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Preparatory Commission for the Organisation for the Prohibition of Chemical Weapons

Document number: PC-XIII/B/WP.5
Document date: 16 February 1996
Original: ENGLISH
Corrigenda () have been inserted at the relevant places!

Thirteenth Session (18 - 22 March 1996)


EXPERT GROUP ON INSPECTION PROCEDURES

ELEVENTH REPORT

1. Introduction

1.1 In accordance with the Plan of Activities and Schedule of Meetings for Expert Groups approved by the Commission at its Twelfth Session and contained in the Annex to the Report of the Commission (PC-XII/17), the Expert Group on Inspection Procedures met in The Hague on 12, 13 and 16 February 1996 to continue its work.

1.2 Mr. Sergei Kisselev of the Russian Federation continued as Chairman of the Group. He was assisted by the Chairpersons of the Group's Specialist Task Forces: Dr. Marjatta Rautio of Finland (Analytical Issues), Dr. Eric Wils of the Netherlands (OPCW Analytical Databases) and Dr. Henk Boter of the Netherlands (Inspection Equipment Issues).

1.3 The Group received the reports of its three Specialist Task Forces: Analytical Issues, OPCW Analytical Databases, and Inspection Equipment Issues. The Secretariat re-circulated its position paper entitled "Laying the Foundation for the Implementation of a QA/QC Regime in the OPCW". Copies of these documents are available from the Secretariat on request.

2. Tasks of the Group

    The Group chose to concentrate its work on the following issues drawn from the list of tasks assigned to it by the Commission:

      (a) the reports of its three Specialist Task Forces and related topics;

      (b) the related topics of the list of approved equipment, the definition of a particular type of inspection and the provisions for indicating the specific types of equipment for the specific types of inspection;

      (c) quality assurance/quality control for the Technical Secretariat of the OPCW; and

      (d) possible standards of services as noted in subparagraphs 8.2(b) and 8.2(e) of the Report of the Sixth Meeting of the Finance Group (PC-XI/A/WP.3).

3. Analytical Issues

3.1 The Group received and discussed the report of the Specialist Task Force on Analytical Issues dated 11 January 1996.

3.2 It agreed to adopt the "Standard Operating Procedure for Evaluation of Results of OPCW/PTS Proficiency Tests" (Annex 1 to this Report, including the attached Appendix) and to request Working Group B to take note of it.

3.3 It reviewed the revised document entitled "Performance Rating Criteria for OPCW/PTS Proficiency Testing" and noted the proposed new title "Criteria for the Conduct of OPCW/PTS Proficiency Testing" (Annex 2 to this Report). The Group agreed to approve this revised document and to forward it through Working Group B for adoption by the Commission.

3.4 In accordance with the further recommendations submitted by the Task Force, the Group:

    (a) requested the Secretariat to assist, to the extent that resources could be made available, Finland and the USA in the evaluation and method development for on-site GC/MS analysis and to communicate the result of the development to interested Member States well in advance of the next meeting of this Task Force;

    (b) tasked the Secretariat to send the modified report forms to the laboratories participating in the First Official Proficiency Test not later than four weeks before the start date of the test;

    (c) considered the possible budgetary implications of laboratory proficiency testing and agreed on a number of recommendations (see paragraph 8 of this Report); and

    (d) requested a further three-day meeting for this Specialist Task Force to address the remaining tasks in accordance with the decisions taken by the Twelfth Session of the Commission (PC-XII/17, Annex, Part I, Section BI).

3.5 Upon the request of the Secretariat, the Chairman of the Group drew attention to the following point in relation to the recommendations outlined in subparagraphs 3.4(a) and (b) above, and indicated that, whilst the Secretariat wished to see the issue of the sample preparation methods for the GC/MS resolved, it regretted that, with the impending approach of the trigger point, it did not have sufficient resources to assist in the proposed evaluation and integration process.

3.6 The Group noted that Finland and the United States of America had met and established a joint evaluation protocol for on-site sample preparation methods for use with GC/MS analysis; that the evaluations were scheduled to be completed by the end of May 1996; and that this date coincided with the beginning of the First Official Inter-Laboratory Proficiency Test. The Group requested that the next meeting of the Task Force on Analytical Issues, already mentioned in subparagraph 3.4(d) of this Report, therefore be scheduled some time after the completion of the proficiency test, to enable it to discuss the results of the joint evaluation, including recommendations, if any, on changes to the approved specifications for the sample preparation kit.

4. OPCW Analytical Databases

4.1 The Group received and discussed the report dated 16 January 1996 submitted by the Specialist Task Force on OPCW Analytical Databases and, in accordance with the recommendations of the Task Force:

    (a) approved the results of the evaluation of the NMR and MS spectra (Annex 3 to this Report);

    (b) requested the Secretariat to request Member States to re-submit the approved spectra contained in Annex 3 to this Report in the agreed format;

    (c) requested the Secretariat to send an electronic copy of the re-submitted data for the creation of the electronic database to Finland;

    (d) requested the Secretariat to assemble databases for the evaluation of analytical inspection equipment and for training purposes;

    (e) requested the Secretariat to produce a background paper containing options for the validation of the central OPCW Analytical Database and the on-site analytical databases;

    (f) tasked the Secretariat to forward information, when available, on the on-site data analysis software systems to the Task Force on OPCW Analytical Databases;

    (g) encouraged Member States which have submitted spectral data to send qualified IR specialists to the Task Force on OPCW Analytical Databases for spectral evaluation;

    (h) requested the Task Force on Analytical Issues to adopt the GC recording conditions as contained in paragraph 9 of the report of this Task Force; and

    (i) requested a further three-day meeting of this Task Force in the next intersessional period to address the remaining tasks as contained in the report of the Task Force.

4.2 The Group also requested the Secretariat to report, at its next meeting, on the progress in the development and integration of the central OPCW Analytical Database.

