GSR PT Proficiency Test On Detection And Identification Of .

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GSR PT – Proficiency Test on Detection andIdentification of Gunshot Residue Particlesby SEM/EDS according to ASTM E1588Scheme DescriptionIn cooperation with the ENFSI expert working group Firearms/GSR

ImprintQuoData GmbHQuality & Statistics!Prellerstr. 1401309 DresdenGermanyPhone: 49 (0) 351 40 28867 0Fax: 49 (0) 351 40 28867 .de/gsr-quality-scheme.phpAuthorsPD Dr. habil. Steffen UhligDipl.-Psych. Kirsten SimonDipl.-Math. Kirstin FrostDr. Tina FichtnerDr. Ludwig Niewöhner (German Federal Criminal Police Office, BKA)January 2021

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme DescriptionContents12345Introduction .41.1Quality Standards .41.2Aims of the Scheme .41.3List of Abbreviations .4Scheme Organisation and Management .52.1Announcement .52.2Website and Notification .52.3GSR PT Online Portal .52.4Establishment of an Advisory Board .62.5Timescales.72.6Frequency of Participation .82.7Confidentiality .82.8Subcontracting services .82.9Scheme Development .82.10Potential major sources of errors .9Test Material .103.1Test Material Preparation .103.2Quality Control .103.3Distribution .103.4Sample Properties .10Analysis and Reporting of Results .114.1Methods of Analysis .114.2Performance of the Test .114.3Data Reporting .124.4Reporting Format .124.5Late Return of Results .12Performance Assessment .135.1Preparation of Raw Data and Plausibility Check .135.2Cross-Checking .135.3Statistical Analysis .145.3.16Assessment of laboratory’s performance . 145.3.1.1On the basis of the detection capability . 145.3.1.2On the basis of the number of correctly detected PbSbBa-particles . 145.3.2Overall performance . 155.3.3Additional analyses . 155.3.3.1Correlation of laboratory performance between two PT rounds. 155.3.3.2Bias analysis . 155.3.3.3Other additional analyses . 165.4Final Report of Results and Individual Certificates.165.5Complaints .16References and Sources of Information .17QuoData GmbHPage 3 of 17

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description1Introduction1.1Quality StandardsProficiency testing (PT) is defined by ISO/IEC 17043:2010 [1] as the use of interlaboratory comparisonsfor the determination of the performance of individual laboratories in specific tests or measurements andfor the monitoring of the laboratories’ long-term performance.When carried out within the context of a comprehensive quality assurance programme, proficiencytesting is an independent means of reflecting the quality of test and calibration results, as described byISO/IEC 17025 [2].All the schemes within QuoData GmbH are operated in accordance with the international guidesISO/IEC 17043:2010 and ILAC G13:2007 [3]. Furthermore, especially the forensic GSR scheme isoperated in accordance with the ENFSI Guidance document [4].1.2Aims of the SchemeThe aim of the GSR-QS (Quality Scheme on the Detection and Identification of Gunshot Residue) is toenable laboratories to undertake forensic GSR examinations using automated SEM/EDS techniquesaccording to ASTM E1588 [5], to monitor and improve the quality of their measurements. The schemeenables laboratories to demonstrate the quality of their measurements to accreditation bodies and otherappropriate authorities. This scheme is designed for 50 to 1000 expected participants annually.1.3List of AbbreviationsAbbreviationMeaningBSEBackscattered electronsEDSEnergy dispersive X-ray spectroscopy (also known as EDX)ENFSIEuropean Network of Forensic Science InstitutesEWGExpert working groupGSRGunshot residuePTProficiency testQCQuality controlQSQuality scheme on the detection and identification of gunshot residueSEMScanning electron microscopeTORTerms of referencePage 4 of 17QuoData GmbH

