Southwestern Institute of Forensic Sciences Criminal Investigation Laboratory

Trace Evidence Training Manual Collection, Version 2.0

Approved by: David Spence, Trace Evidence Supervisor Timothy J. Sliter, Ph.D., Section Chief Chris Heartsill, Acting Quality Manager

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Corrections & Revisions Trace Evidence Training Manual Collection Effective Date 1/22/2008 Description Existing training procedures consolidated into a pdf collection (Version 1.0); no changes made to individual procedures Training Manual Collection, Version 1.0 archived; replaced with Version 2.0 with the following changes: • Revision by memo of Glass Training Protocol, Version 1.0 • Revision by memo of Bloodstain Pattern Analysis Training Protocol, Version 1.0 • Fire Debris and Ignitable Liquid Training Protocol Version 1.0 replaced by Version 1.1 • GC-MS Analysis Training Procedure Manual Version 2.0 replaced by Version 2.1 • GSR & Range Determination Training Manual Version 1.0 replaced by Version 1.1 • Hair Training Protocol Version 1.0 replaced by Version 1.1 • Primer Residue Handwiping Training Protocol Version 1.0 replaced by Version 1.1 • SEM EDS GSR Training Manual Version 1.0 replaced by Version 1.1 Authorizing Individual Sliter

1/23/2008

Spence

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Revisions & Corrections Bloodstain Pattern Analysis Training Protocol Version 1.0 Effective Date 1/23/2008 Description Minor revisions described in memo of 1/18/2008 Authorizing Individual Spence

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SOUTHWESTERN

INSTITUTE OF FORENSIC SCIENCES
AT DALLAS 5230 Medical Center Drive Dallas, Texas 75235

Trace Evidence Unit

Interoffice Memorandum
To: Tim Sliter, Ph.D., Chief of Physical Evidence From: David W. Spence, Trace Evidence Supervisor Date: January 18, 2008 Subject: Change to Bloodstain Pattern Analysis Training Protocol used in the Trace Evidence Laboratory

This memo will serve to document a change being made to the Bloodstain Pattern Analysis Training Protocol used in the Trace Evidence Laboratory. The following change is as follows: Deletion: The wording “Version 1” in Section II “Requirements”, subsection “Reading”, first bulleted item was deleted.

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Dallas County Institute of Forensic Sciences Trace Evidence Unit

Fire Debris and Ignitable Liquid Training Protocol, Version 1.1

Dallas County Institute of Forensic Sciences Forensic Laboratory

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Fire Debris and Ignitable Liquid Training Protocol, version 1.1

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Revisions & Corrections Fire Debris and Ignitable Liquid Training Protocol – Version 1.1 Effective Date Description Changes from Version 1.0 to 1.1: • Addition: A written test was added. • Deletion: The entire sections for “Second-Opinion Casework” and Annual Competency Tests were removed. “Second Opinion Casework” is accomplished during administrative and peer reviews. Also, the Quality Manual covers the practice of annual competency / proficiency testing. • Revision: All references to the ASTM Method 1387 were changed to ASTM Method 1618-06. • Addition: The classification scheme referenced in ASTM Method 1618-06 was used in the description of some of the lectures and practical exercises. • Deletion: Since the purge and trap attachment to the GC/MS is no longer in use, the practical exercise using the purge and trap was removed. • Addition: A reference (Fire Debris Analysis by Stauffer, Dolan and Newman) was added to the list of reading in section II Authorized by

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Fire Debris and Ignitable Liquid Training Protocol, version 1.1

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I. Introduction This program is designed to begin and complete training in ignitable liquids and fire debris analysis through a series of lectures, practical exercises, and casework. It includes a combination of working with an experienced trace evidence examiner and self-training by the trainee. The trainee must have a working knowledge of gas chromatography / mass spectrometry. II. Requirements - Completion of In-House Ignitable Liquid Training For the completion of the ignitable liquid training, the following are student requirements: 1. Maintaining a training log outlining progress. 2. Completing a basic gas chromatography / mass spectroscopy course, focusing on electron ionization, scan mode mass spectrometry. This course may be taught either inhouse or by an outside source (e.g, Agilent, FBI, NFSTC, SWAFS, etc.). 3. Completing an ignitable liquid / fire debris analysis course from the ATF, NFSTC, FBI or other qualified agency. This class is desirable, but is not absolutely necessary. 4. Course of study as outlined below: Reading – The student will be required to read various journals, reference materials, and books that explain the basics of fire debris analysis. The following are among the recommended reading: o GC/MS Guide to Ignitable Liquids. Newman, Gilbert & Lothridge, CRC Press, 1998, Boca Raton. o Analysis and Interpretation of Fire Scene Evidence, Almirall & Furton, editors, CRC Press, 2004, Boca Raton. o “GC/MS Data Interpretation for Petroleum Distillate Identification in Contaminated Arson Debris”, Raymond Keto, Journal of Forensic Sciences, 40(3), May 1995, pp. 412-423. o “Chemical Markers in Weathered Gasoline”, Ronald Coulombe, Journal of Forensic Sciences, 40(5), September 1995, pp. 867-872.

o “Turpentine in Arson Analysis”, Michael Trimpe, Journal of Forensic Sciences, 36(4), July 1991, pp. 1059-1073. o “Improved Charcoal Packaging for Accelerant Recovery by Passive Diffusion”, William Dietz, Journal of Forensic Sciences, 36(1), January 1991, pp. 111-121. o “The Use of Activated Charcoal Strips for Fire Debris Extractions by Passive
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Diffusion. Part 1: The effects of Time, Temperature, Step Size and Sample Concentration”, Newman, Dietz and Lothridge, Journal of Forensic Sciences, 41(3), May 1996, pp. 361-370. o “An Accelerant Classification Scheme Based on Analysis by Gas Chromatography/Mass Spectrometry (GC/MS)”, Jack Nowicki, Journal of Forensic Sciences, 35(5), September 1990, pp. 1064-1086. o ASTM Method E 1618-06 Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass Spectrometry. o FBI Laboratory Analysis of Fire Debris Evidence course book. o National Forensic Science Training Center, Advanced Fire Debris Analysis Course student and reference manuals o Fire Debris Analysis, Stauffer, Dolan, and Newman, Elsevier, 2008. Lectures – A series of explanations/discussions is presented to the student and focuses on general criminalistics, classes of ignitable liquids, gas chromatography / mass spectrometry and its relation to the analysis of fire debris and sampling techniques.

A.

General Criminalistics 1. Philosophy of trace evidence. 2. Transfer of trace evidence. 3. Clothing examination and collection of ignitable liquids. 4. General case approach involving fire debris.

B.

Classes of Ignitable Liquids 1. Classification Scheme. 2. Petroleum Distillate – Light range. 3. Petroleum Distillate – Medium range. 4. Petroleum Distillate – Heavy range. 5. Gasoline – Neat and weathered. 6. Miscellaneous. 7. Oxygenated solvents.

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8. Isoparaffinic products.

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9. Normal Alkane products 10. Aromatic products 11. Naphthenic / Paraffinic products. C. Gas Chromatography / Mass Spectrometry 1. Chromatography overview. 2. The mass spectrometer as a detector. 3. The role of ions and interpretation of TIC. 4. Retention times and their importance. 5. Comparison of unknown and reference spectra. 6. The reference library and its uses. D. Practical Exercises 1. Using DFLEX / carbon strip in a paint can. 2. Using DFLEX / carbon strip in a Kapak / Nylon bag. 3. Solvent extractions. 4. Burned debris passive headspace extraction. 5. Data interpretation. 6. Comparison to reference data. E. Analysis of Reference Samples Each student will be responsible for analyzing known gasoline samples in their various forms of evaporation. This will be done with an experienced trace evidence examiner, as well as on one’s own. Each trainee will also be required to burn various substrates in and out of the presence of an ignitable liquid to in order to study pyrolyzates. Reference Samples: Analyze the following ignitable liquids for study: • •

Samples from each of the ASTM classes. Evaporated samples of samples from each ASTM classes.
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• • • • III. Written Test After analyzing the reference samples, the trainee will be required to satisfactorily pass a written test to demonstrate his/her knowledge of ignitable liquid analysis by GC/MS. IV. Co-working Cases The new examiner will then be asked to work cases with the experienced examiners. This is to provide the student with experience in the complex mixtures and burned by-products observed in actual casework. This will also offer instruction on the various methods used in case approach in the examination of ignitable liquids and fire debris. The student will observe the experienced examiner working the case and will also examine / review any data from the GC/MS. V. Competency Test After working cases with an experienced examiner, the new examiner will be required to complete a competency test involving ignitable liquids and fire debris. This competency test will focus on the student examiner’s ability to properly detect trace amounts of ignitable liquids, correctly identify their class, and compare them to known samples of ignitable liquids either in our reference library or from an outside agency. VI. Mock Testimony The trainee will be required to testify in a mock trial circumstance. The competency test or one of the co-worked cases will serve as the trainee’s “casework”. VII. Co-signed Casework The new examiner will then start to co-sign casework, in which he/she has the responsibility to collect trace evidence, design the case approach, examine the evidence, reach conclusions, and write a clear, concise report capable of being peer reviewed. The case is co-signed by a more experienced examiner who is also responsible for reviewing all of the data, case notes and evidence to determine that the case was handled properly and that the conclusion is correctly reached by the new examiner. Gasoline in dirt. Various mixtures. Wood samples. Carpet samples.

VIII. Checklist Upon completion of training, the trainers will be required to complete a prepared checklist outlining the training program and documenting the successful completion of the program by
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new examiners. The completed checklist will be sent to the Senior Trace Evidence Examiner, Chief of Physical Evidence and the Quality Manager for final assessment and official recognition of training completion.

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Ignitable Liquid Training Progress Checklist
Student’s Name: _____________________________________________________________ Initial and Date: Instructor(s) attest to the satisfactory completion of the element. Element 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. Basic GC/MS Course. Fire Debris Training (ATF, NFSTC, FBI, etc.). Philosophy of trace evidence examination. Definitions of terms relating to Fire Debris Analysis. Trace evidence transfer theory. Operation of the oven. Head space extraction. Solvent extraction. Head space vs solvent extraction. Working with CS2. HP GC/MS overview. Using GC/MS and software. GC/MS carousel. Comparing samples (data analysis). Overlaying samples. Ignitable liquid worksheet. Classification of ignitable liquids (ASTM). Weathered samples and their analysis . Target compounds for I. L. classification. Flowchart for ignitable liquids. Identifying ignitable liquids. Note taking for casework.
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Date

Initial

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23. Written reports. A. B. Evidence description. Reporting the examination and comparison process procedure. Date Initial

Element C. D. E. 24. 25. Examination results. Examination conclusions. Disposition of evidence.

Competency testing. Reading. A. GC/MS Guide to Ignitable Liquids. Newman, Gilbert & Lothridge, CRC Press, 1998, Boca Raton. “GC/MS Data Interpretation for Petroleum Distillate Identification in Contaminated Arson Debris”, Raymond Keto, Journal of Forensic Sciences, 40(3), May 1995, pp. 412-423. C. “Chemical Markers in Weathered Gasoline”, Ronald Coulombe, Journal of Forensic Sciences, 40(5), September 1995, pp. 867-872. B.

D. “Turpentine in Arson Analysis”, Michael Trimpe, Journal of Forensic Sciences, 36(4), July 1991, pp. 1059-1073. E. “Improved Charcoal Packaging for Accelerant Recovery by Passive Diffusion”, William Dietz, Journal of Forensic Sciences, 36(1), January 1991, pp. 111-121.

“The Use of Activated Charcoal Strips for Fire Debris Extractions by Passive Diffusion. Part 1: The effects of Time, Temperature, Step Size and Sample Concentration”, Newman, Dietz and Lothridge, Journal of Forensic Sciences, 41(3), may 1996, pp. 361370. G. “An Accelerant Classification Scheme Based on Analysis by Gas Chromatography/Mass Spectrometry (GC/MS)”, Jack Nowicki, Journal of Forensic Sciences, 35(5), September 1990, pp. 1064-1086.

F.

H.

ASTM Method E1618-06 - Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography – Mass Spectrometry.
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I. FBI Laboratory Analysis of Fire Debris Evidence course book. National Forensic Science Training Center, Advanced Fire Debris Analysis Course student and reference manuals.