5. Inspection Equipment Issues

5.1 The Group received and discussed the report dated 26 January 1996 submitted by the Specialist Task Force on Inspection Equipment Issues and, in accordance with the recommendations of the Task Force:

    (a) adopted the operational requirements and technical specifications of the inspection equipment item Team Decontamination Kit as included at Annex 4 to this Report;

    (b) revisited the issue of the use of the hydrogen concentration measurement (HCM) non-destructive evaluation (NDE) equipment and agreed that the issue of how HCM, as a possible form of neutron interrogation (NI), could be considered further will be discussed at the next meeting of the Task Force;

    (c) discussed the proposed operational requirements and technical specifications for the Alleged Use Sample Collection Kit (Biomedical Module), at Annex 5 to this Report. The Group approved the technical specifications, pending the outcome of the following procedure, which will allow comments to be made by medical experts from Member States to the Secretariat. If no comment has been received by the Secretariat by 30 April 1996, the specifications will be sent forward to Working Group B to be taken note of. If any comment is received by the Secretariat prior to the 30 April 1996, the Group will return to this issue at its next meeting with a view to finalising it;

    (d) agreed that the question of the role of portable devices for on-site determination of acetylcholinesterase activity, as discussed in paragraph 6 of the report of the Task Force, will be discussed at the next meeting of the Task Force;

    (e) requested the Secretariat, in consultation with Member States, to develop, as soon as practicable, an administrative package addressing the aspect of medico-legal, religious, ethical and chain-of-custody issues and to make the package available to delegations upon request; and

    (f) agreed that the X-ray equipment item will be discussed at the next meeting of the Task Force.

5.2 The Group agreed that, in order to facilitate the resolution of the work on the remaining inspection equipment items (occupational health equipment, HCM equipment, X-ray equipment, as well as possible devices for on-site determination of acetylcholinesterase activity) the Friend of the Chair on Inspection Equipment Issues should hold private consultations with those delegations which had expressed a particular interest in these items prior to the next meeting of the Task Force, which will address these issues.

6. National accreditation for laboratories seeking designation

6.1 At its Sixth Session the Commission adopted the criteria to be used for the designation of laboratories (PC-VI/22, subparagraph 6.4). One of the adopted criteria is that laboratories seeking designation should " . . . have obtained accreditation by an internationally recognised accreditation body for tasks for which they are seeking designation . . . ". Subsequently questions arose within this Group as to what is the precise meaning of this particular requirement, and the Secretariat was requested to prepare a background paper on possible solutions to the problems associated with the national accreditation required for laboratories seeking designation. The Secretariat has not been informed, in writing, by any laboratory or representative of a Member State of problems in this area and therefore has difficulty in taking this matter further. It was, however, suggested that the Secretariat approach the European Cooperation for Accreditation of Laboratories (EAL) and the International Laboratory Accreditation Council (ILAC) to discuss the problem regarding accreditation of laboratories. In the meantime the Secretariat continues to encourage Member States that have problems to present them for discussion.

6.2 The Group discussed the issue of accreditation and agreed that it was necessary to clarify what was precisely meant by the phrase ". . . have obtained accreditation. . .": was this a general accreditation for the analysis of samples related to the Convention or was it accreditation for a specific type of sample or method? The Group requested those Member States whose laboratories have achieved the necessary accreditation to provide the Secretariat and the Group with information on what their accreditation covered and how this was obtained. The Group also requested interested Member States to inform the Secretariat about the substance of any problems that their laboratories seeking designation with the OPCW might experience as regards appropriate accreditation. In the absence of such information the Group felt that it was very difficult to reach a firm conclusion on this issue. The Group recommended that the Secretariat, as a first step, approach the European Cooperation for Accreditation of Laboratories (EAL) and the International Laboratory Accreditation Council (ILAC) to clarify the issue of accreditation of laboratories and requested that the outcome of this contact be presented to, and discussed in, the Task Force on Analytical Issues at its future meeting.

6.3 The Group requested the Secretariat to prepare a discussion paper outlining its views on the scope of activities of designated laboratories, and the role and status of "other laboratories", as reflected in the Annex to PC-VI/B/WP.4, and to present it for consideration by this Group at its next meeting. This paper should also clarify the issue of types of accreditation and possible implications for the laboratory proficiency testing.

7. Transportation-related costs of sample analysis

The Secretariat is consulting Member States which have had some experience in this area with a view to drafting a paper for consideration by this Group. The Group encouraged those Member States with experience in this area to share it with the Secretariat.

8. Conduct of proficiency tests within existing budgetary limits

8.1 The Secretariat was also requested to report on this issue. Since it first raised this issue last year, the Secretariat has received only a few oral comments from Member States. The Secretariat is working on the assumption that EIF might occur at either the end of 1996 or the beginning of 1997. It is also working on the assumption that three official tests will have to be conducted by EIF or shortly thereafter. Switzerland has agreed to prepare the samples and Finland has agreed to perform the evaluation of the test results, free of cost to the Secretariat, for the first of these tests (planned for May 1996). Support for the sample preparation and subsequent evaluation of the analytical results for the second and third tests has been limited. In the absence of further offers from Member States the Secretariat, given the constraints imposed by the 1996 Budget, will have no choice but to seek full cost recovery from the participating laboratories.

8.2 The Republic of Korea announced that its laboratory was prepared to produce one set of test samples at no cost to the Secretariat and provided further information to the Secretariat. France also indicated that it may be in a position to provide support for a further test. The Group again requested those Member States with experience in this field to provide whatever support they can to the Secretariat in the area of sample preparation and evaluation of the test results.

8.3 The Group noted that the Secretariat, in order to avoid the persistence after EIF of this situation and its associated administrative complications, will request that adequate provision be made in the OPCW Budget to cover the cost of proficiency testing. The Group also noted that, after EIF, laboratories participating in proficiency tests would fall into two categories - those already designated and those seeking designation. It would be necessary to consider further whether both types of laboratory should be treated in a similar fashion with regard to covering the cost of the proficiency tests.

