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
QA1
Concen
Spare
Vial
QA2
tration g/L
Spare
Vial
gA3
hA Check of 10 g/L VOC stock solution, reference analyses, used in test HA for 80 % of range. Spare vials are not sent for analysis, but kept in
the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
hA1
Concen
Spare
Vial
hA2
tration g/L
Spare
Vial
hA3
53
-------
IA Check of 10 g/L VOC stock solution, reference analyses, used in test N. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
iA1
Concen
Spare
Vial
iA2
tration g/L
Spare
Vial
iA3
jA Check of 10 g/L VOC stock solution, reference analyses, used in test P. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
JA1
Concen
Spare
Vial
JA2
tration g/L
Spare
Vial
JA3
54
-------
kA Check of 10 g/L VOC stock solution, reference analyses, used in test R. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
kA1
Concen
Spare
Vial
kA2
tration g/L
Spare
Vial
kA3
IA Check of 10 g/L VOC stock solution, reference analyses, used in test T. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
IA1
Concen
Spare
Vial
IA2
tration g/L
Spare
Vial
IA3
55
-------
mA Check of 10 g/L VOC stock solution, reference analyses, used in test V. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
mA1
Concen
Spare
Vial
mA2
tration g/L
Spare
Vial
mA3
nA Check of 10 g/L VOC stock solution, reference analyses, used in test CA. Spare vials are not sent for analysis, but kept in the freezer.
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Usage
Date
nA1
Concen
Spare
Vial
nA2
tration g/L
Spare
Vial
nA3
56
-------
B Check of 0.1 g/L VOC solution, reference analyses, used in lab dispenser pre-testing
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Preparation
Date
B1
Concen
Preparation
Date
B2
tration g/L
Preparation
Date
B3
aB Check of 0.1 g/L VOC solution, reference analyses, used in test J
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Preparation
Date
aB1
Concent
Preparation
Date
aB2
ration mg/L
Preparation
Date
aB3
57
-------
C Check of VOX standard dilution, reference analyses
Compound
Date
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Preparation
Date
C1
Concent
Preparation
Date
C2
ration mg/L
Preparation
Date
C3
aD Check of MiliQ water from tap
Compound
Date
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
aD1
Concent
Sample 2
aD2
ration ug/L
Sample 3
aD3
58
-------
bD Check of water from lab dispenser sample tap after 30 minutes.
Compound
Date
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
bD1
Concent
Sample 2
bD2
ration ug/L
Sample 3
bD3
D Check of water from lab dispenser sample tap after 6 days
Compound
Date
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
D1
Concent
Sample 2
D2
ration ug/L
Sample 3
D3
59
-------
cD Check of ground water (blank)
Compound
Date:
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
cD1
Concenl
Sample 2
cD2
ration ug/L
Sample 3
cD3
E VOC stability check of sample dispenser, reference samples after 30 minutes
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
E1
Concenl
Sample 2
E2
ration ug/L
Sample 3
E3
60
-------
aE VOC stability check of sample dispenser, reference samples after 6 day
Compound
Date
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
aE1
Concent
Sample 2
aE2
ration ug/L
Sample 3
aE3
F and G are omitted, covered by experiment J.
61
-------
H LoD direct application, samples
Compound
Date of spiking
Temperature
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Date of rinsing
mL passed (measured)
mL passed (by tracer salt)
ID
H1
ID
H2
M
ID
H3
ass on sampler |j
ID
H4
g
ID
H5
ID
H6
ID
H7
is omitted, covered by experiment C.