J. 26. 27. 28. 29. 30.

Conduct independent examinations and cosign reports. Courtroom testimony principles. Witness expert ignitable liquid court testimony (if possible). Mock trial exercises. The student on this checklist has the knowledge and skill necessary to perform independent ignitable liquid analysis.

IX.

Experienced Ignitable Liquid / Fire Debris Examiners Training Assessment Program Trace evidence examiners, with experience in ignitable liquid analysis in a laboratory other than SWIFS, will be assessed according to the following program before being assigned independent casework responsibilities. The assessor(s) will be experienced and current in ignitable liquid analysis. A. Review Trace Evidence Unit ignitable liquid protocol and reading list. The “new” examiner and assessor will document this review on the standard IGNITABLE LIQUID TRAINING PROGRESS CHECKLIST. During this process, the new examiner will initial all areas of the CHECKLIST where he/she feels competent. This will allow the assessor to focus on areas of needed attention. The assessor will prepare five tests with emphasis on the examination of ignitable liquids currently in our reference collection and that occur in routine casework. 1. The new examiner will work all test samples, take notes and write sample reports. The new examiner will notify the assessor when he/she has finished each test sample. The assessor will then provide the new examiner with the next sample. After the new examiner has completed the second test sample, the assessor and the new examiner will meet, preferably at the new examiner’s workstation, to review the data, examination results, notes, and reports of the first two test samples. The same procedure will follow for the third, fourth and fifth samples.

B.

2.

3.

C.

If major deficiencies surface during evaluation of the five test samples above, then a customized training plan designed to overcome those deficiencies will be developed
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and implemented with appropriate documentation on the CHECKLIST. Minor deficiencies are defined as those which are corrected by actions taken between test sample assignments (such as lectures by the assessor, reading assignments, oral testing of the new examiner, technique or skill demonstration by the new examiner, and other actions). If no deficiencies are encountered, or when noted deficiencies are corrected, continue to Step D. D. The new examiner will work at least two actual cases with the new assessor. The critical elements of assessments in this exercise will be directed toward: 1. 2. 3. 4. 5. 6. E. F. G. Case approach principles. Evidence examination principles. Collection of trace evidence. Examination of ignitable liquid evidence. Appropriate conclusion development. Final written report construction.

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Review and update of the CHECKLIST by the assessor and new examiner. A mock trial will be held prior to the new examiner’s first ignitable liquid testimony. The assessor will prepare a memo recommending the trainee for independent ignitable liquid casework assignment when the assessment has been satisfactorily completed and the CHECKLIST has been signed off. Otherwise, the assessor will recommend an alternate course of action.

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Fire Debris and Ignitable Liquid Training Protocol, version 1.1

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Dallas County Institute of Forensic Sciences Trace Evidence Unit

Gas Chromatography / Mass Spectrometry Analysis / Training Procedure Manual Version 2.1

Dallas County Institute of Forensic Sciences Forensic Laboratory

GC/MS Analysis / Training Procedure Manual, Version 2.1 1 of 27

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Revisions & Corrections Log Gas Chromatography/Mass Spectrometry Analysis/Training Procedure Manual Version 2.1

Effective Date

Description Changes from Version 2.0 to 2.1: • Revision: Changes previously referenced from August 9, 2002 and March 22, 2005 were incorporated into this version. • Revision: Typographical errors were corrected throughout the document. • Deletion: Extraneous information was removed from the Introduction. • Addition: Additional solvents were added to “Equipment, Materials & Reagents” • Revision: Section V. “Safety” now has a more concise description of safety guidelines and PPE. • Revision: The instrument parameters in Section VII were consolidated. Resolution check mix samples from ASTM 1387 and ASTM 1618 were specifically designated in Section VII “Instrument Parameters” and Section IX “Quality Assurance & Quality Control” • Deletion: Since the purge and trap attachment to the GC/MS is no longer in use, the alternate method section was removed. • Deletion: The appendix that included the printed methods was removed. These printed methods will now be included in the analysis method manuals.

Authorized by Spence

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I. Introduction Examinations identifying unknown organic compounds may provide probative evidence of that chemical on clothing of suspect or victim or scene evidence. These techniques are well documented and are fully accepted in the forensic science community. The following procedure is specific for pepper sprays and other lacrimation agents (capsaicin and CN), however the procedure is adaptable for general chemical unknowns. II. Abbreviations GC/MS Gas Chromatography/Mass spectrometry Capsaicin Pepper spray active ingredient MeOH Methanol TIC Total Ion Chromatogram Resck, Reschk, Reschek or other variation Resolution Check Mixture Pos / + Positive Neg / Negative III. Equipment, Materials & Reagents Gas chromatograph and mass spectrometer (GC/MS), Carbon Disulfide (CS2), chloroform, Methanol, glass pipets, glass vials with teflon septums, autosampler vials with inserts and caps, crimper, known standards (ie Capsacin), vent hood, oven, and Grade 5.0 Helium (carrier gas) IV. Sample & Standard Requirements The ability of the analyst to identify a chemical unknown is dependant on the ability of the analyst to identify the ions as well as the TIC in some cases. A known sample or one from the GC/MS library of analyzed compounds (NIST library) is crucial to being able to identify samples. V. Safety Care must be taken to prevent injury from the toxic, caustic or lacrimating effects of potential samples. Also, universal precautions for handling biohazards and chemical hygiene guidelines for handling volatile solvents shall be observed. Adequate ventilation should be utilized when working with any chemicals, especially carbon disulfide in this protocol. Appropriate personal protective equipment (PPE), such as masks, gloves, lab coat, face shields and/or safety glasses shall be worn while preparing samples for analysis.
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VI.

Training: Before a scientist can begin independent forensic examination of trace evidence, a training program must be completed. A general list of steps involved in training: 1. Completion of a basic gas chromatography / mass spectroscopy course taught either in-house or externally. This should include the basic theory and application of gas chromatography / mass spectrometry and typical methods of examinations. “Hands on” experience using the interactive tutorials and training manuals on the HP CD-ROM. Followed by the general test. Thorough understanding of the general trace evidence procedures manual and clothing examination manual. Detailed training in the specific discipline where the GC/MS will be used to assist in the separation and identification of unknown samples. Examples include pepper spray, CN gas, dyes, pesticides, or any other organic unknown. Working with an experienced analyst in the setup, calibration, QC and general maintenance procedures of the GC/MS system. Completion of a competency test where the analyst must set up the GC/MS, run any pertinent QC tests, and identify a chemical unknown based on retention time and mass spectral data.

2.

2.

3.

4.

5.

VII.

Instrument Parameters The procedure utilizes a Hewlett Packard 6890 Gas Chromatograph with auto sampler and a 5973 Mass Selective Detector. A 30 meter HP-1 or equivalent column is used with Helium as the carrier gas. The column must be suitable for resolving test mix components. For specific operating instructions, refer to the instrumentation manuals. An acceptable sensitivity range is 0.005 volume percent in CS2 (10:1 dilution of E 1618 Test Mixture). The type of analyte that can be detected will be dependant on two things: the solvent and

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the column. This method can be changed to suit the needs of the analyst. A column suitable for the specific analyte in question should be used. Instrument parameters should be optimized for the particular analysis at hand. Before each sequence of samples is run, an autotune is performed. A sequence begins with at least one blank solvent injection (blank method) followed by the Resolution Check Mixture (E1387 or E1618) being analyzed using an ignitable liquid method. A blank solvent sample is then analyzed after the Resolution Check Mixture. Between each case sample, a blank solvent sample is analyzed to insure no carryover has occurred. The blank, ignitable liquid and CN methods are retained in the respective procedure manuals. The 0.005 % volume Sensitivity check solution is run semi-annually or on a monthly basis as casework dictates. VIII. Procedure for General Unknown 1. 2. 3. 4. 5. 6. 7. Evidence is received and inventoried. Document all results on separate note pages. If the material to be tested is not on swabs, then solvent swabs must be applied to the area of interest. Place each swab in individual glass vials containing 1 - 2 ml of MeOH, chloroform or CS2. Evaporate the sample extract to approximately 100 µl. Transfer an aliquot of the sample extract into a pre-labeled glass autosampler vial using one of the inserts. Cap the autosampler vial. If the case sample is in a liquid form, first check its solubility in MeOH, chloroform or CS2. Dilute the sample in the appropriate solvent and fill an autosampler vial/insert with the sample/solvent mixture and continue with the procedure. If the sample is not soluble in methanol, chloroform or CS2 report these findings and do not analyze by GC/MS. Run a sequence on the GC/MS. Utilize a sequence which includes at least one blank solvent sample and Resolution Check sample. Run a blank solvent sample between each case sample. Run each case sample using an appropriate method. Compare results to known standards in the database. Analyze additional known reference standards as needed.

8.

9. 10. 11. IX.

Quality Assurance & Quality Control The autotune is checked for any evidence or leaks of other instrumental problems. Refer to Appendix 3 for autotune parameters and corrective actions. A resolution check mix (ASTM E1387 or E1618), containing a known mixture of hydrocarbons, is run with

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every sequence of casework samples. This check mix is also analyzed with a 10:1 dilution (0.005 % volume) sensitivity check. The sensitivity check should be performed semi-annually or on a monthly basis as casework dictates. The target compounds identified in the ASTM E1618 method should be resolved and identified in an accepted resolution check mix. If any of the target compounds cannot be resolved or identified, the analyst should check the system for leaks, remake the resolution check mix, and/or any other maintenance necessary. Each resolution check mix and sensitivity check should be kept in the GC/MS logbook along with notations about any problems or maintenance. Blank solvent samples are run before each sample analyzed to insure that no carryover has occurred from previous samples. If the TIC of a blank sample displays compounds that may interfere with sample data interpretation, the analyst should perform checks and maintenance. A suitable blank should exist prior to samples being analyzed. Any maintenance should be recorded in the GC/MS logbook. X. Notes The notes should reflect the material being tested, the source of the material, date and time(s) analysis and results. The type of material being tested can be an important component when analyzing the spectra. XI. Report and Reporting Guidelines A comparable chromatogram from the standard library should be included in the notes on all positive cases. XII. Continuing Education For continuing development as a trace evidence examiner, each scientist will be required to complete proficiency cases, peer review casework for/by other examiners, stay current with forensic literature, and seek to attend outside courses/seminars involving trace evidence examination.

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Appendix 1: Recommended Reading This is not an all inclusive list: 1. Saferstein, R. (Ed.), Forensic Science Handbook, Hall, Englewood Cliffs, New Jersey, 1982, pp. 92-138. Saferstein, R. (Ed.), Forensic Science Handbook, Vol II, Hall, Englewood Cliffs, New Jersey, 1988, pp. 38-65 (David T. Stafford PhD., Chapter Author). Jehuda, Y. (Ed.), Forensic Applications of Mass Spectrometry, CRC Press Florida, 1995. Jehuda Y. (Ed.), Forensic Mass Spectrometry, CRC Press, Florida, 1987.

2.

3.

4.