9. Logistics of integrating various kits for on-site analysis

The Group noted that the Secretariat considers that this is largely an operational issue for the Secretariat to resolve. In the first instance it will depend on the outcome of the selection process for the on-site analytical method for the GC-MS to be carried out by Finland and USA, which has yet to be completed. The Secretariat is also conducting discussions with manufacturers and vendors on the possibility of integrating some of the kits, and will bring forward a paper for discussion in due course. This will clearly be an interactive process which will last for some time: one important element in this process will be the training of inspectors who are analytical chemists, which will constitute an opportunity to test the results of this integration and, if necessary, to take corrective measures.

10. List of approved equipment for specific types of inspections.

10.1 The Group returned to its discussion of the issue of the list of approved inspection equipment and took the approach suggested in an earlier meeting that this problem could be broken down into the following issues:

    (a) the list of approved inspection equipment;

    (b) the types of inspections; and

    (c) the specific type(s) of equipment for specific types of inspections.

10.2 The Group recalled the need to develop a list of approved inspection equipment in accordance with paragraph 27 of Part II of the Verification Annex for submission to the First Conference of the States Parties.

10.3 Whilst further agreement could not be reached on this occasion the following proposals were received from a number of delegations:

    (a) the types of inspection should be based on those covered by facility agreements (CWSF, CWPF, CWDF, Schedule 1, 2 and 3) and inspections related to old and abandoned chemical weapons, or by some other formulation of category;

    (b) the types of inspections should include inspections in non-declared sites; i.e. challenge inspections (as recorded in paragraph 15 of the Annex to PC-IV/B/WP.7)

    (c) the types of inspection should be based on the Parts of the Verification Annex; and

    (d) there is a need for predictability, transparency and flexibility in the selection of specific types of inspection equipment for particular types of inspection.

11. Quality assurance/quality control

The Group endorsed the conclusions regarding the establishment of a QA/QC regime for the Organisation contained in the report of the Laboratory of the Government Chemist (LGC) contracted by the Commission. This report is available from the Secretariat on request. The Group agreed that the Secretariat take necessary steps, consistent with the 1996 Commission Budget, to start implementing the conclusions contained in the LGC report.

12. "Standards of services"

12.1 This issue was added to the task list of the Group at the request of the Finance Group, which is seeking some clarification of the standards of service to be provided under Part II, paragraph 26. In most cases, after the initial inspection, the services to be provided and the associated reimbursement costs will be clarified by the facility agreement. In the case of initial inspections, however, it might be necessary to agree on some common understandings on the types and quality of services to be provided.

12.2 The Group discussed this issue at some length and came to a general understanding along the following lines:

    (a) inspected States Parties would provide or arrange for accommodation and meals commensurate with what was generally available in the location of the inspection;

    (b) charges for accommodation, meals etc. should also be commensurate with local rates; and

    (c) inspectors should not be unduly discomforted to the extent that this would prejudice the satisfactory conduct of verification activities.

13. Recommendations

13.1 The Group recommended that Working Group B approve and forward to the Commission for adoption the "Criteria for the Conduct of OPCW/PTS Proficiency Testing" (Annex 2 to this Report).

13.2 The Group recommended that Working Group B take note:

    (a) of the "Standard Operating Procedure for Evaluation of Results of OPCW/PTS Proficiency Tests" (Annex 1 to this Report, including the attached Appendix);

    (b) of the results of the evaluation of the NMR and MS spectra (Annex 3 to this Report);

    (c) of the operational requirements and technical specifications of the inspection equipment item Team Decontamination Kit as included at Annex 4 to this Report;

    (d) of the operational requirements and technical specifications of the inspection equipment item Alleged Use Sample Collection Kit (Biomedical Module) (Annex 5 to this Report) on the understanding contained in subparagraph 5.1(c) of this Report;

    (e) of the contents of paragraph 9 of this Report;

    (f) of the decision of the Group recorded in paragraph 11 of this Report; and

    (g) of the general understanding recorded in subparagraph 12.2 of this Report.

13.3 The Group recommended that Working Group B include in the plan of activities and schedule of meetings for the next intersessional period:

    (a) adequate time for this Expert Group to address the remaining issues on its agenda;

    (b) a three-day meeting for the Specialist Task Force on Analytical Issues to address its tasks as mentioned in subparagraphs 3.4(d) and 3.6 of this Report; and

    (c) a three-day meeting of the Specialist Task Force on OPCW Analytical Databases to address its remaining tasks as set out in the report of that Task Force dated 16 January 1996; and

    (d) a two-day meeting of the Specialist Task Force on Inspection Equipment Issues to address its remaining tasks, on the understanding that the decision to hold the meeting will be taken by the Chairman of the Task Force in consultation with interested delegations.

14. Future work

The Group recommended that its work during the forthcoming intersessional period should concentrate on the following issues:

    (a) Tasks identified in the Paris Resolution:

    1. Develop a list of approved equipment in accordance with Part II, paragraph 27, of the Verification Annex (subparagraph 12(e) of the Paris Resolution).

    2. Develop procedures for inclusion in the inspection manual concerning the security, integrity and preservation of samples and for ensuring the protection of the confidentiality of samples transferred for analysis off-site, in accordance with Part II, paragraph 56, of the Verification Annex (subparagraph 12(h) of the Paris Resolution).

    (b) Other priority tasks:

    1. Consider the reports of the Specialist Task Force on Analytical Issues, the Specialist Task Force on OPCW Analytical Databases and the Specialist Task Force on Inspection Equipment Issues.

    2. Develop provisions for indicating the specific types of equipment for the specific types of inspection.

    3. Develop a common understanding of the term "particular type of inspection" and the possible equipment-related consequences of the application of this term.

    (c) Other tasks:

    1. Finalise its recommendation on the adoption of a single standard reference system for geographical co-ordinates to be used by the OPCW.

    2. Elaborate administrative procedures for the conduct of inspections, including the issues of non-scheduled aircraft and communications procedures.