62
-------
J LoD standpipe, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
ID
J1
ID
J2
Co
ID
J3
ncentration |j
ID
J4
3/L
ID
J5
ID
J6
ID
J7
Dates
Setup
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Setup
Sampled
External
pressure
bar
-
-
-
-
-
-
K LoD standpipe, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
K1
Sample 2
Date
K2
Co
Sample 3
Date
K3
ncentration ug/L
Sample 4
Date
K4
Sample 5
Date
K5
Sample 6
Date
K6
Sample 7
Date
K7
63
-------
L Precision direct application, samples
Compound
Date of spiking
Temperature
Chloroethene
1,1-Dichloroethene
1,2-Dichloroethenes
Trichloroethene
Tetrachloroethene
Date of rinsing
mL passed (measured)
mL passed (by tracer salt)
ID
L1
ID
L2
M
ID
L3
ass on sampler |j
ID
L4
g
ID
L5
ID
L6
ID
L7
M omitted, dilution volume will be insufficient
64
-------
N Precision standpipe 10%, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
N1
oncentration |j
ID
N2
g/L
ID
N3
Dates
Setup
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Setup
Sampled
External
pressure
bar
-
-
-
-
-
-
O Precision standpipe 10%, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
Sample 1
Date
O1
Concentration ug/L
Sample 2
Date
O2
Sample 3
Date
O3
65
-------
Compound
MTBE
Concentration ug/L
P Precision standpipe 25%, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
P1
oncentration |j
ID
P2
g/L
ID
P3
Dates
Set up
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Set up
Sampled
External
pressure
bar
-
-
-
-
-
-
Q Precision standpipe 25%, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
Sample 1
Date
Q1
Concentration ug/L
Sample 2
Date
Q2
Sample 3
Date
Q3
66
-------
Compound
o-Xylene
m+p-Xylene
MTBE
Concentration ug/L
R Precision standpipe 50%, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
R1
oncentration |j
ID
R2
g/L
ID
R3
Dates
Set up
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Set up
Sampled
External
pressure
bar
-
-
-
-
-
-
S Precision standpipe 50%, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Concentration ug/L
Sample 1
Date
S1
Sample 2
Date
S2
Sample 3
Date
S3
67
-------
Compound
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Concentration ug/L
68
-------
T Precision standpipe 75%, samples
ompound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
ID
T1
Concentrat
ID
T2
ion (jg/L
ID
T3
Dates
Set up
Sampled
Pressure
head
at sep-up
cm
-
-
-
-
-
-
Tem-
pera-
tures
Set up
Sam-
pled
Exter-
nal
pres-
sure
bar
-
-
-
-
-
-
69
-------
U Precision standpipe 75%, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
U1
Concentration ug/L
Sample 2
Date
U2
Sample 3
Date
U3
V Precision standpipe 100%, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
V1
oncentration |j
ID
V2
g/L
ID
V3
Dates
Set up
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Set up
Sampled
External
pressure
bar
-
-
-
-
-
-
70
-------
X Precision standpipe 100%, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
X1
Concentration ug/L
Sample 2
Date
X2
Sample 3
Date
X3
Z omitted, redundant initially.
71
-------
AA Precision field, samples, and groundwater chemistry
Well number
Samples
Compound
Chloroethene
1,1-Dichloroethene
trans-1,2-Dichloroethene
cis-1,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
L sampled (by tracer salt)
Date set up
Date sampled
Temperature, °C
Depth water table set up, mbs
Depth water table sampling, mbs
Depth top sampler, mbs
Depth bottom well, mbs
Pump yield m3/L
AA General chemistry
Parameter
Conductivity
Nitrate
Fluoride
Chloride
Bicarbonate
Sulphate
Value
mS/m
mg/L
mg/L
mg/L
mg/L
mg/L
Parameter
Value
DOC
mg C/L
Iron
mg/L
Ammonium
mg/L
Sodium
mg/L
Potassium
mg/L
Calcium
mg/L
Magnesium
mg/L
72
-------
AA Precision field, reference samples
Well number
Compound
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
AA4
Concentr;
Sample 2
Date
AA5
jtion ug/L
Sample 3
Date
AA6
Sample 4
Date
AA7
73
-------
AB Precision field, samples, and groundwater chemistry
Well number
Samples
Compound
Chloroethene
1,1-Dichloroethene
trans-1,2-Dichloroethene
cis-1,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
L sampled (by tracer salt)
Date set up
Date sampled
Temperature, °C
Depth water table set up, mbs
Depth water table sampling, mbs
Depth top sampler, mbs
Depth bottom well, mbs
Pump yield m3/L
AB General chemistry
Parameter
Conductivity