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Appendix 2: GC/MS Maintenance and Calibration HP6890 GC with 5973 Series Mass Spectrometer Autotunes will be performed each day that casework is performed. Calibration of the instrumentation will be performed as needed. Analysts will perform the following preventive maintenance activities. All maintenance or repair activities will be recorded in the GC/MS Logbook. HP GC/Mass Spectrometer Maintenance Schedule Daily/with use Refresh wash vials Check gases As needed Change gas tanks Replace column Change filament Change septum Change liner Change gold seal Cut columns Clean Source Clean split side arm Check autocal vial Change rough pump oil Tune (autotune)

MAINTENANCE OF THE HP6890 GC/5973 Series Mass Spectrometer Maintenance activities should be consolidated to minimize instrument down time. For example, if it is time to change the gold seal and cut the column, it may be more prudent to change the liner and septum at that time or hold off changing the gold seal until the liner and septum are changed. The maintenance interval is not a rigid schedule and should be based upon workflow. Unless there is an immediate problem, a chromatographic run should continue to completion, and the maintenance performed at the end of a run. Ultraclean Technique: Liners, gold seals, and certain other parts must be handled using ultraclean techniques to avoid contamination of the part with oils from the skin, plasticizers from plastic benchcoat, etc. Do not handle an ultraclean part with your hands; wear cotton gloves or use a fresh Kimwipe. Lay the ultraclean part on its cloth wrapping or on a clean Kimwipe.
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Changing the Wash Vials: Discard unused solvent into the hazardous waste, rinse the containers with fresh solvent, fill with solvent, and replace the vials in the appropriate location on the autosampler. 5973 mass spec – CS2, Methanol Changing the Liner and Septum: Tools needed: inlet wrench and tweezers. NOTE: Turn off carrier gas; if the septum nut is removed without turning off the carrier gas, the glass wool plug may be blown out. Use ultraclean technique at all times when handling the new liner. 1. Cool the inlet to room temperature to minimize oxidation and prevent burns. 2. Turn off the carrier gas on the GC by using the software or from the front panel on the GC, from the front panel on the GC, push the FRONT INLET button. Scroll down using the _ button to the Total Flow line. Turn off the flow by pressing the OFF button. Once maintenance is complete, turn the flow back on by pressing the ON button. 3. Once the inlet is cool and the gas is off remove the top septum nut. Remove and replace the septum. Reinstall the top septum nut. These are not ultraclean parts but care should be taken to avoid any unnecessary contamination. 4. Remove the nut covering the liner. Remove the old liner and discard. 5. Using ultraclean technique, carefully drop the new liner into the inlet. The glasswool plug, if present, should be nearest the top of the liner. 6. Using ultraclean technique, place the o-ring over the end of the liner. Use tweezers to work the o-ring flat against the inlet surface. 7. Replace the nut and turn on the inlet temperature and carrier gas flow. 8. A blank run should be made to bake out the new liner before analyzing samples. Use the highest routinely used temperature program. (Note: It is sometimes recommended that liners be sonicated in solvent such as methylene chloride and dried in an oven prior to installation. This process has been found to decrease the life of the glasswool.) Changing the Gold Seal: Tools needed: appropriate screw driver (Phillips/Torx/etc.), 9/16 wrench, ¼ wrench Note: The gold seal is located at the bottom of the inlet. It is accessed through the nut in the oven where the column comes out of the inlet.
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Use ultraclean technique at all times when handling the gold seal.

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1. Cool the inlet to room temperature to minimize oxidation and prevent burns. 2. If maintenance is going to be quick, the carrier gas does not need to be turned off. If you feel that you need to turn off the carrier gas flow, follow the procedure listed above for “Changing the Liner and Septum.” 3. Remove the column from the inlet. (Once the column is removed, the ferrule will need to be replaced and the column cut.) 4. Remove the insulator cup (2 Phillips/Torx screws) to reveal the nut housing the gold seal. 5. Remove the nut and turn upside down to remove the gold seal and washer. 6. Insert the new gold seal and washer into the nut: a. Insert the washer into the nut; the washer goes between the gold seal and the nut (i.e. below the gold seal.) b. Insert the gold seal into the nut with the grooves on top. (These grooves are the exits for the split gas during split injection and for the purge that comes on after a splitless injection. They must be on top for this to work properly.) 7. Reinstall the nut containing the gold seal and washer and tighten. 8. Replace the insulator cup over the nut. 9. Replace the ferrule and cut the column as described below. 10. Reinstall the column and check for leaks with a leak detector. (If you turned off the carrier gas, turn it back on and let it flow for a few minutes before you check for leaks.) 11. Turn on the inlet temperature. 12. A blank run should be made to bake out the system before analyzing samples. Cutting the Column Tools needed: column cutting wafer or crystal, ¼ inch wrench Any time a column is removed from the inlet or detector, the ferrule should be replaced and the column should be cut. The inlet end of the column may be cut several inches to remove active sites and restore separation capacity. The inlet ferrule should also be replaced. 1. Cool the inlet or detector to room temperature. This will minimize oxidation and prevent burns. 2. Remove the column from the inlet/detector. 3. Remove the nut and ferrule. The ferrule which is made of a graphite may be stuck to the nut; remove all of the ferrule. 4. Place a new ferrule over the column with the flat end toward the nut. 5. Cut two or three inches off the end of the column: a. The column should be cut by scoring one side with a wafer or column cutting crystal and then snapping the column at the score. b. Inspect this cut with a magnifying glass. This cut must be clean and contain no rough edges. If there are rough edges, cut the column again. c. Wipe the end of the column with a Kimwipe and methanol. d. Place the column back into the inlet/detector. When installed, the column should protrude 5 mm (4mm to 6 mm) beyond the ferrule into the
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inlet/detector. 6. Turn on the carrier gas, if you turned it off, and check for leaks with a leak detector. 7. Measure the length of column that was cut off and enter the new corrected column length into the appropriate location for all methods.

Installing a New Column: 1. 2. 3. 4. 5. 6. 7. Cool the injector and detector. Turn off the carrier flow following the procedure in “Changing the Liner and Septum.” Loosen the column ferrules from the injector and detector and remove the column. Place a nut and ferrule on each end of the column. (The flat side of the ferrule goes toward the nut.) Cut about ½ inch from the inlet end of the column using techniques described in “Cutting the Column.” Install the new column into the inlet only. Use a plug to cap the detector entrance in the column oven. This step may not be necessary depending upon the type of column used. An “MS” column which has been developed for use in a mass spec has extremely low column bleed and can be conditioned in the detector. Proceed to steps 9 and 10 before conditioning the column in this case. Condition the column. If conditioning is not done properly the column may be ruined. a.

8.

Allow the carrier gas to flow through the column for approximately one hour with the GC oven at room temperature. b. Ramp the oven temperature at 10-15 degrees per minute to the final conditioning temperature. The final conditioning temperature should be at least 10 degrees higher than the maximum oven temperature to be used in the method but may not exceed 10 degrees below the maximum operating temperature of the column as recommended by the manufacturer. c. Condition the column several hours or overnight. 9. Cool the oven. Cut approximately 2 inches from the detector end of the column as described in “Cutting the Column.” 10. Install the detector end of the column if it has not been done previously. Cleaning the Split Side Arm The split vent side arm is the exhaust for split gasses and compounds that are split off during an injection. This can become very dirty and without maintenance can cause deleterious results. 1. Cool the injector temperature and turn off the helium. 2. Remove the liner from the inlet as specified in the “Changing the Liner and Septum” section. 3. Remove the autosampler tray and tower and the top rear instrument cover and fan
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cover. 4. Remove the split side arm from the inlet to the filter located at the rear of the instrument. 5. Inspect the ends of the side arm to make sure they are not clogged. If they are, use an old syringe to unclog the ends. 6. Use a vacuum; pull a solvent such as chloroform through the side arm into a waste container. 7. Repeat step 6 using a solvent such as methanol and then room air to dry. 8. Using a small brush or Q-tip dipped in chloroform to clean out the inlet arm where the side arm attaches. 9. Reconnect the side arm to the inlet and the filter. 10. Replace the covers and autosampler tray and tower. 11. Change the liner and septum. 12. Turn on the oven temperature and helium. 13. Check for leaks.

Tuning: Autotunes should be done on a quarterly basis or with instrument use. Tunes should also be done before instrument operation after maintenance. For the 5973 instrument tune as follows: 1. Select the instrument control screen. 2. Select the instrument menu item. 3. Select perform MS autotune menu item. 4. Review the tune. Criteria for an acceptable tune are as follows: 1. 2. 3. 4. 5. Low water and air - < 10% Correct mass assignments - +/- 0.2 amu (69, 219, 502) Symmetrical, smooth mass peak shapes Consistent mass peak widths - +/- 0.1 units from target values. - 5973 peak width default is 0.60. Appropriate EM voltage – 1000 to 2800 electron volts. If the voltage is not within these limits, review the history of the electron multiplier or consult a supervisor. The EM voltage will increase over time as the source becomes dirty. Cleaning the source should return the EM voltage to a normal operating level. Isotope mass assignments should be 1 amu greater than parent peaks. Mass 69 abundance should be 200,000 to 500,000. Relative abundance: - Mass 69 = 100% - Mass 219 = 70 – 250 % - Mass 502 > = 3 % Isotope ratios: - Mass 69 = 0.5 – 1.6% (1) - Mass 219 = 3.2 – 6.4% (4) - Mass 502 = 7.9 – 12.3% (10)
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6. 7. 8.

9.

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Autotune: Autotune maximizes instrument sensitivity over the mass range, using PFTBA masses 69, 219, and 502. Use this tune for applications requiring maximum sensitivity that do not require traditional abundance ratios. Standard Spectra Tune: Standard Spectra Tune ensures standard response over the full mass range. This tune may be used if you are planning to perform mass spectral library searches. Quick Tune: Quick Tune provides re-tuning for optimum response and resolution, and for accurate mass assignment. Only the mass axis, peak widths, and EM voltage are adjusted; the lenses are unaffected. Use this tune for daily tuning as long as the relative abundances of the tuning masses are acceptable. Corrective Action if a Tune/Autotune does not meet laboratory criteria: If the Autotune or Standard Spectra Autotune fails, the operating chemist will take note of any error messages generated by the Chemstation Software, and check all sources of leaks for tightness. Re-evaluate the instrument, and monitor the instrument through the manual tune functions of the software. Once the problem is corrected, an Autotune and Standard Spectra Autotune shall be performed, and technical information and troubleshooting performed written in the GC/MS Logbook. If further assistance is needed, contact Agilent Technical Support. Cleaning the Source for Mass Spectrometers: Follow instruction provided in the manual for the 5973 mass spec. Changing the Filament: Follow instruction provided in the manual for the 5973 mass spec. Fill Autocal Vial: Follow instruction provided in the manual for the 5973 mass spec. Change Rough Pump Oil: Follow instruction provided in the manual for the 5973 mass spec.

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Appendix 3: Operations of the 5973 Series Mass Spectrometer

Operation of the 5973 Series Mass Spectrometer.
(Utilizing G1701BA Version B.01.00 Mass Spectrometer Chemstation) Overview

Users may begin using the chemstation by clicking on the top icon (named GC/MS Instrument # 1) located on the desktop. There are several ways to move around in the chemstation software. The following instructions are a guideline in which to follow and will not represent all of the ways that may be possible. The primary method of movement from one screen to another in the chemstation software is through the view menu item. If you are in the top level, instrument control or data analysis, the view menu item will allow the user to move to any of the other screens. Users are referred to the appropriate instrument manuals for additional information. Top Level Screen

From the top level screen the user has the ability to edit, print, load, and save methods and sequences. This screen enables the user to begin instrument operation. Instrument Control Screen

From the instrument control screen the user has the ability to modify instrument parameters such as injector, inlet, column parameters, oven parameters, mass spec temperatures, and electron multiplier voltages. The user can also edit, load, save and print methods from this screen. This screen enables the user to monitor instrument parameters during a run. Instrument tuning is also done from this screen. Data Analysis Screen

From the data analysis screen the user can edit the data analysis portion of a method, edit and select libraries, review total ion chromatograms, review individual spectra, compare unknown spectra to known libraries, and print reports. Storage of Data files, Methods and Sequences The hard drive is partitioned into two drives, drive C and drive D. The C drive is the location of the chemstation and the operating system (Windows NT 4.0). The D drive is
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designated for storage of other installed software. For the operation of the Mass Spectrometer Chemstation there are three key areas of storage. Data is stored in C:\hpchem\1\data. Data consists of data.ms files containing total ion chromatograms and their spectra, pre_post.ini files containing information on the status of the instrument during the run of the indicated file, and log files containing information regarding the sequence that was run. Methods are stored in C:\hpchem\1\methods. Methods contain all of the information required to execute a run. Methods contain the required macros and instrument parameters such as oven ramp parameters, pressure and flow parameters, injection parameters, and instrument temperatures as well as other information. Sequences are stored in C:\hpchem\1\sequence. Sequences contain the information required to complete a series of injections utilizing the autosampler tower and tray. The information consists of vial number, sequence line number, sample name, method name, and operator information.

I. Sequences

Loading a sequence or creating a new sequence

From the top level: 1. Select sequence menu item. 2. Select load menu item. 3. Select the default.s or a previous sequence and ok. This sequence of events will load the selected sequence in the instruments memory. Proceed to Edit sequence section to edit the sequence or Running a sequence section to run the loaded sequence. Edit sequence

Once the desired sequence has been loaded you may want to edit the sequence. From the top level: 1. Select sequence menu item.
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2. Select edit sample log table menu item. The edit screen will appear at this time with the sequence that the user had previously loaded. The user may edit, cut, copy, paste, or repeat lines in the sequence. Information that is required is type, vial, method, sample name. Line and Data File will be completed automatically by the chemstation software.