    3. Develop sampling procedures and procedures for on-site and off-site analysis, including sampling and analysis for Schedule 1 chemicals.


    Annex 1

    STANDARD OPERATING PROCEDURE (SOP) FOR EVALUATION OF RESULTS OF OPCW/PTS PROFICIENCY TESTS

    1. Scope

    The aim of OPCW/PTS proficiency tests is to establish and maintain a recognised and transparent methodology for the continued assessment of the technical competence of the participating laboratories. For this reason, every effort shall be made to ensure that the evaluation of results will be uniform and fair for all participating laboratories and that the test interpretation will be consistent and unambiguous. The Secretariat has the responsibility to evaluate the analytical results. If the Secretariat is not in a position to perform evaluation of the analytical results, an accredited (or seeking accreditation) laboratory with demonstrated experience in the analysis of chemicals related to the Convention will be selected to support this process. To facilitate open and transparent testing, the laboratory evaluating the analytical results shall not participate in the same proficiency test. However, such a laboratory must analyse the samples.

    This SOP addresses the following:

      (a) the evaluation of the analytical results; and

      (b) the overall evaluation of the proficiency testing.

    The evaluating laboratory shall evaluate the analytical results obtained by the test participants as set out in paragraph 5 below and the Appendix to this Annex, shall document the evaluation results, and shall report the results to the Secretariat. These activities shall be carried out under the direction of the Secretariat and in accordance with:

      (a) an appropriate quality assurance/quality control (QA/QC) system;

      (b) "ISO Guide 43" and "WELAC Criteria for Proficiency Testing in Accreditation" relevant to evaluation of results for proficiency tests;

      (c) "Criteria for Acceptable Performance of Laboratories in Proficiency Testing" (PC-XI/B/WP.6, Annex 1); and

      (d) an appropriate confidentiality policy required for accreditation.

    2. Contact point

    The Secretariat shall appoint a contact person responsible for coordination of the test.

    3. Information provided by the Secretariat

    The Secretariat shall inform in time agreed upon between the Secretariat and the laboratory evaluating the analytical results of the following:

      (a) the test plan;

      (b) the availability of the test samples to the evaluating laboratory;

      (c) the number of participating laboratories;

      (d) the estimated time within which the analytical results shall be sent for evaluation and the chosen means of transportation; and

      (e) sample composition (test sample preparation and analysis report).

    The delivery of information and reports shall be done in a way which ensures confidentiality.

    4. Reports of the participating laboratories

    The reports from the participating laboratories as well as the report of the sample preparation shall be kept confidential. The Secretariat shall ensure that laboratory identifications have been removed and replaced with laboratory codes in the participants' reports before sending the report copies to the evaluating laboratory. The participating laboratories shall be requested to use the accepted test forms. Measurements carried out on the blank samples[1] shall also be documented on the test forms. When filling out the test forms participants shall be requested:

      (a) to use their laboratory code number and not their names;

      (b) not to provide more or less data than requested (unless asked for during the evaluation phase);

      (c) to number all pages and to indicate the total page number in the beginning of the report; and

      (d) to provide the report as loose sheets.

    When including the supporting analytical data (spectra, chromatograms, etc.) with the test report the participating laboratories shall be requested:

      (a) to delete the names of the laboratory and the analysts;

      (b) to clearly indicate the analytical method, sample code, subsample code and identified chemical(s); and

      (c) to provide copy of sufficient quality for use as supporting analytical data.

    QA/QC data shall be submitted upon request of the Secretariat only. In case additional information not found in the participant report is required for the evaluation, the evaluating laboratory shall contact the Secretariat which shall forward the matter to the laboratory in question and shall forward the answer with participant identification data removed to the evaluator.

    5. Evaluation of analytical results

    The experts responsible for evaluation of analytical results shall verify the correctness of the reported analytical data on the basis of:

      (a) the test sample preparation report;

      (b) the reported analysis information from participating laboratories;

      (c) their experience and knowledge of available state-of-the-art analytical techniques and methods; and

      (d) additional experimental work when required.

    No information other than that found in the participant's report shall be considered. The main emphasis is to assess whether the reported chemicals have been correctly identified and whether the presented data supports the identifications. Each identification shall be backed up by the measurements carried out on the blank samples. Analytical results obtained using different techniques shall also be confirmed and consistent. There must be an unbroken chain of evidence linking each test sample to each chemical identified by a defined method of analysis.

    Furthermore comments shall be given on the possible reasons for false positives and false negatives (e.g. cross-contamination or misinterpretation of analytical data) and the possible reasons for false negatives (e.g. poor separation, unsuitable detection system, lack of reference data). The available equipment and analytical procedures used including the QA/QC procedures shall be assessed to see whether they could explain the mistake.

    The evaluation of the analytical results obtained with the commonly used analytical techniques (i.e. GC, MS, IR and NMR) is described in the Appendix to this Annex. Results obtained by using analytical techniques shall be assessed by an expert in the relevant field in accordance with the guidelines presented in this Appendix.

    5.1 Evaluation of sample preparation

    The effectiveness of the sample preparation methods used to recover the spiking chemicals shall be assessed. Especially, the differences between the recommended procedures (ROPs[2]) and the methods used by a participant should be evaluated with a view to assessing whether possible false negatives can be explained. Possible reported artefacts resulting from sample preparation shall be assessed. The evidence linking each test sample, its sample preparation phases and corresponding subsamples that were analysed shall be assessed. Information provided by the analysis of the corresponding blank samples shall be taken into account as well.

    On the basis of the evaluation the expert shall comment on the possible reasons for false results.

    6. Evaluation report of analytical results

    The evaluation of the results of the participants shall start as soon as the evaluating laboratory obtains the set of complete participant reports from the Secretariat. The evaluation report of analytical results shall be submitted within four weeks to the Secretariat. The Secretariat shall compile and produce the preliminary proficiency test report. The Secretariat shall submit this preliminary report to the participating laboratories for comment. The laboratory evaluating the results shall check the comments received from participating laboratories and shall make the necessary corrections to the evaluation report. Then the final analytical evaluation report shall be submitted to the Secretariat for further actions.