Nitrate
Fluoride
Chloride
Bicarbonate
Sulphate
Value
mS/m
mg/L
mg/L
mg/L
mg/L
mg/L
Parameter
Value
DOC
mg C/L
Iron
mg/L
Ammonium
mg/L
Sodium
mg/L
Potassium
mg/L
Calcium
mg/L
Magnesium
mg/L
74
-------
AB Precision field, reference samples
Well number
Compound
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
AB4
Concentr;
Sample 2
Date
AB5
jtion ug/L
Sample 3
Date
AB6
Sample 4
Date
AB7
75
-------
AC Precision field, samples, and groundwater chemistry
Well number
Samples
Compound
Chloroethene
1,1-Dichloroethene
trans-1,2-Dichloroethene
cis-1,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
L sampled (by tracer salt)
Date set up
Date sampled
Temperature, °C
Depth water table set up, mbs
Depth water table sampling, mbs
Depth top sampler, mbs
Depth bottom well, mbs
Pump yield m3/L
AC General chemistry
Parameter
Conductivity
Nitrate
Fluoride
Chloride
Bicarbonate
Sulphate
Value
mS/m
mg/L
mg/L
mg/L
mg/L
mg/L
Parameter
Value
DOC
mg C/L
Iron
mg/L
Ammonium
mg/L
Sodium
mg/L
Potassium
mg/L
Calcium
mg/L
Magnesium
mg/L
76
-------
AC Precision field, reference samples
Well number
Compound
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
AC4
Concentr;
Sample 2
Date
ACS
jtion ug/L
Sample 3
Date
AC6
Sample 4
Date
AC7
77
-------
AD Precision field, samples, and groundwater chemistry
Well number
Samples
Compound
Chloroethene
1,1-Dichloroethene
trans-1,2-Dichloroethene
cis-1,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
L sampled (by tracer salt)
Date set up
Date sampled
Temperature, °C
Depth water table set up, mbs
Depth water table sampling, mbs
Depth top sampler, mbs
Depth bottom well, mbs
Pump yield m3/L
AD General chemistry
Parameter
Conductivity
Nitrate
Fluoride
Chloride
Bicarbonate
Sulphate
Value
mS/m
mg/L
mg/L
mg/L
mg/L
mg/L
Parameter
Value
DOC
mg C/L
Iron
mg/L
Ammonium
mg/L
Sodium
mg/L
Potassium
mg/L
Calcium
mg/L
Magnesium
mg/L
78
-------
AD Precision field, reference samples
Well number
Compound
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
AD4
Concentr;
Sample 2
Date
ADS
jtion ug/L
Sample 3
Date
AD6
Sample 4
Date
AD7
79
-------
AE Precision field, samples, and groundwater chemistry
Well number
Samples
Compound
Chloroethene
1,1-Dichloroethene
trans-1,2-Dichloroethene
cis-1,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
L sampled (by tracer salt)
Date set up
Date sampled
Temperature, °C
Depth water table set up, mbs
Depth water table sampling, mbs
Depth top sampler, mbs
Depth bottom well, mbs
Pump yield m3/L
AE General chemistry
Parameter
Conductivity
Nitrate
Fluoride
Chloride
Bicarbonate
Sulphate
Value
mS/m
mg/L
mg/L
mg/L
mg/L
mg/L
Parameter
Value
DOC
mg C/L
Iron
mg/L
Ammonium
mg/L
Sodium
mg/L
Potassium
mg/L
Calcium
mg/L
Magnesium
mg/L
80
-------
AE Precision field, reference samples
Well number
Compound
Chloroethene
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
AE4
Concentr;
Sample 2
Date
AE5
jtion ug/L
Sample 3
Date
AE6
Sample 4
Date
AE7
81
-------
BA Reference robustness lab dispenser, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
BA1
oncentration |j
ID
BA2
g/L
ID
BA3
Dates
Set up
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Set up
Sampled
External
pressure
bar
-
-
-
-
-
-
BB Reference robustness lab dispenser, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
BB1
Concentration ug/L
Sample 2
Date
BB2
Sample 3
Date
BBS
82
-------
CA Sampling depth robustness standpipe, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
CA1
oncentration |j
ID
CA2
g/L
ID
CAS
Dates
Setup
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Setup
Sampled
External
pressure
bar
-
-
-
-
-
-
CB Sampling depth robustness standpipe, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
CB1
Concentration ug/L
Sample 2
Date
CB2
Sample 3
Date
CBS
83
-------
DA Ionic strength robustness lab dispenser, 10 mS/cm, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
DA1
oncentration |j
ID
DA2
g/L
ID
DAS
Dates
Set up
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Set up
Sampled
External
pressure
bar
-
-
-
-
-
-
DB Ionic strength robustness lab dispenser, 10 mS/cm, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
DB1
Concentration ug/L
Sample 2
Date
DB2
Sample 3
Date
DBS
84
-------
EA Ionic strength robustness lab dispenser, 100 mS/cm, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