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description2Scheme Organisation and Management2.1AnnouncementAnnually, a scheme application form is available on the website of the QuoData GmbH (as given inSection 2.2), containing information about the test materials included in the scheme, and the intendeddistribution dates. To participants that attended the scheme in former years, an email with theannouncement of the current scheme will be sent. New participants are invited to complete anapplication form on the website of the QuoData GmbH, indicating their interest. However, the finaldecision about participation lies in the responsibility of the Advisory Board.Additionally, the current scheme may be announced in proficiency scheme databases (e.g. EPTIS) onthe internet.2.2Website and NotificationAll deadlines will be published on the non-restricted website of the QuoData y-scheme.htmlAll important changes in the timescale will be announced by email as well as on the website.2.3 GSR PT Online PortalSince 2019, the GSR profiency tests are managed via the GSR PT Online Portal available athttps://gsr.quodata.de.Each participant has a separate account, where the data reported as well as the final reports of results,the individual results plots as well as the individual certificates of the respective participant’s institutionare made available. Access to the documents is possible at any time – for all PT rounds participated infrom 2019.The enrollment for a GSR PT round is also done via the GSR PT Online Portal – so far the interestingparticipant is already registered.The registration for the GSR PT Online Portal is possible via an online application form provided here:https://gsr.quodata.de/pt-participant/lab applicant/addQuoData GmbHPage 5 of 17

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description2.4Establishment of an Advisory BoardGSR-QS is managed and operated by QuoData GmbH. Technical direction and advice is provided byan Advisory Board, consisting of at least two representatives of the ENFSI Expert Working GroupFirearms/GSR (ENFSI-EWG).The members of the Advisory Board are Ludwig Niewöhner, PhDForensic Science Institute, BKA, 65193 Wiesbaden, Germany. Amalia Brouwer-Stamouli, PhDNetherlands Forensic Institute, NFI, 2490 AA The Hague, Netherlands.The Advisory Board may seek advice from other organisations/individuals with specific expertise on anad hoc basis. The membership of the Advisory Board is reviewed on a regular basis.QuoData GmbH is responsible for the planning of the proficiency test scheme, the evaluation ofperformance, and the authorization of the final report, according to ISO 17043. In addition, QuoDataGmbH manages also the day-to-day operation of the scheme, including sample purchase andpreparation, dispatch, data processing, reporting of the results in a final report, and providing individualcertificates.The terms of reference (TOR) of the Advisory Board are: To consider the scope and direction in which the scheme should develop. To represent the views of the ENFSI EWG. To provide specialist advice to the scheme organisers on technical and other matters, tocontribute to a smooth performance of the scheme. To assess the results obtained in the scheme and examine the implications they have for theprogress of the scheme. To consider the nature and timing of proficiency testing rounds and to decide on the testmaterials to be used. To assist in the revision of the scheme description. To advise on the promotion and publicity of the scheme. To provide, when requested, expert advice to participants on specific analytical difficultiesencountered in the scheme. To discuss technical comments on each round for inclusion in the report.The Advisory Board will meet when necessary to ensure progression of the scheme, but at least oncea year.Page 6 of 17QuoData GmbH

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description2.5TimescalesThe scheme is operated once a year. Test materials are distributed to participants annually, withdistribution dates published on the website of the QuoData GmbH1. Samples are dispatched no laterthan the announced dates specified on the website. After the dispatch of the samples, laboratories haveapproximately four weeks in which to analyse the samples and report their results.Dates of the reporting deadlines are also available on the website of the QuoData GmbH1.The structure within the scheme round is as follows: Procurement, preparation, dispensing and quality control testing of test materials. Dispatch of test materials and instructions to participants. Request to participants to analyse test materials and report results to QuoData GmbH asinstructed and within the specified deadline. Data preparation and plausibility check by QuoData GmbH. Cross-check and possible corrections of results by laboratories. Analysis of results and comparison of performance of laboratories using appropriate techniques,such as 𝑧 scores. Distribution of final report of results and individual certificates to participants. Review of PT round and identification of requirements for subsequent PT rounds. Start of the subsequent PT round.The final report of results is issued as soon as possible after the round closure, although the timescalebetween closing dates and issue of final report of results can vary from round to round.All important changes in the timescale will be announced by email as well as on the website of theQuoData ity-scheme.htmlQuoData GmbHPage 7 of 17

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description2.6Frequency of ParticipationAs part of a comprehensive quality assurance programme, and to gain most benefit from trend analysis,an annual participation in the proficiency test is recommended.2.7ConfidentialityIn order to ensure confidentiality, a unique laboratory reference number (Lab ID) is allocated to eachparticipant in all PT rounds, where the Lab IDs differ from round to round per participant. This Lab IDenables results to be reported without divulging the identities of participant laboratories.In cases where anonymity could not be preserved, laboratory reference numbers may be changed onrequest from the participating laboratory, at the discretion of QuoData GmbH.For some PT rounds, participants may select to have their identity made known to others, but this willonly be done with the knowledge and full permission of the participant.2.8Subcontracting servicesVarious aspects of the GSR PT scheme can from time to time be subcontracted. When subcontractingoccurs, it is placed with a competent subcontractor and the proficiency testing provider is responsiblefor this work.2.9Scheme DevelopmentQuoData GmbH is continually striving to improve the proficiency test and to introduce newrecommendations where appropriate. This will be accomplished in close collaboration with the AdvisoryBoard.Page 8 of 17QuoData GmbH