    7. Assessment of the proficiency test

    The Secretariat shall make an assessment of the applicability of the test prior to reaching its final conclusions on the performance of individual laboratories participating in the proficiency test. The applicability of the test shall be judged on the basis of the sample preparation and analysis report, the analytical evaluation report, and the test plan, including the test scenario, the timetable, and other relevant matters sent to participants before the test start. The test samples shall be accepted as equivalent for all participating laboratories with respect to the chemicals in question when:

      (a) the concentration range of spiking chemicals corresponds to the one agreed for the proficiency tests;

      (b) the samples can be regarded as sufficiently homogeneous; and

      (c) the reported degradation can be found acceptable within the test scenario.

    The chemicals shall be categorised in accordance with the test scenario as spiking chemicals, as degradation products, as non-relevant chemicals, and as false positive chemicals. The performance of participating laboratories shall be assessed on the basis of "Criteria for Acceptable Performance of Laboratories in Proficiency Testing" (PC-XI/B/WP.6, Annex 1). The Secretariat shall calculate a score on the basis of final results for each participating laboratory fulfilling the required performance criteria.

    8. Proficiency test report

    The Secretariat shall compile a full proficiency test report including:

      (a) evaluation of participating laboratories' performance and scoring;

      (b) sample preparation and analysis information; and

      (c) information on evaluation of analytical results.

    The Secretariat shall provide a preliminary version of the proficiency test report for participating laboratories. Participating laboratories are given a minimum of one week to inform the Secretariat whether they accept the proficiency test evaluation results and to provide their comments on the preliminary report. Comments shall be assessed by relevant experts and incorporated in the final report as appropriate.

    9. Follow-up actions

    The Secretariat shall inform the appropriate laboratory of the errors (false positives and negatives) that may have occurred. The Secretariat shall request information on remedial actions taken by the laboratory. The participating laboratory in question shall submit a full report to the Secretariat stating the cause of the problem and remedial actions taken before their participation in another test. Depending on the problem, the evaluating laboratory may be asked to provide an expert opinion on whether or not the remedial actions taken by the participating laboratory are found to be effective and to submit this report to the Secretariat for further action.

    10. Additional information

    1. Nomenclature of Interlaboratory Analytical Studies (IUPAC Recommendations 1994).

    2. ISO Guide 43, Development and Operation of Laboratory Proficiency testing, ISO/IEC Guide 43-1984 (E).

    3. WELAC Criteria for Proficiency Testing in Accreditation, WELAC Guidance Document No. WGD 4, Final proposal June 1993.

    4. AOAC Official Methods of Analysis, Appendix: Guidelines for Collaborative Study Procedure to Validate Characteristics of a Method of Analysis.

    5. Thompson M., Wood R., J. AOAC Int. 76 (1993) 926. "International Harmonised Protocol for Proficiency Testing of (Chemical) Analytical Laboratories".


    Appendix

    1. Chromatographic techniques and capillary zone electrophoresis

    Results of chromatographic techniques such as gas chromatography (GC) and liquid chromatography (LC) techniques, and capillary zone electrophoresis (CZE) shall be checked that they support the correct identification. The evaluating laboratory shall check that each method reported is named; described in sufficient detail as described in the test forms and that representative chromatograms or electropherograms are found to support results obtained for each sample.

    1.1 Evaluation of gas chromatographic (GC) analyses

    Gas chromatographic data shall be evaluated to assess whether the available equipment and procedures used allow separation and detection of the spiking chemicals. It shall be clear which samples (and which subsample solutions) have been analysed by which method. A representative chromatogram shall be found to support findings from each subsample solution of which the detection was made and corresponding blank subsample solution.

    2. Evaluation of mass spectrometric (MS) analyses

    Mass spectrometric data is evaluated to assess whether the spectra correspond to the proposed chemicals. The evaluating expert shall check whether each mass spectrometric method reported to be used by a participant is described in sufficient detail; whether it is clearly linked using appropriate names to a corresponding gas chromatographic or liquid chromatographic method; whether a representative spectrum is found to support identification of each chemical found from each sample; and whether a reference spectrum and/or spectral interpretation is found to support each identified chemical. When evaluating the mass spectral data the following features shall be checked:

      (a) is the full mass spectral region presented for the proposed chemical consistent with identified chemicals?

      (b) is the retention data in the applied GC or LC conditions consistent with the identified chemical?

      (c) are all ions belonging to the proposed structure present?

      (d) are the isotopic ion ratios appropriate?

      (e) are any impurity peaks present?

      (f) does the spectrum correspond with the ionisation method used (e.g. in CI; M+1, adduct ions) or analysis mode (e.g. MS/MS)?

      (g) the quality of reference data used (which database was used, is the spectrum correct, what kind of reference material was used to produce an authentic reference spectrum?) Is the information sufficient?

      (h) in case of spectral interpretation, is the information sufficient for identification? Are the mass fragments found credibly explained by spectral interpretation?

    3. Evaluation of infrared spectrometric (IR) analyses

    The infrared spectrometric data shall be evaluated to assess (i) whether the quality of spectra and the information obtained is sufficient for identification, (ii) how the identification was made, and (iii) whether the data can only be considered to support identification made by other techniques. The expert shall check whether each IR method reported to have been used by a participant is described in sufficient detail and, if applicable, whether it is clearly linked using appropriate names to a corresponding gas chromatographic method; whether a representative spectrum is be found to support identification of each chemical found from each sample; and whether a reference spectrum and/or spectral interpretation is found to support each identified chemical. When evaluating the IR spectra, the following features shall be assessed:

      (a) is the spectral range (e.g. 4000-700 cm-1) presented adequate for the proposed structure?