Line – the line number in the sequence completed by the chemstation. Type – the type of sample: sample, blank, calibrator, etc. Data File – unique number for a particular sequence generated by the chemstation. This number is only unique for the specific sequence and may be repeated in other sequences. Method – the method that the user wishes to employ. Sample Name – the description of the sample. Repeat – will increment the highlighted line and vial # by one number and will copy the highlighted line for all other information. Cut – will delete the highlighted line (will hold it in memory for paste function until another cut or a copy is executed). Copy – will copy the highlighted line to be used with the paste function.
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Paste – will paste the highlighted line that has been cut or copied and insert it above the current highlighted line. Once the editing is complete select OK to exit. If you do not exit out of the edit screen the sequence will not continue. Edit a sequence while it is running

The user may also edit the sequence while a sequence is running to add a specimen to the running sequence. If the sequence is running the menu items will not be available and the user must select the edit sample log tbl button from the center screen. At this time, the edit sequence screen will appear.

Saving a sequence

After the user has loaded and edited a sequence, he must save the sequence. From the top level: 1. Select the sequence menu item. 2. Select the save menu item.

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Running a sequence There are several ways to begin a sequence. The user may select run, load and run, or position and run. The run menu item will begin the current sequence. The load and run sequence menu item will allow the user to load a new sequence and then run it. The position and run menu item will allow the user to begin the current sequence at a user specified location within the current sequence. To begin a sequence from the top level: 1. Select the sequence menu item. 2. Select the run, load and run sequence, or position and run menu item. 3. The user will be prompted to enter the data path for the storage of the data collected during the sequence run. The following screen will appear:

4. Make sure that full method is selected. The user may or may not want to select the overwrite existing data files. Select the appropriate option on the barcode mismatch section. 5. Type the correct path for the storage of data. The default path is C:\HPCHEM\1\Data\. The default location is where the chemstation looks for data from the data analysis screen. If the user does not store the data in the default location be aware of the location that was selected. 6. Select run sequence button. If the sequence does not begin at this time, check the above screen and the selections to make sure that the proper selections have been made. If load and run or position
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and run are selected the user will be prompted to load a sequence or select a position within a sequence before the above screen appears.

Using Keywords

The chemstation allows the use of keywords within a sequence. These keywords allow the user to perform certain functions within the sequence such as running a command or macro, tuning the instrument, pausing the sequence and more. The most common keyword used is pause. The pause command will allow the user to pause the sequence after the current injection and method are complete. To use a keyword the sequence must be running. To use a keyword: 1. Select the edit sample log tbl button as seen in the section titled “Edit sequence while it is running”. 2. The edit screen will appear with the sequence lines that have been run greyed out. 3. Select the next line to be run, copy and paste so there are two identical lines. 4. Select the keyword command in the type box. 5. This will prompt the user to type the keyword that is to be used. Select the keyword in the keyword box. 6. Select ok. When the current method is complete the keyword command will be executed. II. Methods

The method in the chemstation software is the location of all of the instrument parameters and data analysis parameters that will take place during the execution of a method in a sequence. Methods should only be created or modified by those with knowledge of the required parameters or experience with instrument parameters.

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Creating a new method

To create a new method the user may select menu items from either the top level screen or the instrument control screen. From either screen: 1. Select the method menu item. 2. Select the load menu item. 3. Load the default method or load an existing method and modify to create your new method. 4. Select the save menu item to save the method. Editing an existing method If the user needs to edit a method or check the contents of a method, he can access the method from the top level screen or the instrument control screen. From either screen: 1. Select the method menu item. 2. Select the edit entire method menu item. 3. Edit or review the method. Save the method ONLY if you are aware of the changes that have been made. If you have not made changes and you are not sure if the method should be saved DO NOT save the method.

III. Data Analysis

You may enter data analysis in several different ways. You may open it from the icon on the desktop, from the top level screen during the execution of a sequence, or from the view menu item from any screen.

Loading a chromatogram (data file)

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The data file contains the total ion chromatogram and the spectra for the identified compounds in the chromatogram. To load a chromatogram: 1. Select the file menu item. 2. Select the load data file menu item. 3. Select the appropriate data file and OK. (The data file will be in the location that was specified when the sequence was

started. The default location is

C:\HPCHEM\1

Reviewing Data Once the chromatogram has been loaded it will appear in window 2. It will appear as the total ion chromatogram (TIC) with peaks representing detector response to compounds and their retention times. There are many items that the user may want to use to review data. These include but are not limited to integrating, searching for specific ions, comparing unknown spectra to known libraries, generating reports, and printing spectra. The TIC will be normalized on the largest peak. This means that the largest peak will be completely visible from the top of the peak to the baseline. Large peaks in a TIC may make smaller peaks not visible when looking at the normalized chromatogram. If the user wishes to look at the smaller peaks he can zoom in on the peak. To do this left click and hold the mouse, drag a box around the area to be analyzed and release. This will zoom in on the area that the box was drawn around.

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Generating, comparing and printing spectra To generate a spectra at a specific retention time of a TIC double click the right mouse button at the point of interest. This will generate a mass spectrum of the area that was clicked on and it will appear below the TIC in window 1.

The method that is loaded will determine what library or libraries have been selected for use (see searching libraries for instructions on changing). To compare the generated spectrum with the library that is specified in the method:

1. Double click the right mouse button while the cursor is in window 1.

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2. This will generate a comparative spectrum with the best match being shown first. This comparative spectrum is generated in window 24.

The spectrum for the unknown compound is located on top and the spectrum for the best match is located on the bottom. The library that the best match spectrum came from is listed in the PBM Search Results box. 3. To print the comparison select the print button located in the PBM Search Results box.

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The user may also want to print the TIC or the unknown spectrum without using the comparison method. To do this: 1. 2. 3. 4. Load chromatogram and generate spectrum. Select the file menu item. Select the print menu item. The user will be prompted to enter the window that he wants to print. Enter the number of the window that you wish to print: 1 = spectrum, 2 = TIC.

Searching for specific ions

When a specific ion needs to be isolated so the user may separate coeluting compounds or find a compound with a weak response, the chemstation can search for specific ions within a TIC. To do this: 1. Select the chromatogram menu item. 2. Select the extract ion chromatograms menu item 3. This will prompt the user to enter the ion or ions that the chemstation will look for and the retention time windows in which to look. 4. Enter the ions of interest. 5. Enter the retention time window in which to look. 6. Select the OK button. This will prompt a window displaying the extracted TIC and each ion will be displayed in a different color. Full spectrum may be generated by double clicking the right mouse button on the area of interest.

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Subtracting Spectra In the event that two compounds coelute or a compound with a weak response is hidden in the baseline it may be desirable to subtract spectra. An example would be a drug that gives a weak response and is hidden in the baseline. In this instance the user would look for the ions in the compound of interest by a manual search or by searching for extracted ions. Once the compound is found the full spectrum may have ions from the baseline included in the ions for the compound. The chemstation allows the user to subtract one spectrum from another to clean up or clarify a spectrum. To subtract a spectrum: 1. Obtain a spectrum of the compound (with the interfering ions). 2. Move the cursor to a location, usually just before or just after the compound of interest and obtain a spectrum of that area. 3. Select spectrum menu item. 4. Select subtract menu item. The resulting spectrum will be the difference of the second obtained spectrum removed from the first obtained spectrum. When the subtract menu item is selected it will subtract the current spectrum in window 1 from the previous spectrum that was in window 1 and show the difference of the two in window 1.

Printing reports

There are many ways to print reports and a number of reports are available in the chemstation software. The most common way to print a report for a designated method is to: 1. Load the appropriate TIC. 2. Select the method menu item. 3. Select the run method menu item. 4. This will run the data analysis portion of the method that has been selected in data analysis. It will print the report as if the sample had been run in a sequence. The user may also want to use the options available under the quantitate and tools menu items.

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Using the quantitate menu item the user will be limited to the chemstation report format and any custom reports will not apply. The tools menu item allows the user to reprocess quantitative and qualitative reports and are linked to custom reports found in the deuser.mac macro associated with each method. Searching Libraries

There are many different libraries that are available in the chemstation ranging from inhouse libraries to commercially purchased libraries. The libraries are located on the C: drive of the computer in C:\database. To change the libraries that are automatically searched in a method:

1. Select the spectrum menu item. 2. Select the select library menu item. 3. This will prompt the user to type in the name of the library to be used. This will affect the library that is used when the user is comparing an unknown spectrum to a library spectrum. Once a spectrum is obtained in window 1, the user can also search specific libraries by selecting one of the menu items located at the bottom of the spectrum menu item.
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Parametric Retrieval is located under the view menu item in data analysis only. Parametric retrieval can be used to search a user designated library for compounds based upon name, molecular weight, CAS number, library entry number, etc. However, the information must be in the library before the search parameters will work. Occasionally all of the information may not be available with in-house libraries.

Quantitative data analysis

Each quantitative method will have associated data analysis that will occur automatically and perhaps manually. The user will be trained on an individual basis regarding interpretation of data and use of the chemstation reporting and analysis.

Tuning the 5973

The tuning instructions and parameters can be located in Appendix 2 or the reference collection found near each instrument.

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Revisions & Corrections Glass Analysis Training Protocol Version 1.0 Effective Date 1/23/2008 Description Revisions described in memo of 1/18/2008 Authorizing Individual Spence

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SOUTHWESTERN

INSTITUTE OF FORENSIC SCIENCES
AT DALLAS 5230 Medical Center Drive Dallas, Texas 75235

Trace Evidence Unit

Interoffice Memorandum
To: Tim Sliter, Ph.D., Chief of Physical Evidence From: David W. Spence, Trace Evidence Supervisor Date: January 18, 2008 Subject: Revision to Glass Training Protocol used in the Trace Evidence Laboratory

This memo will serve to document a change being made to the Glass Training Protocol used in the Trace Evidence Laboratory. The following change is as follows: Deletion: The wording “, Appendix 1-3.” in Section V. “PHYSICAL/OPTICAL PROPERTY DETERMINATION”, subsection C “Reading”, sub-section 1 was deleted.

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Dallas County Institute of Forensic Sciences Trace Evidence Unit

Gunshot Residue and Range Determination Training Manual Version 1.1

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Revisions & Corrections Trace Evidence Unit – Gunshot Residue and Range Determination Training Manual, Version 1.1 Effective Date Description Changes from Version 1.0 to 1.1: • Revision: Revision of section IX.: change of title to “Independent Casework” and clarification of documentation required to complete training • Revision: Revision of section III.: to add/clarify training topics • Revision: Revision of section X.: to add references. • Revision: Revisions of page numbers Authorized by Spence

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Gunshot Residue and Range Determination Training Manual, Version 1.1

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I.

Introduction This training manual is an outline for the training of an examiner in the sub-discipline of gunshot residue analysis and range determination. The trainee should complete the training and be able to show his/her proficiency before being allowed to perform casework alone. Lectures, discussions, readings, demonstrations and active participation are the majority of the training.

II.

Requirements for Completion of Gunshot Residue and Range Determination Training For the completion of the gunshot residue and range determination training, the following are student requirements: • • • • • Maintaining a training log, outlining progress. Understanding basic firearms knowledge, safety and terminology. Understanding chemical, biohazard and blood-borne pathogen safety procedures. Understanding the procedures and interpretation of gunshot residue patterns and range determinations. Course of study as outlined below:

Reading B The student will be required to read various journals, reference materials, and books that explain the basics of visual, microscopic and chemical procedures for gunshot residue and range determinations. Lists of required and recommended readings can be found at the end of this training manual. Lectures B A series of explanations/discussions is presented to the student which focuses on general criminalistics, chain of evidence, gunshot residue detection and interpretations. • • • • General Criminalistics. Chain of Custody. Basic Firearms Terminology and Safety. Gunshot Residue Detection Procedures.
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• • • III.

Test Firing Procedures. Range of Fire Estimations. Interpretation of Results.