EA1
oncentration |j
ID
EA2
g/L
ID
EA3
Dates
Setup
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Setup
Sampled
External
pressure
bar
-
-
-
-
-
-
EB Ionic strength robustness lab dispenser, 100 mS/cm, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
EB1
Concentration ug/L
Sample 2
Date
EB2
Sample 3
Date
EB3
85
-------
FA Sampling time robustness lab dispenser, 3 days, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
FA1
oncentration |j
ID
FA2
g/L
ID
FAS
Dates
Setup
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Setup
Sampled
External
pressure
bar
-
-
-
-
-
-
FB Ionic strength robustness lab dispenser, 3 days, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
FB1
Concentration ug/L
Sample 2
Date
FB2
Sample 3
Date
FB3
86
-------
GA Sampling time robustness lab dispenser, 9 days, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
GA1
oncentration |j
ID
GA2
g/L
ID
GAS
Dates
Setup
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
Temperatures
Setup
Sampled
External
pressure
bar
-
-
-
-
-
-
GB Ionic strength robustness lab dispenser, 9 days, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
GB1
Concentration ug/L
Sample 2
Date
GB2
Sample 3
Date
GB3
87
-------
HA Concentration integration robustness, lab dispenser, samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
mL sampled (measured)
mL sampled (by tracer salt)
C
ID
HA1
oncentration |j
ID
HA2
g/L
ID
HAS
Date & time
Start 20%
End 20%
Start 50%
End 50%
Start 80%
End 80%
-
Temperatures
Setup
Sampled
Pressure head
at sep-up
cm
-
-
-
-
-
-
HB Concentration integration robustness, lab dispenser, reference samples
Compound
1,1-Dichloroethene
trans-1 ,2-Dichloroethene
cis-1 ,2-Dichloroethene
Trichloroethene
Tetrachloroethene
Benzene
Toluene
Ethylbenzene
o-Xylene
m+p-Xylene
MTBE
Sample 1
Date
HB1
Concentration ug/L
Sample 2
Date
HB2
Sample 3
Date
HB3
88
-------
APPENDIX 6
Data management
89
-------
In general, the data filing and archiving procedures of the DHI Quality Management
System will be followed.
All data recording and reporting is done in English, communication with Danish ex-
ternal and internal can be in Danish.
Data storage, transfer and control
The data to be compiled and stored are summarized in Table 8.
Analytical raw data will be filed and archived according to the specifications of the
laboratories quality management systems under their ISO 17025 accreditation and are
thus not the concern of DHI staff.
Table 11 Data compilation and storage summary
Data type
Test plan and
report
Test details in
laboratory and
field
Calculations
Analytical re-
ports
Data media
Protected PDF
files
Log book and
pre-pre pared
forms
Excel files
Paper
Data recorder
Test responsi-
ble, DHI
Technician,
DHI
Test responsi-
ble, DHI
Test responsi-
ble, DHI
Data re-
cording tim-
ing
When ap-
proved
During collec-
tion
During calcula-
tions
When received
Data storage
Files and ar-
chives at DHI
Files and ar-
chives at DHI
Files and ar-
chives DHI
Files and ar-
chives DHI
Implementation
All e-mail communication is filed in the Outlook Exchange folders, see below struc-
ture.
The DHI person receiving an e-mail (to field, not cc field) will file the e-mail. The
DHI person sending an e-mail will use the "send and file" option and thereby ensure
prompt filing of all e-mails sent. There is generally no need to widespread cc when
sending e-mails, unless specific action or communication is required.
All paper communication is immediately filed in the binder established by GHE and
available in his office. The title page of the binder will resemble the folder structure at
dkstor, see below.
All recordings during testing in the laboratory or in the field are done in water proof
writing in hardback log-books with all pages numbered page/total page number. The
log books are filed with the staff member using them until the testing is completed,
then with GHE and available at his office.
All data needed for the tests are recorded in the data sheets available from Appendix 5
of the Test Plan. The format can be Word tables, Excel worksheets or paper sheets as
decided by GHE as test responsible. The outline and format are mandatory and can
only be deviated from by recording a deviation with justification, see the Test Plan.