      (b) in the case of GC-FTIR, is the retention data in the applied GC-conditions consistent with the identified chemical ?

      (c) are all significant bands present?

      (d) are any impurity bands present?

      (e) the quality of reference data used (which database was used, is the spectrum correct, what kind of reference material was used to produce an authentic reference spectrum?) Is the information sufficient?

      (f) in case of spectral interpretation is the information sufficient for identification? Are the bands found credibly explained by spectral interpretation?

    4. Evaluation of nuclear magnetic resonance (NMR) spectrometric analyses

    The NMR spectrometric data shall be evaluated to assess whether the quality of spectra and the information provided are sufficient for identification, how the identification was made, or whether the data can only be considered to support identification made by other techniques. The expert shall check whether each NMR method reported to have been used by a participant is described in sufficient detail; whether a representative spectrum is found to support identification of each chemical found from each sample; and whether a reference spectrum and/or spectral interpretation is found to support each identified chemical. When the NMR spectral data is being evaluated, the following features shall be assessed:

      (a) are all significant resonances revealed or do resonances of other chemicals in the same sample overlap?

      (b) are the effects of solvent, concentration, pH, and the chemical shift reference taken into account?

      (c) are comparable resonances found in the sample spectrum and reference spectrum? Are the resonances found credibly explained by spectral interpretation (chemical shifts, coupling constants)?

      (d) the quality of reference data used (is the spectrum correct, has it been acquired under the same conditions, what kind of reference material was used to produce an authentic reference spectrum, does the published data support spectral interpretation?). Is the information provided sufficient for interpretation?


    Annex 2

    CRITERIA FOR THE CONDUCT OF OPCW/PTS PROFICIENCY TESTING

    1. Introduction

    One of the criteria for laboratories seeking designation for the analysis of authentic samples is that those laboratories should regularly participate and perform successfully in inter-laboratory proficiency tests (PC-VI/B/WP.4). Criteria for acceptable performance of laboratories in a single proficiency test have been established (PC-XI/B/WP.6, Annex 1) and adopted by the Commission.

    Proficiency testing is conducted by the Secretariat. In this process the Secretariat may be assisted by laboratories preparing the test samples and evaluating the results in accordance with the following standard operating procedures (SOPs):

      (a) "Standard Operating Procedure (SOP) for Preparation of Test Samples for OPCW/PTS Proficiency Tests"; and

      (b) "Standard Operating Procedure (SOP) for Evaluation of Results of OPCW/PTS Proficiency Tests".

    As these assisting laboratories may be seeking designation for the analysis of authentic samples, their position in respect of their intention to become an OPCW designated laboratory needs to be considered.

    In relation to the conduct of proficiency testing this paper addresses the following:

      (a) the role of the Secretariat;

      (b) the number of tests to be performed before applying for designation;

      (c) the evaluation of laboratories for a series of tests; and

      (d) considerations for laboratories preparing the test samples and evaluating the results.

    2. The role of the Secretariat

    The Secretariat shall inform the proficiency test participants before the test of the purpose and the scenario of the test. After completion of the test by the participating laboratories, the Secretariat has the responsibility for evaluating the results of the proficiency test. Prior to drawing any conclusions on the performance of individual laboratories participating in the proficiency test, the Secretariat shall make:

      (a) an assessment of the stability, quality and validity of the test samples to assess the applicability of the test ; and

      (b) an assessment of the evaluation of the results of the test .

    Then the Secretariat shall make a preliminary evaluation based on the "Criteria for Acceptable Performance of Laboratories in Proficiency Testing":

      (a) evaluation of whether each of the participating laboratories fulfils all performance criteria; and

      (b) scoring of the performance of those laboratories fulfilling all performance criteria in accordance with the scoring rules.

    The Secretariat shall prepare a preliminary test report based on all above-mentioned data and shall thereafter inform the participants of their performance and shall request comments. The participants shall be given a minimum of one week to inform the Secretariat whether they accept the performance evaluation. The Secretariat shall inform the evaluating laboratory about the comments received concerning the evaluation of analytical data to allow it to take corrective measures if needed and to finalise its report. The Secretariat will finalise its test report on the basis of these results.

    3. Number of proficiency tests to be performed before applying for designation

    Applications by laboratories seeking designation for the analysis of authentic samples must be based on participation in at least three proficiency tests, and must take into account the following:

      (a) laboratories must have participated in at least three out of the last five proficiency tests; and

      (b) laboratories must have performed successfully in their last three consecutive proficiency tests.

    4. The evaluation of laboratories for a series of proficiency tests

    Since test scenarios, number of spiking chemicals, samples and matrices vary between proficiency tests, a straightforward addition of scores achieved from different tests will not lead to fair or meaningful assessment of participating laboratories. The evaluation of laboratories over a series of proficiency tests shall be carried out as follows:

      (a) once all the performance criteria have been fulfilled, the scoring rules as presented in "Criteria for Acceptable Performance of Laboratories in Proficiency Testing" shall be applied separately for each proficiency test for measuring the performance in an individual test (see table below);

      (b) the performance of laboratories in an individual test shall be rated as presented in the table below to allow for a comparison of performance in a number of different proficiency tests in a simple and unambiguous way;

      (c) the performance rating for three individual tests shall be combined and shall form the technical basis on which the Director-General may grant designation for the analysis of authentic samples provided that other criteria (quality assurance, accreditation) have been fulfilled; and

      (d) the combined rating shall be used as a basis on which the Director-General shall classify laboratories consistent with their capabilities to support the analytical needs of the Convention.

    Table. Method of evaluating laboratory performance.