Training Procedure Before an analyst can begin independent forensic examination of gunshot residue evidence, a thorough training program must be completed. A general list of steps involved in training includes: 1. Extensive reading and comprehension of texts, journals and articles relating to gunshot residue analysis. 2. A proper and complete understanding of all information and procedures needed prior to the execution of any gunshot residue analyses which includes: a. b. c. d. e. Checking out evidence and establishing an official chain of custody. Utilizing Field Agent and Medical Examiner=s reports as supplemental information. Following universal precautions for blood borne pathogens, contamination and integrity of evidence at all times. Solution preparation, quality control and quality assurance for the Modified Griess, Sodium Rhodizonate, and Dithiooxamide (DTO) tests. Proper etiquette when speaking to investigators, attorneys, etc.

3. Basic firearms knowledge and ballistics training is necessary to understand the sources of gunshot residue. Time spent with a firearms examiner is useful. Areas to be covered should include: a. b. c. d. e. f. Firearms safety. Pertinent firearms terminology. Study, observe, draw and describe gunpowder knowns (burned and unburned). Become familiar with various types of firearms (automatic, semiautomatic, revolvers, shotguns, rifles) and ammunition. Components and firing process of the cartridge. Actions of residues before, during and after discharge as they travel toward and deposit on the target.
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g. h.

Various shot sizes and other shotgun ammunition as well as general Arules of thumb@ for shotgun distances. Assist firearms examiners in the range.

4. The trainee should observe a trained examiner in the analysis of gunshot residue. The following steps of analysis should be observed by the trainee: a. b. c. d. e. f. g. h. i. Inventorying the evidence. Defect location, visual observation and comprehensive note taking. Microscopic examination for the presence of gunpowder and gunshot residues Modified Griess test for gunpowder residue. Sodium Rhodizonate test for lead residue. Dithiooxamide test for copper and nickel residue (as needed). Test firing and how to make a justifiable range of fire estimation. Proper packaging of press-outs and appropriate release of evidence. Photography of significant defect and/or residue patterns, as needed.

5. Following the analysis of the evidence the trainee should understand how to interpret the results and prepare a report as to those findings. 6. Observation of court testimony in the area of gunshot residue analysis is a necessary step in the training. Ongoing discussions with the trained examiners will provide the trainee knowledge of questions often asked by attorneys, investigators, medical examiners, etc. 7. Successful completion of numerous practical proficiency examinations, as well as knowledge based written examinations, are required. 8. Recommended attendance at the FBI gunshot residue course or at a similar course taught by non-SWIFS personnel. 9. The trainee will undergo a period of having their report co-signed by an experienced examiner. 10. A mock trial is the last step in the training process. IV. Written Test After the completion of the test samples, the student will be required to pass a written test on the basics of gunshot residue analysis and range determination.
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V.

Co-working Cases The new examiner will then be asked to work cases with the experienced examiners. This is to provide the student with experience in the various methods of case approach, examination of evidence, test firings and range determinations. The student will observe the experienced examiner work the case, participate in any chemical testing and attend test firings.

VI.

Competency Tests After working cases with an experienced examiner, the new examiner will be required to complete numerous competency tests. These competency tests will focus on the student=s ability to perform the procedures for gunshot residue detection, determine the test firing distances required and make range of fire estimations.

VII.

Co-signed Casework The new examiner will then start to co-sign casework, in which he/she has the responsibility to examine the evidence, perform detection procedures, perform test firings to reach justifiable conclusions, and write a clear, concise report capable of being peer reviewed. The case is co-signed by a more experienced examiner who is also responsible for reviewing the case notes and evidence to determine that the case was handled properly and that the conclusions are correctly reached by the new examiner.

VIII. Mock Trial Before a new examiner testifies in his/her first gunshot residue case, mock trials will be held in-house. IX. Independent Casework Upon successful completion of all elements of this training protocol and approval by the Trace Evidence Supervisor, Section Chief and Quality Manager, the analyst will be allowed to perform independent casework in gunshot residue and range determination.

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Gunshot Residue and Range Determination Training Manual, Version 1.1

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GUNSHOT RESIDUE TRAINING Student=s Name: _____________________________________________________________ Initial and Date: Instructor(s) attest to the satisfactory completion of the element. Date: Date of sign off by the instructor. Element 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Evidence handling and documentation Firearms terminology and safety Modified Griess test Sodium Rhodizonate test Dithiooxamide test Shotgun and rifle evidence Test firings Handgun practical exercises Rifle practical exercises Shotgun practical exercises Interpretation/Results Report writing Testimony observation Written test Competency test Mock trial Date Initial

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Gunshot Residue and Range Determination Training Manual, Version 1.1

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X. Reading Lists Required Readings 1. FBI notebook, Gunshot residue class. 2. “The Modified Griess Test: A Chemically Specific Chromophoric Test for Nitrite Compounds in Gunshot Residues”, John Dillon, AFTE Journal, 22(3), July 1990, pp. 243-250. 3. “The Sodium Rhodizonate Test: A Chemically Specific Chromophoric Test for Lead in Gunshot Residues”, John Dillon, AFTE Journal, 22(3), July 1990, pp. 251-256. 4. Gunshot Wounds: Practical Aspects of Firearms, Ballistics, and Forensic Techniques, First and Second Editions, Vincent J.M. Di Maio, CRC Press. 5. Forensic Science Handbook, edited by Saferstein, 1982, Chapter 11, p. 572. Recommended Readings This is not an all inclusive list. 1. “A Protocol for Gunshot Residue Examinations in Muzzle-to-Target Distance Determination”, John Dillon, AFTE Journal, 22(3), July 1990, pp. 257-274. 2. “An Empirical Study of Gunpowder Residue Patterns”, F.C. Barnes and R.A. Helson, Journal of Forensic Sciences, Vol. 19, No. 3, July 1974. 3. “Copper and Nickel Detection on Gunshot Targets Dithiooxamide Test”, J.A. Lekstrom and R.D. Koons, Journal of Forensic Sciences, Vol. 31, No. 4, p. 1283. 4. “A Protocol for Shot Pattern Examinations in Muzzle-to-Target Distance Determinations”, John Dillon, AFTE Journal, 23(1), January 1991. 5. “Characterization of Smokeless Powder Flakes from Fired Cartridge Case and from Discharge Patterns on Clothing”, J. Andrasko, Journal of Forensic Sciences, Vol. 37, No. 4, p.1030-1047. 6. “Gunshot Residue: An Overview”, Dahl, Lott and Cayton, AFTE Journal, 19(3),
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p. 247-252. 7. “Survey of Gunshot Residue Analysis in Forensic Science Laboratories”, DeGaetano and Siegel, Journal of Forensic Sciences, Vol. 35, No. 5, p. 1087. 8. “Weathering Time Factor in GSR Proximity Determinations”, D.A. Lindman, AFTE Journal, 21(3), p. 500-502. 9. “Gunshot Residue B A Review”, Meng and Caddy, Journal of Forensic Sciences, Vo. 42, No. 4, p. 553-570. 10. “Gunshot Residue Particles Formed by Using Different Types of Ammunition in the Same Firearm”, Zeichner, Levin and Springer, Journal of Forensic Sciences, Vol. 36, No. 4, p. 1020-1026. 11. “Range of Fire Estimates from Shotgun Pellet Patterns: The Effect of Shell and Barrel Temperature”, Horvath, Gardner and Siegel, Journal of Forensic Sciences, Vol. 38, No. 3, p. 585-592. 12. “Effects of Range, Caliber, Barrel Length, and Rifling on Pellet Patterns Produced by Shotshell Ammunition”, Speak, Kerr and Rowe, Journal of Forensic Sciences, Vol. 30, No. 2, p. 412-419. 13. “Method for Improving the Griess and Sodium Rhodizonate tests for GSR Patterns on Bloody Garments”, L.C. Haag, AFTE Journal, 23(3), p. 808-815. 14. “Forensic Applications of Infrared Imaging for the Detection and Recording of Latent Evidence”, Lin, Heish, Tsai, Linacre and Lee. Journal of Forensic Sciences, Vol. 52. No. 5. p. 1148-1150.

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Gunshot Residue and Range Determination Training Manual, Version 1.1

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Dallas County Institute of Forensic Sciences Trace Evidence Unit

Hair Training Protocol, Version 1.1

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Hair Training Protocol, version 1.1 1 of 11

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Revisions & Corrections Trace Evidence Unit – Hair Training Protocol, Version 1.1 Effective Date Description Changes from Version 1.0 to 1.1: • Revision: Revision of Section II to delete duplicate entries of the FBI Hair Microscopy Course book from the reading list and to correct author name (Hair Analysis Workshop Manual) to “James Robertson.” • Revision: Revision of Section II, subsection D to add de-mounting of hairs to lecture list. • Revision: Revision to Section II, subsection E to clarify types of reference samples to be examined and to delete chemotherapy hairs. • Revision: Revision of section ordering to allow for better flow in training process. • Deletion: Deletion of Second Opinion Casework section and duplicate entry of Competency Test section. • Revision: Addition of Section IX: “Independent Casework” • Revision: Revision of Appendix 1 “Hair Training Progress Checklist” to delete crime scene processing and wigs from the training topics and to re-order sections. • Revision: Revisions of page numbers and section numbers. Authorized by

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I. Introduction This program is designed to begin and complete training in hair evidence analysis through a series of lectures, practical exercises, and casework. It includes a combination of working with an experienced hair examiner and self-training by the trainee. II. Requirements - Completion of Hair Examination Training For the completion of the in-house human hair examination training, the following are student requirements: • • Maintaining a training log outlining progress. Completing a basic microscopy course, focusing on polarized light and compound comparison microscopy. This microscopy course may be taught either in-house or by an outside source (e.g, McCrone, FBI, NFSTC, etc.). Completing an introductory hair examination course. This class is desirable, but it is not absolutely necessary. Course of study as outlined below:

• •

Reading B The student will be required to read various journals, reference materials, and books that explain the basics of microscopic examination of hair evidence. The following are among the recommended reading: • • • • • In-laboratory hair article notebook and reference articles. FBI notebook from the AMicroscopy – Hairs and FIbers@ course. Forensic Science Handbook, edited by Saferstein, 1982 (pp. 184-221). Atlas of Human Hair, Microscopic Characteristics by Robert R. Ogle, Jr. Manual from James Robertson=s Hair Analysis Workshop

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Lectures B A series of explanations/discussions is presented to the student and focuses on general criminalistics, characteristics of hair, and examination of hair evidence. A. General Criminalistics • • • • B. Philosophy of trace evidence. Transfer of trace evidence. Clothing examination and collection of trace evidence. General case approach involving hair evidence.

Characteristics of Hair Evidence • • • • • • • Human vs. animal hair. Structure and function of hair. Racial characteristics. Somatic origin determination. Damage characteristics. Chemical treatment. Growth stages.

C.

Comparison of Hair Evidence • • • Comparison of known (reference) and questioned hairs. Conclusions reached in examination/comparison of hair evidence. Written reports and courtroom testimony principles.

D.

Practical Exercises Collection of control samples (head, pubic, body) from the student and from other individuals for addition to the reference collection. Mounting hair samples. De-mounting hair samples Manipulation of comparison microscope.

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Casting hair shafts for cuticle study. Distinguishing human hair from animal hair, microscopically. E. Microscopic Examination of Reference Samples Each student will be responsible to microscopically examine prepared slides of hair, focusing on hair characteristics previously discussed (racial, somatic origin, treatment, etc.). This will be done with an experienced hair examiner, as well as individual examination. Each person will also be required to mount samples of their own hair for detailed study. Reference Samples: Examine hairs from the following categories: • • • • • • • • • Animal hairs. Human hairs. Somatic origin (head, pubic, body, and beard). Racial characteristics (Negroid, Mongoloid, Caucasian). Chemically treated hair. Damaged hairs. Root structures (anagen, catagen, telogen). Color variations. Decomposing hairs.

III.