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description2.10 Potential major sources of errorsThe potential major sources of errors involved in the area of proficiency testing are offered in Table 1.Table 1: Potential major sources of errors in the GSR PT programNo.123PhasePreparation of samplesDispatch of test samplesto the participantsMeasuring errors at theparticipants’ siteLabelPotential error in each phaseavarying of coating parametersberrors in the data conversion for the mask productioncmissing particlesadefect or damage of the test samples during thetransportawrong alignment of the sample on the SEM/EDSbunsuitable choice of parameters during the measurementprocesscno usage of the Standard Operating Procedure (SOP) formeasuring the sample4Submission of data bythe participantsasubmission of incomplete data sets5Data preparation andplausibility checkaerrors in the data submission process by the participants6Generation of the finalreport of resultsawrong transfer of the data (tables, graphics) into the finalreport of results7Generation of theindividual certificatesawrong transfer of the laboratory specific results into theircertificatesQuoData GmbHPage 9 of 17

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description3Test Material3.1Test Material PreparationWherever practical, test materials should be as similar as possible to those routinely tested byparticipating laboratories. However, in some cases, in order to achieve the required degree ofhomogeneity and stability, test materials may be in the form of simulated samples.In this scheme a synthetic particle sample is used with Lead/Antimony/Barium particles, which representcharacteristic GSR particles. This sample shows all the criteria demanded in proficiency testing (inparticular: identical sample material and homogeneity of sample sets). That means there is a certainnumber of synthetic GSR particles consisting of Pb, Sb and Ba on each sample and the composition ofthe particles as well as location and size are exactly known by the organiser.3.2Quality ControlTest samples are, as far as possible, prepared using a well-controlled process, which has been verifiedto produce homogeneous material. If, in the opinion of QuoData GmbH, any material does not meethomogeneity requirements, a replacement material will be obtained for dispatch. Details of testsperformed, acceptability criteria and results will be given in the scheme reports.3.3DistributionThe test material is sent in an appropriate packaging and under conditions chosen to protect the samplesduring transit.Participants are asked to check the contents of packages immediately after reception and to contactQuoData GmbH if there are any problems with the condition of the test materials or accompanyingdocuments.3.4Sample PropertiesA glassy carbon chip of 8 x 8 mm² is mounted on a standard 1/2-inch stub. On this chip there is an areaof 6 x 6 mm² where an exactly defined number of PbSbBa particles is distributed (the composition of the"GSR particles" is Pb, Sb, Ba, and F; the F-signal results from the BaF2 that is used within the samplepreparation process). The PbSbBa particles have to be searched and filed.The sample is almost free of "contamination" for reasons of a standard for system validation purposesin future applications. For protective reasons the chip has finally been coated with a thin carbon layer,which is supposed to avoid charging. Nevertheless, if charging occurs, the participants are requested toperform a supplementary carbon coating of the sample.Page 10 of 17QuoData GmbH

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDSaccording to ASTM E1588Scheme Description4Analysis and Reporting of Results4.1Methods of AnalysisParticipants are asked to treat the PT material in the same way as a routine sample. The analysis of thetest sample should be performed – where possible – with the same SEM/EDS parameter settings asused for routine casework with a automated software control [5].Participants are requested to report also their acquisition parameters. It is important that this informationis accurate as the results are analysed and reported according to the parameters stated.4.2Performance of the TestThe test sample has to be mounted on the stage in such a way that the small 100 x 100 µm² pad isdisplayed in the lower left corner of the SEM screen (see e.g. Figure 1). At least the centre area of6 x 6 mm² of the chip which is margined by four markers n

GSR PT – Proficiency Test on Detection and Identification of Gunshot Residue Particles by SEM/EDS according to ASTM E1588 Scheme Description Page 4 of 17 QuoData GmbH 1 Introduction 1.1 Quality Standards Proficiency te

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