    Performance criteria fulfilled [3]Identification of chemicalsPerformance scoring [4]Performance rating
    YesLaboratory identifies all chemicalsMaximum score A
    YesLaboratory identifies all chemicals except oneMaximum score minus twoB
    YesLaboratory identifies more than half of the chemicalsScore between zero and maximum minus twoC
    YesLaboratory misses more chemicals than it identifiesNegative scoreD
    No.No score Failure

    5. Considerations for laboratories preparing the test samples and evaluating the results

    The Secretariat shall consider the laboratories assisting it in preparing the samples or evaluating the analytical results and which are also in the process of seeking designation for the analysis of authentic samples as follows:

      (a) laboratories preparing the samples shall be credited with a maximum performance rating of A (see table) for one proficiency test if the test samples meet the requirements of the "Standard Operating Procedure (SOP) for Preparation of Test Samples for OPCW/PTS Proficiency Tests";

      (b) laboratories evaluating the analytical results shall be credited with a maximum performance rating of A (see table) for one proficiency test if the evaluation meets the requirements of the "Standard Operating Procedure (SOP) for Evaluation of Results of OPCW/PTS Proficiency Tests";

      (c) laboratories cannot use performance rating for preparing the samples or evaluating the analytical results of more than one of their last three consecutive proficiency tests (i.e. laboratories must participate in at least two of the three tests as regular participants); and

      (d) laboratories preparing the samples or evaluating the analytical results cannot participate as regular participants in a given test. However, such laboratories must analyse the samples.


    Annex 3

    RESULTS OF THE EVALUATION OF MS AND NMR SPECTRA

    LIST OF CHEMICALS WITH APPROVED MS SPECTRA

    Chemical nameCAS numberSpectrum numberSchedule numberNumbers of already approved spectra
    Ethyl ethylphosphonofluoridate650-20-41_2_481.A.15-2-15, 7-2-15
    Isopropyl ethylphosphonofluoridate1189-87-31_2_491.A.15-2-17, 7-2-17
    Cyclohexyl ethylphosphonofluoridate7284-84-61_2_501.A.15-2-24
    1,2,2-trimethylpropyl ethylphosphonofluoridate97931-20-91_2_511.A.15-2-21
    2-methylcyclohexyl ethylphosphonofluoridate.1_2_521.A.1.
    Isopropyl isopropylphosphonofluoridate665-33-81_2_541.A.1.
    Cyclohexyl isopropylphosphonofluoridate.1_2_551.A.1.
    2-methylcyclohexyl isopropylphosphonofluoridate.1_2_571.A.1.
    Cyclohexyl n-propylphosphonofluoridate28364-21-81_2_601.A.1.
    1,2,2-trimethylpropyl n-propylphosphonofluoridate.1_2_611.A.1.
    2-methylcyclohexyl n-propylphosphonofluoridate.1_2_621.A.1.
    Cyclopentyl methyl methylphosphonate.1_2_632.B.46-2-47
    Cyclopentyl 2-methoxyethyl methylphosphonate.1_2_642.B.4.
    Methyl n-propyl methylphosphonate.1_2_662.B.4.
    2-methoxyethyl n-propyl methylphosphonate.1_2_672.B.4.
    Benzyl n-butyl methylphosphonate.1_2_692.B.4
    Di-n-propyl N,N-dimethylphosphoramidate.2_2_742.B.6.
    Di-n-butyl N,N-dimethylphosphoramidate.2_2_762.B.6.
    Di-n-pentyl N,N-dimethylphosphoramidate.2_2_772.B.6.
    Di-n-octyl N,N-dimethylphosphoramidate.2_2_822.B.6.
    Di-n-hexyl N,N-dimethylphosphoramidate.2_2_842.B.6.
    Di-n-heptyl N,N-dimethylphosphoramidate.2_2_862.B.6.
    Thiodiglycol111-48-813_2_12.B.135-2-70, 6-2-135, 7-2-126
    Dimethyl methylphosphonate756-79-613_2_22.B.45-2-53, 7-2-106
    3-quinuclidinol1619-34-713_2_42.B.96-2-191
    Ethyl methyl methylphosphonate18755-36-713_2_62.B.45-2-54, 6-2-43, 7-2-110
    2-diisopropylaminoethanol96-80-013_2_72.B.116-2-113
    Mustard gas505-60-213_2_91.A.41-2-20, 4-2-7, 5-2-46, 7-2-50
    Diisopropyl methylphosphonate1445-75-613_2_112.B.45-2-57, 7-2-108
    Methyl pinacolyl methylphosphonate7040-59-713_2_142.B.45-2-56, 6-2-45, 7-2-113
    Sesquimustard3563-36-813_2_161.A.45-2-47, 6-2-124, 7-2-51
    Dimustard ether63918-89-813_2_181.A.41-2-23, 7-2-52
    Di-n-octyl methylphosphonate1832-68-413_2_202.B.46-2-236
    Diisopropyl methylthiophosphonate66295-45-314_2_12.B.4.
    Isopropyl methyl methylthiophosphonate.14_2_22.B.4.
    Methyl pinacolyl methylthiophosphonate.14_2_32.B.4.
    Cyclohexyl isopropyl methylthiophosphonate62507-66-814_2_42.B.4.


    LIST OF CHEMICALS WITH APPROVED NMR SPECTRA

    Spectrum numberChemical nameCAS numberSchedule numberNucleus
    6-3-209Cyclopentyl S-2-diethylaminoethyl methylphosphonothiolate93240-66-51.A.(3)1H
    6-3-210Cyclopentyl S-2-diethylaminoethyl methylphosphonothiolate93240-66-51.A.(3)13C
    6-3-216Tris(2-chloroethyl)amine HCl817-09-41.A.(6)1H
    6-3-218Tris(2-chloroethyl)amine HCl817-09-41.A.(6)13C
    6-3-222Pinacolyl alcohol464-07-32.B.(14)13C


    Annex 4

    TEAM DECONTAMINATION KIT

  1. Purpose

    To be used for field decontamination of the inspection team and decontamination of their equipment contaminated or suspected of being contaminated with chemical weapons in solid, liquid or aerosol form.

  2. Operational requirements

      (a) Must be able to decontaminate under field conditions independent of the on-site infrastructure.

      (b) Could be assembled in a modular concept to allow for flexibility with different combinations of equipment.