Completion of Test Samples The student will then be presented with test samples of various difficulties for examination: • • • • Closed Head Hair B two or three control samples and five questioned hairs, all belonging to the controls. Open Head Hair B two or three control samples and up to five questioned hairs from either control or from other sources. Closed Pubic Hair B using pubic hair controls with a similar format to the closed head hair test samples. Open Pubic Hair B similar to the open head hair test samples.
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Each new examiner will be expected to successfully complete at least ten test samples of head hair comparisons and ten test samples of pubic hair comparisons. IV. Co-working Cases The new examiner will then be asked to work cases with the experienced examiners. This is to provide the student with experience in the various methods of case approach and examination of hair evidence. The student will observe the experienced examiner work the case and will also examine any hair evidence recovered. V. Written Test After the completion of the test samples, the student will be required to pass a written test on the basics of hair examination and comparison. VI. Competency Tests After co-working cases with an experienced examiner, the new examiner will be required to complete at least two competency tests of hair evidence. These competency tests will focus on the student=s ability to make the proper hair comparisons necessary in a case. VII. Co-signed Casework The new examiner will then start to co-sign casework, in which he/she has the responsibility to collect trace evidence, design the case approach, examine the evidence, reach conclusions, and write a clear, concise report capable of being peer reviewed. The case is co-signed by a more experienced examiner who is also responsible for examining the hair evidence and for reviewing the case notes and evidence to determine that the case was handled properly and that the hair evidence conclusions are correctly reached by the new examiner. VIII. Mock Testimony Before a new examiner testifies in his/her first hair case, mock trials will be held in-house. IX. Independent Casework Upon successful completion of all elements of this training protocol and approval by the Trace Evidence Supervisor, Section Chief and Quality Manager, the analyst will be allowed to perform independent casework in hair analysis.

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X.

Experienced Hair Examiners Training Assessment Program Hair examiners, with experience in hair examination in a laboratory other than SWIFS, will be assessed according to the following program before being assigned independent casework responsibilities. The assessor(s) will be experienced and current in hair examination casework. A. Review Trace Evidence Unit hair training protocol and reading list. The Anew@ hair examiner and assessor will document this review on the standard HAIR TRAINING PROGRESS CHECKLIST. During this process, the new examiner will initial all areas of the CHECKLIST where he/she feels competent. This will allow the assessor to focus on areas of needed attention. The assessor will prepare five test case samples with emphasis on the examination of hairs encountered typically in casework. 1. The new examiner will work all test samples, take notes and write sample reports. The new examiner will notify the assessor when he/she has finished each test sample. The assessor will then provide the new examiner with the next sample. After the new examiner has completed the second test sample, the assessor and the new examiner will meet, preferably at the new examiner=s workstation, to review the hair examination results, notes, and reports of the first two test samples. The same procedure will follow for the third, fourth and fifth samples.

B.

2.

3.

C.

If major deficiencies surface during evaluation of the five test samples above, then a customized training plan designed to overcome those deficiencies will be developed and implemented with appropriate documentation on the CHECKLIST. Minor deficiencies are defined as those which are corrected by actions taken between test sample assignments (such as lectures by the assessor, reading assignments, oral testing of the new examiner, techniques or skills demonstration by the new examiner, and other actions). If no deficiencies are encountered, or when noted deficiencies are corrected, continue to Step D. The new examiner will co-work at least two actual cases with the new assessor. The critical elements of assessments in this exercise will be directed toward: 1. 2. 3. Case approach principles. Evidence examination principles. Collection of trace evidence.
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D.

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4. 5. 6. E. F. Examination of hair evidence. Appropriate conclusion development. Final written report construction.

Review and update of the CHECKLIST by the assessor and new examiner. A minimum of three competency samples will be assigned in accordance with the hair training plan and CHECKLIST. The new examiner must satisfactorily pass the competency testing before continuing in this assessment program. The new examiner will complete co-signed hair casework examinations in at least three cases. The actual number of cases depends on the complexity of the examinations, range of evidence involved, and quality of conclusions expressed in the reports by the new examiner. The assessor will prepare a memo recommending the trainee for independent hair casework assignment when the assessment has been satisfactorily completed and the CHECKLIST has been signed off. Otherwise, the assessor will recommend an alternate course of action. A mock trial will be held prior to the new examiner=s first hair testimony. Independent Casework Upon successful completion of all elements of this training protocol and approval by the Trace Evidence Supervisor, Section Chief and Quality Manager, the analyst will be allowed to perform independent casework in hair analysis.

G.

H.

I. J.

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Appendix 1

< Hair Training Progress Checklist =
Student=s Name: _____________________________________________________________ Initial and Date: Instructor(s) attest to the satisfactory completion of the element. Element 1. 2. 3. 4. 5. 6. 7. 8 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. Basic light microscopy course. Basic one-week hair training course (recommended). Philosophy of trace evidence examination. Definition of terms relating to hair examinations. Trace evidence transfer theory. Clothing examination B collection of trace evidence. Collection and preservation of hair evidence. Hair evidence control samples. Comparison microscope operation and use. Stereo microscope operation and use. Mounting hair on microscope slides. Manipulating microscope slides on stage. Casting hair shafts. Hair structure and function. Micro and macroscopic hair characteristics. Human hair characteristics. Animal hair characteristics. Distinguishing human hair from animal hair. Distinguishing parts of a hair. Somatic origin characteristics and determination. Racial characteristics. Growth stages of hair.
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Date

Initial

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23. Damage characteristics. A. Putrefication. Date Initial

Element B. C. D. E. 24. 25. 26. Thermal. Disease. Environmental effects when hair is debris. Violent force, such as fragmentation.

Chemical treatment characteristics. Human hair comparisons. Case approach. A. B. C. D. E. Case consultation with investigators and attorneys. Establishing the significance of hair evidence. Establishing the relative value of hair evidence. Case consultation with other forensic scientists involved in the case. Case consultation with peers.

27. 28. 29.

Hair examination and comparison conclusions. Note taking for casework. Written reports. A. B. C. D. Evidence description. Reporting the examination and comparison process procedure. Examination results. Examination conclusions.

30. 31.

Courtroom testimony principles. Training samples. A. B. C. Head hair samples: Number___ Open system. Head hair samples: Number___ Closed system. Pubic hair samples: Number___ Open system.
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D. Pubic hair samples: Number___ Closed system. Date Initial

Element E. F. G. Body hair samples: Number___ Open system. Body hair samples: Number___ Closed system. Other hair samples: Number___ Type Number___ Type Number___ Type 32. Competency samples. A. B. C. D. Head hair samples: Number___ Type Pubic hair samples: Number___ Type Body hair samples: Number___ Type Other hair samples: Number___ Type Number___ Type Number___ Type 33. Reading. A. B. C. D. In-laboratory hair article notebook. FBI notebook from the AMicroscopy of Hair@ course. Microscopy of Hair: A Practical Guide and Manual by the FBI. Forensic Science Handbook, edited by Saferstein, 1982, pp. 184-221.

E. 1985 Proceedings of International Symposium of Forensic Hair Comparisons, FBI Academy. F. 34. 35. 36. 37. 38. Atlas of human Hair, Microscopic Characteristics.

Co-work cases. Written Test Competency Test. Co-signed cases. Mock Trial

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Dallas County Institute of Forensic Sciences Trace Evidence Unit

Primer Residue/Handwiping Training Protocol, Version 1.1

Dallas County Institute of Forensic Sciences Forensic Laboratory

Primer Residue/Handwiping Training Protocol, Version 1.1

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Revisions & Corrections Trace Evidence Unit – Primer Residue/Handwiping Training Protocol, Version 1.1 Effective Date Description Changes from Version 1.0 to 1.1: • Revision: Revisions to the outline of the training process; “Written Test” was moved from after “Cosigning Casework” to before “Co-signing Casework”. • Revision: Revision to Section II “Lectures” to clarify the lecture topic “The degradation/persistence of GSR”. Addition of “The differences between GSR by GFAAS and SEM/EDS” as a lecture topic. • Revision: Revision to Section IV “Co-working Cases” to require 10 co-worked cases. • Revision: Revision of Section V title to “Competency Samples”. • Revision: Revision of Section VI “Written Test” to clarify wording. • Revision of Section VIII “Mock Trial” to state that a previously co-signed case will be used for that trial. • Revision: Revision to Section IX title from “Bibliography” to “Required Reading”; deletion of non-relevant references. • Revision: Revisions of page numbers and section numbers. Authorized by

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I. Introduction This program of instruction is designed to begin and complete the training in Primer Residue/Handwiping (HW) analysis by Graphite Furnace Atomic Absorption Spectroscopy (GFAAS). This protocol details the training process through a series of lectures, practical exercises, test samples, proficiencies, and casework. It is designed for a combination of working with an experienced Primer Residue/Handwiping examiner(s) and self-instruction by the trainee. A. The student will be required to maintain a training log outlining his/her training progress. The student will be required to read various journal articles, reference materials, and books that explain the basics of primer gunshot residue examination.

B.

II.

Lectures A. B. C. D. E. F. G. H. I. J. K. L. M. The History of GSR analysis. The value of GSR as evidence. Terminology. The origin/source of GSR. The chemistry/formation of GSR. The transfer of GSR. The degradation / persistence of GSR. The collection of GSR. The basic theory of Graphite Furnace Atomic Absorption Analysis Spectrometry (GFAAS). The operation and maintenance of the GFAAS. The analysis of GSR by GFAAS, including pipetting techniques. The interpretation and limitations of GSR results. The differences between GSR by GFAAS and SEM/EDS.

III.

Practical Exercises A. Examination of various types of firearms (revolvers, pistols, rifles and shotguns). 1. 2. Describe the functional differences in the various types of firearms. Describe the areas of highest plume concentrations for each class of firearm.

B.

Test-fire various types and calibers of firearms. 1. Collect GSR residues from firing and non-firing hand.
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2.

Collect GSR residues from various distances from front and sides of weapon at time of discharges.

C.

Pipetting Technique and Confirmation of Pipette Calibration. 1. 2. Practice pipetting with each type of pipette. Confirm calibration of each pipette.

D.

Analysis of Samples. 1. Analyze prepared (In-house/known concentration) samples by Graphite Furnace AA. Analyze all GSR samples from (step “B “above) by Graphite Furnace AA. Interpret the results of GSR analysis.

2. 3. IV.

Co-Working Cases The student will work at least 10 cases with experienced examiners. This is to provide the student with experience in the various methods of case approach and examination of primer residue evidence. The student will observe the experienced examiner work the cases and will also interpret the results.

V.

Competency Samples After co-working cases with an experienced examiner, the student will be required to complete at least three competency test cases. The test cases are to be treated as casework and formal lab reports will be written by the examiner. One of the test cases will be chosen for the mock trial.

VI.

Written Test After completion of the competency samples, the student will be required to pass a written examination on the analysis of primer residue by GFAAS. Upon satisfactory completion of this test, the trainee will begin co-signing casework with a qualified examiner.

VII.

Co-signing Casework The new examiner will co-sign casework (minimum of 10 cases) with an experienced examiner. The scientist has the responsibility to analyze the evidence, interpret the

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results, and write a report on his/her findings. The case is co-signed with a more experienced examiner who is also responsible for examining the evidence and for reviewing the case notes and evidence to determine that the case was handled properly and that the primer residue conclusions are correctly reached by the new examiner. VIII. Mock Trial An in-house mock trial will be performed using one of the previously co-signed cases. IX. Required Reading 1. Basu, S., “Formation of Gunshot Residues”, J. Forensic Sci., 27(1), 72-91, 1982.Booker, J. L. and Schroeder, D. D., “A Note on the Variability of Barium and Antimony Levels in Cartridge Primers and its Implication for Gunshot Residue Identification”, J. Forensic Sci. Soc., 24(2), 81-84, 1984. Bydal, B. A., “Percussion Primer Mixes”, Assoc. Firearms and Toolmark Examiners J., 22, 1-26, 1990. Cooper, R., Guileyardo, J. M., Stone, I. C., Hall, V., and Fletcher, L., “Primer Residues Deposited by Handguns”, Am. J. Forensic Med. Pathol., 15, 325-327, 1994. Cornelis, R. and Timperman, J., “Gun Firing Detection Method Based on Sb, Ba, Pb, and Hg Deposits on Hands: Evaluation of Credibility of the Test”, Med Sci. Law, 14(2), 98-116, 1974. DeGaetano, D. and Siegel, J. A., “Survey of Gunshot Residue Analysis in Forensic Science Laboratories”, J. Forensic Sci., 35(5), 1087-1095, 1990. FBI Academy, Primer Residue Notebook Goleb, J. A. and Midkiff, Jr., C. R., “Firearms Discharge Residue Sample Collection Techniques”, J. Forensic Sci., 20(4), 701-707, 1975. Guileyardo, J. M., Stone, I. C., and Odom, C. B., “Gunshot Residue, Ten Years Later”, Am J. Forensic Med. Pathol., 13(1), 88, 1992. Havakost, D. G., Peters, C. A., and Koons, R. D., “Barium and Antimony Distributions on the Hands of Nonshooters”, J. Forensic Sci., 35(5), 10961114, 1990.
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2.