90
-------
All calculations are done using Excel spreadsheets with names identifying the contents
and with headings and notes explaining the calculations.
All electronic files are stored at dkstor in the folder structure shown below. File names
are constructed to identify the contents. Subfolders can be established as found con-
venient, while again constructing folder names that identify the contents. When work-
ing away from network connection (offline), copies of files can be used on own PC,
but the server version is updated and the offline version deleted immediately after re-
turning to network connection.
91
-------
Favorite Links
^, Documents
£ Pictures
^ Music
More »
Name
Folders
I
80137 Sampler education pilot project
80142.MEMBAQ
* 80144.NOWATECH
Center documents
^ Sorbisense documents
Calculation;
External data reports
A ,. Field info
. Wells Glostrup
Wells Statoil
Wells Soborg
Laboratory info
* Jk> Plan & protocol
Obsolete
Review
Reports
jj Drafts
Review
> Jk X-Miscellaneous
> Jl 11093220 (91252] VMG annoncering
11700096_Aftercare
11700116_Modellering_dikloramindannelse
11700363_o verfl a d eaf str.0 m n i n g
2 items
®]Review report Sorbisen,,
te}] Review report Sorbisen..
Offline status: Online
Offline availability: Not available
O 3§ S S E B ^
92
-------
fi| Reports In Public Folders - Microsoft i
File Edit View CJQ Tools Acti
New *• < • , ,'-.'- • :
Folder List
All Folders
All Outlook Items
±1 ^4 80143 - OpenMI LIFE
d _,J 80144 - NOWATECH
Lj. 0 SECRETARIATS FILE
VT^
L J. 1 Administration 8t Coi
^4 10 CEN Workshop
i_4 ^ Client Comrnunicatio
d _ 4 3 Other External Comrr
•ff
^4 Aquateam
^4 Commission
L^ DHI/AU
_ DHl/MMK
^4 Joint verifications
d _4 Sorbisense
_4 External data re
'_4 F'6^ info
_4 Laboratory info
! •- 4 Plan and protocj
_4 Reports
J ^4 TESTNET info
:i -4VTT
L4 4 Internal Com muni cat
I d L4 5 Contract & Invoices
-,< LjiLJ.1"""^'""""^
'i , Mall
93
-------
94
-------
APPENDIX 7
Deviations and amendments
95
-------
96
-------
Deviation reports
The test plan version approved must be followed. If (or rather when) deviations are needed during testing, the deviations are noted and
justified in the format:
Deviation
number
Experiment
label
Test Plan
Table 1
Test method
step
Test Plan
Appendix 3
Deviation
Cause
Impact as-
sessment
Corrective
action, if any
Date
Signature
test or field
responsible
Date
Signature
verification
responsible
Date
Signature
Battelle AMS
QM
The verification protocol version approved must be followed. If deviations are needed during testing, the deviations are noted and justi-
fied in the format:
Deviation
number
Verification
protocol
Chapter
Deviation
Cause
Impact as-
sessment
Corrective
action, if any
Date
Signature
verification
responsible
Date
Signature
internal audi-
tor
Date
Signature
Battelle AMS
QM
Deviation reports are continuously filed in and filed in the appropriate folder at dkstor, see Appendix 6.
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Amendment reports
All changes in the protocol and test plan done in advance of verification and testing
must be done by the document owner (protocol CHG, plan GHE) and approved by the
verification responsible and the internal auditor. Amendments shall be made available
for all involved.
The amendments will mostly have the form of a revised section or chapter of the pro-
tocol or plan, with the below given front page.
Deviation reports are continuously filed in and filed in the appropriate folder at dkstor,
see Appendix 6.
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AMENDMENT
TESTING DOCUMENT TITLE AND DATE:
AMENDMENT NUMBER: _
DATE OF REVISED PART: _
PART TO BE CHANGED/REVISED:
CHANGE/REVISION:
Reference to revised part
REASON FOR CHANGE:
ORIGINATED BY:
DHIWMC Verification or Test Responsible
DATE
APPROVED BY:
DHI WMC Internal Auditor DHI WMC Verification Responsible
DATE DATE
Battelle AMS Center Quality Manager Battelle AMS Center Manager
DATE DATE
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