      (c) Must allow for safe transport by means of commercial passenger and cargo aircraft. For this kit there is no requirement for the return transport of used or contaminated materials.

      (d) Must at least be capable of decontaminating all items that have been exposed to Schedule 1 chemicals, especially when used as chemical weapons, to an extent that treated items do not constitute an appreciable risk.

  3. Technical specifications

      (a) The kit must at least comprise the following items:

        (i) a one-person-portable spray unit of no more than 25 kg;

        (ii) a selection of brushes for various surfaces;

        (iii) a supply of up to 10 kg (in units of 1 kg) of decontaminant, in either powder or concentrated form;

        (iv) a supply of up to 10 kg (in units of 1 kg) of sorbent material such as fuller's earth and activated charcoal;

        (v) a selection of chemical resistant containers for decontamination solution;

        (vi) a set of preferably collapsible containers sufficient to contain at least 60 litres of water;

        (vii) two containers for transportation of organic solvents, each of at least 5 litres;

        (viii) no container should hold more than 20 litres.

      (b) The kit must have a shelf life of at least five years.


Annex 5

ALLEGED USE SAMPLE COLLECTION KIT

Module for Collection of Biomedical Samples

  1. Operational requirements

      (a) Must allow for the collection, preservation and safe transportation of biomedical samples.

      (b) Must allow for safe containment of sharp items and biologically contaminated items.

      (c) Must allow for field separation of serum, plasma and red blood cells.

      (d) Must allow for biomedical sampling of at least 20 subjects.

      (e) Must provide blood collection tubes for clotted and whole blood.

      (f) Relevant items must be packed sterile and maintained as such during storage and transportation.

  2. Technical specifications

    The standard kit must contain the items as listed below. Packaging must allow for the inclusion of additional equipment supplies that might be required for specific circumstances.


/TR> 25
ItemNo. of items
Reusable items.
Portable centrifuge for blood sample separation, either power or hand operated - 4 tube capacity1
Portable fridge/freezer unit, with temperature recording ability and variable temperature control to a maximum of -10ºC.1
Scalpel handle (blade holder), no.31
Forceps, haemostatic, curved, 15 cm2
Forceps, splinter, tweezers type1
Forceps, tissue, toothed, 18 cm1
Scissors, general surgical, straight, one blunt point, one sharp point, 12.5 cm1
Scissors, general surgical, straight, two sharp points, 12.5 cm1
Scissors, heavy duty trauma, 12.5 cm1
Needle holder, straight, 15 cm1
Kidney dish, stainless steel, 15cm1
Dish, stainless steel, rectangular, approx. 25 cm x 10 cm x 3 cm1
Tourniquet2
Splash protection goggles2
Tight sealing container for preservative/sterilising fluid, 1 litre3
Robust container for transport of kit1
Approved container for transporting ambient or frozen biological specimens, capable of being used with OPCW seals5
..
Disposable items.
Sterile surgical gloves, sizes 7, 71/2, and 84 (of each size)
Disposable surgical mask4
Disposable plastic apron2
Plastic urine collection bottles
Evacuated glass blood collection tubes for clotted blood, 10 ml25
Evacuated glass blood collection tubes for clotted blood, 5 ml25
Evacuated glass blood collection tubes for whole blood, EDTA, 5 ml25
Evacuated glass blood collection tubes for whole blood, heparinised, 5 ml25
Evacuated glass blood collection tubes for the separation of blood25
Bottles - glass, clear, wide mouthed, with Teflon lined screw caps, 25 ml10
Bottles - glass, clear, wide mouthed, with Teflon lined screw caps, 100 ml10
Glass slides for preparation of blood smears50
Cover slips for slide preparations1 box
Plastic holder for prepared slides, screw top 2
Sterile needles for vacutainer closed blood collection system25
Needle and tube holder for vacutainer collection system4
Sterile needles, 18G and 21G10 of each size
Sterile syringes, 2 ml, 5 ml, 10 ml10 of each size
Sterile syringes, 20 ml5
Glass transfer pipettes with suction top10
Dressing sheet, 60 x 80 cm2
Sterile throat swabs20
Tongue depressors10
Alcohol swabs for skin cleansing25
Soap, liquid, anti microbial (100 ml in plastic bottle)1
Elastoplast, band-aid type25
Elastoplast, roll, 6 cm width1
Bags, sealable, 20 x 30 cm25
Tamper indicating seals1 roll
Self-adhesive labels5 sheets
Clipboard1
Pens, indelible, ball-point2
Pens, permanent white board type2
Scalpel blades, sizes 10, 12, 222 each
Suture pack (assorted sterile sutures)1
Skin biopsy unit1
Lumbar puncture unit1
Container for safe containment of sharp items1
Containers for the safe primary containment of samples20
Plastic garbage bags2
Sterilising fluids11
Preservative solutions11
Brush (for cleaning instruments)1
Administrative package catering for medico-legal, religious, ethical and chain of custody considerations*1
* To be developed by the Secretariat

- - - o - - -


FOOTNOTES

  1. A blank sample sent together with the corresponding test sample provides the participant with the sample matrix or background without the spiking chemicals. The blank sample should be analysed together with and in the same way as the test sample in order to eliminate and warn of possible errors, such as cross contamination. In principle a chemical that is found both in the sample and in the blank sample in corresponding concentration levels should not be regarded as a spiking chemical. Proper use of blank samples is a part of quality assurance/quality control of an analysis.

  2. The Ministry for Foreign Affairs of Finland, Recommended Operating Procedures for Sampling and Analysis in the Verification of Chemical Disarmament, 1994, Ed. M. Rautio, ISBN 951-724-008-2
  3. See PC-XI/B/WP.6 Annex 1, paragraph 2.
  4. For practical application of the scoring rules reference is made to the Note by the Executive Secretary on the Results of the Third Commission Inter-Laboratory Comparison Test: Trial Proficiency Test (PC-XII/B/3).