3.

4.

5.

6. 7.

8.

9.

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10. Kilty, J. W., “Activity After Shootings and its Effect on the Retention of Primer Residue”, J. Forensic Sci., 20, 219-230, 1975. Koons R. D., “ICP Atomic Spectrometry in the Forensic Laboratory”, Spectroscopy, 8(6). 16-21. 1993. Koons, R. D., “Flameless Atomic Absorption Spectrophotometric Determination of Antimony and Barium in Gunshot Residue Collection Swabs – A Collaborative Study”, Crime Lab Dig., 20, 19-23, 1993. Koons, R. D., Havekost, D. G., and Peters, C. A., “Analysis of Gunshot Primer Residue Collection Swabs Using Flameless Atomic Absorption Spectrophotometry - A Re-examination of Extraction and Instrument Procedures”, J. Forensic Sci., 32(4), 846-865, 1987. Koons, R. D., Havekost, D. G., and Peters, C. A., “Analysis of Gunshot Primer Residue Collection Swabs Using Flameless Atomic Absorption Spectrophotometry and Inductively Coupled Plasma-Atomic Emission Spectrometry – Effects of a Modified Extraction Procedure and Storage of Standards”, J. Forensic Sci., 34(1), 218-221, 1989. Krishnan, S. S., “Detection of Gunshot Residue on the Hands by Trace Element Analysis”, J. Forensic Sci., 22, 304-324, 1977. Krishnan, S. S., “Detection of Gunshot Residue: Present Status”, Saferstein, R., Ed., Forensic Science Handbook, Prentice-Hall, Englewood Cliffs, NJ. 1982, 1, 572-591. Krishnan, S. S., “Trace Element Analysis by Atomic Absorption Spectrometry and Neutron Activation Analysis in the Investigation of Shooting Cases”, J. Can. Soc. Forensic Sci., 16, 144-151, 1971. Meng, H. H. and Caddy, B., “Gunshot Residue Analysis – A Review”, J. Forensic Sci., 42(4), 553-570, 1997. Price, G., “Firearms Discharge Residues on Hands”, J. Forensic Sci. Soc., 5, 199-200, 1965. Reed, G. E., McGuire, P. J., and Boehm, A., “Analysis of Gunshot Residue Test Results in 112 Suicides”, J. Forensic Sci., 35, 62-68, 1990. Singer, R. L., David, D., and Houck, M. M., “A Survey of Gunshot Residue Analysis Methods”, J. Forensic Sci., 41(2), 195-198, 1996.
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12.

13.

14.

15.

16.

17.

18.

19.

20.

21.

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22. Stone, I. C., “Observations and Statistics Relating to Suicide Weapons”, J. Forensic Sci., 32(3). 711-716, 1987. Thornton, J. I., “Close Proximity Gunshot Residues”, J. Forensic Sci., 31, 756-757, 1986. Wallace, J. S., and McKeown, W. J., “Sampling Procedures for Firearms and/or Explosives Residues”, J. Forensic Sci. Soc., 33, 107-116, 1993. Wallace, J. S., and McQuillan, J., “Discharge Residue from CartridgeOperated Industrial Tools”, J. Forensic Sci. Soc., 24(5), 495-508, 1984. Wolten, G. M. and Nesbitt, R. S., “On the Mechanism of Gunshot Residue Particle Formation”, J. Forensic Sci., 25(3), 533-545, 1980. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., Loper, G. L., and Jones, P. F., “Equipment Systems Improvement Program – Final Report on Particle Analysis for Gunshot Residue Detection”, Rep. ATR-77 (7915)-3, The Aerospace Corporation., Washington, D.C., Sept. 1977. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., Loper, G. L., and Jones, P. F., “Particle Analysis for the Detection of Gunshot Residue. II: Occupational and Environmental Particles”, J. Forensic Sci., 24(2), 423430, 1979. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., “Particle Analysis for the Detection of Gunshot Residue. III: The Case Record”, J. Forensic Sci., 24(4), 864-869, 1979. Wrobel, H. A. and Millar, J. J., “Characterization of .22 Calibre Ammunition”, Scanning, 15(3), 118-119, 1993. Wrobel, H. A. and Millar, J. J., and Kijek, M., “Identification of Ammunition From Gunshot Residue and Other Cartridge Related Materials – A Preliminary Model Using .22 Caliber Rimfire Ammunition”, J. Forensic Sci., 43(2), 324-328, 1998.

23.

24.

25.

26.

27.

28.

29.

30.

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X. Checklist Upon completion of each element of the training, the trainee will be required to complete a prepared checklist. Upon the successful completion of the training program, the completed checklist will be reviewed by the trainer. The Trace Evidence Supervisor will send a memorandum of recommendation for Independent casework to the Chief of Physical Evidence and the Quality Manager for final assessment and official recognition of training completion.

Primer Residue/Handwiping Training Progress Checklist

Student’s Name:____________________________________________ ELEMENT 1. Operation/Maintenance of GFAAS 2. Completion of the required reading 3. Completion of Lectures 4. Completion of Practical Exercises 5. Completion of Competency Cases 6. Co-worked Cases 7. Co-signed Cases 8. Written test 9. Mock trial Instructor’s Signature _________________________________ Student’s Signature __________________________________

Date

Initial

Date __________________ Date __________________

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Dallas County Institute of Forensic Sciences Trace Evidence Unit

SEM/EDS GSR Training Manual, Version 1.1

Dallas County Institute of Forensic Sciences Forensic Laboratory

SEM/EDS Gunshot Residue Training Manual, version 1.1 Page 1 of 13

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Revisions & Corrections Trace Evidence Unit – SEM/EDS Gunshot Residue Training Manual, Version 1.1 Effective Date Description Changes from Version 1.0 to 1.1: • Revision: Revision to “Introduction” section for clarification purposes and to remove extraneous information. • Revision: Revision of “Student Responsibilities” section for clarification purposes. • Revision: Revision of “Lectures/Instruction” section to clarify lecture topics. • Revision: Revision of “Practical Exercises” section to add occupational samples. • Revision: Revision of “Co-working Cases” section remove “various methods of case approach” from the paragraph. • Revision: Revision of “Independent Casework” section to add the requirement of approval from the Section Chief and Quality Manager to begin independent casework. • Deletion: Deletion of “Bibliography” section. Selected references from bibliography and additional references were added to “Required Reading Material” section. • Revision: Revisions of page numbers and restructuring of outline. Authorized by Spence

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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL

Introduction Gunshot residue is produced during the discharge of a firearm can be deposited on the shooter=s hands and surrounding environment (including other individuals and inanimate objects such as clothing, car interiors, etc.). Gunshot residue particles (GSR) can be detected through the use of scanning electron microscopy/ energy dispersive x-ray spectroscopy (SEM/EDS). This protocol details the training process through a series of lectures, practical exercises, test samples, proficiencies, and casework. It is designed for a combination of working with an experienced examiner trained in primer gunshot residue analysis by SEM/EDS and selfinstruction by the trainee. Individuals with prior casework experience with GSR analysis by SEM/EDS in other laboratories may be exempted from some elements of the training protocol based on their previous training and experience. However, all competency tests must be completed successfully prior to new examiners performing casework. Student Responsibilities The student will be required to maintain a training log detailing his/her training progress. The training log should detail the dates and specific training activities performed such as articles read, lectures completed, and samples analyzed etc. The analyst should have the training instructor or Trace Evidence Supervisor review and initial the entries in the training log on a regular basis. The student should report periodically to the Trace Evidence Supervisor or Training Instructor to detail progress that has been made toward completion of the training protocol. The student shall use this time to discuss or clarify any issues related to the training material or exercises. Training assignments may require that the student devote additional time beyond their regularly scheduled work hours to complete the training in a timely fashion.

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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL

Required Reading Material The student must read the following reference materials prior to completion of training. Andrasko, J. and Maehly, A.C., ADetection of Gunshot Residues on Hands by Scanning Electron Microscopy@, J. Forensic Sci., 22(2), 279-287, 1977. ASTM E1588-07, Standard Guide for Gunshot Residue Analysis by Scanning Electron Microscopy/ Energy Dispersive X-ray Spectrometry Basu, S., AFormation of Gunshot Residues@, J. Forensic Sci., 27(1), 72-91, 1982. Basu, S., Ferris, S., and Horn, R., ASuicide Reconstruction by Glue-Lift of Gunshot Residue@, J. Forensic Sci., 29(3), 843-864, 1984. Basu, S., Boone, Jr., C. E., Denio, Jr., and Miazga, R. A., AFundamental Studies of Gunshot Residue Deposition by Glue-Lift@, J. Forensic Sci., 42(4), 571-581, 1997. Bergman, P., Springer, E., and Levin, N., “Hand Grenades and Primer Discharge Residues”, J. Forensic Sci., 36(4), 1044-1052, 1991. Berk, R.E., Rochowicz, Wong, M., Kopina, M.A., “Gunshot Residue in Chicago Police Vehicles and Facilities: An Empirical Study”, J. Forensic Sci., 52(4), 838-841, 2007. Bydal, B. A., APercussion Primer Mixes@, Assoc. Firearms and Toolmark Examiners J., 22(1), 1-26, 1990. Cooper, R., Guileyardo, J. M., Stone, I. C., Hall, V., and Fletcher, L., APrimer Residues Deposited by Handguns@, Am. J. Forensic Med. Pathol., 15(4), 325-327, 1994. DeGaetano, D. and Siegel, J. A., ASurvey of Gunshot Residue Analysis in Forensic Science Laboratories@, J. Forensic Sci., 35(5), 1087-1095, 1990. DeGaetano, D. and Siegel, J. A., and Klomparens, K. L., AA Comparison of Three Techniques
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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL Developed for Sampling and Analysis of Gunshot Residue by Scanning Electron Microscopy/ Energy Dispersive X-ray Analysis (SEM-EDX)@, J. Forensic Sci., 37(1), 281-300, 1992. Gerard, R.V., McVicar, M.J., Lindsay, E., Randall, E.D., Smaglinski, C., Harvey, E.A., “LongRange Deposition of Gunshot Residue and the Mechanism of its Transportation”, Scanning, 28(2), 106-107, 2006. Germani, M.S., “Evaluation of Instrumental Parameters for Automated Scanning Electron Microscopy/Gunshot Residue Particle Analysis”, J. Forensic Sci., 36(2), 331-342, 1991. Gialamas, D.M., Rhodes, E.F., Sugarman, L.A., AOfficers, Their Weapons and Their Hands: An Emperical Study of GSR on the Hands of Non-Shooting Police Officers@, J. of Forensic Sci., 40(6), 1086-1089, 1995. Goldstein, J.I., Lyman, C.E., Newbury, D.E., Lifshin, E., Echlin, P., Sawyer L., Joy, D.C., Michael, J.R. Scanning Electron Microscopy and X-Ray Microanalysis. 3rd ed. Chapter 8, 9 and 15. Kluwer Academic/Plenum Publishers, New York. 2003. Goleb, J. A. and Midkiff, Jr., C. R., AFirearms Discharge Residue Sample Collection Techniques@, J. Forensic Sci., 20(4), 701-707, 1975. Gunaratnam, L. and Himberg, K., AThe Identification of Gunshot Residue Particles from LeadFree Sintox Ammunition@, J. Forensic Sci., 39(2), 532-536, 1994. Halberstam, R. C., AA Simplified Probability Equation for Gunshot Primer Residue (GSR) Detection@, J. Forensic Sci., 36(3), 894-897, 1991. Hanson, A.M., Springer, F.A., “An Evaluation of Instant Shooter Identification (ISid™) Gunshot Residue Kits”, AFTE Journal, 37(3), 172-178, Summer 2005. Harris, A., AAnalysis of Primer Residue from CCI Blazer Lead Free Ammunition by Scanning Electron Microscopy/Energy-Dispersive X-ray@, J. Forensic Sci., 40(1), 27-30, 1995. Havakost, D. G., Peters, C. A., and Koons, R. D., ABarium and Antimony Distributions on the Hands of Nonshooters@, J. Forensic Sci., 35(5), 1096-1114, 1990.
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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL Kilty, J. W., AActivity After Shootings and its Effect on the Retention of Primer Residue@, J. Forensic Sci., 20(2), 219-230, 1975. Kosanke, K.L., Dujay, R.C., and Kosanke, B., “Characterization of Pyrotechnic Reaction Residue Particles by SEM/EDS”, J. Forensic Sci., 48(3), 1-7, 2003. Kosanke, K.L., Dujay, R.C., Kosanke, B.J., “Pyrotechnic Reaction Residue Particle Analysis”, J. Forensic Sci., 51(2), 296-302, 2006. Krishnan, S. S., ADetection of Gunshot Residue: Present Status@, Saferstein, R., Ed., Forensic Science Handbook, Prentice-Hall, Englewood Cliffs, NJ. 1982, 1, 572-591. Lebiedzik, J. and Johnson, D. L., AHandguns and Ammunitions Indicators Extracted from the GSR Analysis@, J. Forensic Sci., 47(3), 483-493, 2002. Lebiedzik, J. and Johnson, D. L., ARapid Search and Quantitative Analysis of Gunshot Residue Particles in the SEM@, J. Forensic Sci., 45(1), 83-92, 2000. Lindsay, E., McVicar, M.J., Gerard, R.V., Janson, N., “A Survey of Primer Residues Produced by Contemporary Powertool Rounds and Their Relation to Gunshot Residue”, Scanning, 29(2), 83, 2007. Matricardi, V. R. and Kilty, J. W., ADetection of Gunshot Residue Particles from the Hands of a Shooter@, J. Forensic Sci., 22(4), 725-738, 1977. Meng, H., Caddy, B., AGunshot Residue Analysis - A Review@, J. Forensic Sci., 42(4), 553-570, 1997. Mosher, P.V., McVicar, M.J. Randall, E.D., and Sild, E.H., AGunshot Residue-Similar Particles Produced by Fireworks@, Can. Soc. Forensic Sci. J., 31(3), 157-168. Nesbitt, R.S., Wessel, J.E., Jones, P.F., “Detection of Gunshot Residues by Use of the Scanning Electron Microscope”, J. Forensic Sci., 21(3), 595-610, 1976. Niewoehner, L., Wenz, H.W., Andrasko, J., Beijer, R., and Gunaratnam, L., “ENFSI Proficiency Test Program on Identification of GSR by SEM/EDX”, J. Forensic Sci., 48(4), 1-8, 2003.
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Niewoehner, L., Andrasko, J., Biegstraaten, J., Gunaratnam, L., Steffen, S., and Uhlig, S., “Maintenance of the ENFSI Proficiency Test Program on Identification of GSR by SEM/EDX (GSR2003)”, J. Forensic Sci., 50(4), 1-6, 2005. Oommen, Z., Pierce, S., “Characterization of Gunshot Residue Particles of Lead-Free PrimersFederal BalistiClean”, Scanning, 28(2), 105-106, 2006. Owens, A.D., AA Reevaluation of the Aerospace Corporation Final Report on Particle Analysis. When to Stop Searching for Gunshot Residue (GSR)?@, J. Forensic Sci., 35(3), 698-705, 1990. Reed, G. E., McGuire, P. J., and Boehm, A., AAnalysis of Gunshot Residue Test Results in 112 Suicides@, J. Forensic Sci., 35(1), 62-68, 1990. Schwartz, R. H. and Zona, C. A., AA Recovery Method for Airborne Gunshot Residue Retained in Human Nasal Mucus@, J. Forensic Sci., 40(4), 659-661, 1995. Schwoeble, A. J., Exline, David L., Current Methods In Forensic Gunshot Residue Analysis, CRC Press LLC, 2000 SEM/EDS Analysis of GSR Protocol, Southwestern Institute of Forensic Sciences Criminal Investigation Laboratory, Current Version Singer, R. L., Davis, D., and Houck, M. M., AA Survey of Gunshot Residue Analysis Methods@, J. Forensic Sci., 41(2), 195-198, 1996. Stone, I. C., AObservations and Statistics Relating to Suicide Weapons@, J. Forensic Sci., 32(3). 711-716, 1987. Stone, I.C., Ed., DiMaio, V.J.M., “Characteristics of Firearms and Gunshot Wounds as Markers of Suicide”, Am. J. Forensic Med. Pathol., 13(4), 275-280, 1992. Tassa, M., Adan, N., Zeldes, N., and Leist, Y., AA Field Kit for Sampling Gunshot Residue Particles@, J. Forensic Sci., 27(3), 671-676, 1982.
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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL Tillman, W. L., AAutomated Gunshot Residue Particle Search and Characterization@, J. Forensic Sci., 32(1), 62-71, 1987. Torre, C., Mattutino, G., Basino, V., and Robino, C., “Brake Linings: A Source of Non-GSR Particles Containing Lead, Barium, and Antimony”, J. Forensic Sci., 47(3), 494-504, 2002. Trimpe, M.A., “Analysis of Fireworks for Particles of the Type Found in Primer Residue (GSR)”, I.A.M.A, 4(1), 1-8, 2003. Ward, D., “GSR Summary”, FBI Laboratory, Unpublished Information White, R. S. and Owens, A. D., AAutomation of Gunshot Residue Detection and Analysis by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis (SEM/EDX)@, J. Forensic Sci., 32(6), 1595-1603, 1987. Wolten, G. M. and Nesbitt, R. S., AOn the Mechanism of Gunshot Residue Particle Formation@, J. Forensic Sci., 25(3), 533-545, 1980. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., Loper, G. L., and Jones, P. F., AEquipment Systems Improvement Program B Final Report on Particle Analysis for Gunshot Residue Detection@, Rep. ATR-77 (7915)-3, The Aerospace Corporation., Washington, D.C., Sept. 1977. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., Loper, G. L., and Jones, P. F., AParticle Analysis for the Detection of Gunshot Residue. I: Scanning Electron Microscopy/Energy Dispersive XRay Characterization of Hand Deposits from Firing@, J. Forensic Sci., 24(2), 409-422, 1979. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., Loper, G. L., and Jones, P. F., AParticle Analysis for the Detection of Gunshot Residue. II: Occupational and Environmental Particles@, J. Forensic Sci., 24(2), 423-430, 1979. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., AParticle Analysis for the Detection of Gunshot Residue. III: The Case Record@, J. Forensic Sci., 24(4), 864-869, 1979. Wright, D.M., Trimpe, M.A., “Summary of the FBI Laboratory’s Gunshot Residue Symposium, May 31-June 3, 2005”, FBI Laboratory, Forensic Science Communications, 8(3), 1-18, 2005.
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Wrobel, H. A. and Millar, J. J., and Kijek, M., AIdentification of Ammunition From Gunshot Residue and Other Cartridge Related Materials B A Preliminary Model Using .22 Caliber Rimfire Ammunition@, J. Forensic Sci., 43(2), 324-328, 1998. Zeichner, A., Levin, N., and Dvorachek, M., AGunshot Residues Formed by Using Ammunitions that have Mercury Fulminate Based Primers@, J. Forensic Sci., 37(6), 1567-1573, 1992. Zeichner, A., Levin, N.,ACollection Efficiency of Gunshot Residue (GSR) Particles from Hair and Hands Using Double Sided Adhesive Tape@, J. Forensic Sci., 38(3), 571-584, 1993. Zeichner, A., Levin, N.,ACasework Experience of GSR Detection in Israel, on Samples from Hands, Hair and Clothing Using an Autosearch SEM/EDX System@, J. Forensic Sci., 40(6), 1082-1085, 1995. Zeichner, A., Levin, N.,AMore on the Uniqueness of Gunshot Residue (GSR) Particles@, J. Forensic Sci., 42(6), 1027-1028, 1997. Zeichner, A., Foner, H. A., Dvorachek, M., Bergman, P., and Levin, N., AConcentration Techniques for the Detection of Gunshot Residues by Scanning Electron Microscopy/EnergyDispersive X-ray Analysis (SEM/ EDX)@, J. Forensic Sci., 34(2), 312-320, 1989 Zeichner, A., Levin, N., Springer, E., AGunshot Residue Particles Formed by Using Different Types of Ammunition in the Same Firearm@, J. Forensic Sci., 36(4), 1020-1026, 1991. Zeichner, A., Eldar, B., “A Novel Method for Extraction and Analysis of Gunpowder Residues on Double-Side Adhesive Coated Stubs”, J. Forensic Sci., 49(6), 1-13, 2004.

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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL Lectures/Instruction Topic 1 History of Primer GSR analysis Topic 2 Value and limitations of GSR as evidence. Topic 3 Terminology related to GSR analysis. Topic 4 Origin/source of GSR. Topic 5 Chemistry/formation of GSR. Topic 6 Types of firearms Topic 7 Plume studies of different firearms Topic 8 Transfer and persistence of GSR. Topic 9 Collection methods for GSR samples for SEM/EDS analysis. Topic 10 Sample preparation for SEM analysis Topic 11 Operation and maintenance of the Denton Vacuum DV-502 Coater Topic 12 Theory of operation for the Philips ESEM XL30 Scanning Electron Microscope and EDAX Energy Dispersive X-ray Spectrometer Topic 13 Operation and maintenance of the SEM/EDS - (Read/review ESEM XL30 Training Binder and operating manuals. Also, read/review EDAX Microanalysis Training Binder with two training video CDs and operating manuals Topic 14 Analysis of GSR by automated SEM/EDS. Topic 15 Interpretation and limitations of GSR results.

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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL Practical Exercises Collection of GSR Samples. Test-fire at least one firearm from each of the following categories: (revolvers, pistols, long-guns (semi-automatic and bolt-action). Collect GSR samples from each test-firing using SEM stubs. Collect residues from palms and backs of both the left and right hands of the shooter. Collect residues from the cuffs of the shooter=s shirt sleeves (wrap clean cotton cloth around the shooters wrists to simulate shirt sleeves). Collect residues from the shooter=s face. Analysis of GSR samples. Analyze the previously collected samples by SEM/EDS. Interpret the results of the GSR analysis. Describe the chemistry and morphology of the gunshot residue particles that were detected from the above tests. Compare the results of the GSR findings for each test-firing. Non-GSR Samples. Examine samples of each of the following minerals by SEM/EDS Barite (heavy spar, tiff) (BaSO4) Galena (PbS) Cerrussite (PbCo3)
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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL

Stibnite (SbS3) Talc Note typical morphology, size and elemental composition. Print out typical particles and their corresponding spectra. Environmental and Occupational Samples. Analyze environmental and occupational samples from fifteen individuals including the following: Cigarette lighter residue Automobile battery installer Brake installer Welder Note typical morphology, size and elemental composition of representative particles from each batch. Print out typical particles and their corresponding spectra. Knowledge Based Test A written test will be issued to assess the student=s knowledge and understanding of primer gunshot residue analysis. An acceptable score will be 70 or greater. The student will be required to show his or her knowledge and understanding of the basics of GSR analysis in order to progress to the next section in the training protocol. Co-working Cases The student will work a minimum of twenty five cases with experienced examiners. This will provide the student with experience with examination of primer residue evidence. The student will observe the experienced examiner work the cases and will also interpret the results.
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SEM/EDS GUNSHOT RESIDUE TRAINING MANUAL

Proficiency Samples After co-working cases with an experienced examiner, the student will be required to complete at least three proficiency test cases. The test cases are to be treated as casework and formal lab reports will be written by the examiner. One of the test cases will be chosen for a mock trial. Written Test After completion of the proficiency samples and prior to co-signing casework, the student will be required to pass a written examination on the analysis of primer residue by SEM/EDS. An acceptable score will be 70 or greater.

Mock Trial and Testimony Review An in-house mock trial will be performed based on one of the three proficiency sample cases previously worked. Upon successful completion and review of the mock-trial, the analyst will be allowed to begin co-signing casework with a trained examiner. Co-signing Casework The new examiner will co-sign casework (at least twenty-five cases) with an experienced examiner. The scientist has the responsibility to analyze the evidence, interpret the results, and write a report on his/her findings. The case is co-signed with a more experienced examiner who is also responsible for examining the evidence and for reviewing the case notes and evidence to determine that the case was handled properly and that the primer residue conclusions are correctly reached by the new examiner. Independent Casework Upon successful completion of all elements of this training protocol and approval by the Trace Evidence Supervisor, Section Chief and Quality Manager, the analyst will be allowed to perform independent casework in primer gunshot residue analysis by SEM/EDS.
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