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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
Description Authorizing
Individual
1/22/2008 Existing training procedures consolidated into a pdfcollection (Version 1.0); no changes made to individual
procedures
Sliter
1/23/2008 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 PatternAnalysis Training Protocol, Version 1.0
Fire Debris and Ignitable Liquid TrainingProtocol Version 1.0 replaced by Version 1.1
GC-MS Analysis Training Procedure ManualVersion 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 byVersion 1.1
Primer Residue Handwiping Training ProtocolVersion 1.0 replaced by Version 1.1
SEM EDS GSR Training Manual Version 1.0replaced by Version 1.1
Spence
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Revisions & Corrections
Bloodstain Pattern Analysis Training Protocol Version 1.0
Effective
Date
Description Authorizing
Individual
1/23/2008 Minor revisions described in memo of 1/18/2008 Spence
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SOUTHWESTERN
INSTITUTE OF FORENSIC SCIENCES
AT DALLAS
Trace Evidence Unit5230 Medical Center Drive
Dallas, Texas 75235
Interoffice Memorandum
To: Tim Sliter, Ph.D., Chief of Physical Evidence
From: DavidW. 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 Fire Debris and Ignitable Liquid
Forensic Laboratory 1 of 10 Training Protocol, version 1.1
Dallas County Institute of Forensic Sciences
Trace Evidence Unit
Fire Debris and Ignitable Liquid
Training Protocol, Version 1.1
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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 2 of 10 Training Protocol, version 1.1
Revisions & Corrections
Fire Debris and Ignitable Liquid Training Protocol Version 1.1
Effective
Date
Description Authorized by
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 1387were changed to ASTM Method 1618-06.
Addition: The classification scheme referenced inASTM Method 1618-06 was used in the description of
some of the lectures and practical exercises.
Deletion: Since the purge and trap attachment to theGC/MS is no longer in use, the practical exercise
using the purge and trap was removed.
Addition: A reference (Fire Debris Analysis byStauffer, Dolan and Newman) was added to the list of
reading in section II
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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 3 of 10 Training Protocol, version 1.1
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 in-
house 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, FBIor 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, CRCPress, 2004, Boca Raton.
o GC/MS Data Interpretation for Petroleum Distillate Identification in ContaminatedArson Debris, Raymond Keto, Journal of Forensic Sciences, 40(3), May 1995, pp.
412-423.
o Chemical Markers in Weathered Gasoline, Ronald Coulombe, Journal of ForensicSciences, 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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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 4 of 10 Training Protocol, version 1.1
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 GasChromatography/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 inExtracts 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 ongeneral 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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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 6 of 10 Training Protocol, version 1.1
Gasoline in dirt. Various mixtures. Wood samples. Carpet samples.
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 examiners 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 trainees 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 amore 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.
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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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 7 of 10 Training Protocol, version 1.1
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.
Ignitable Liquid Training Progress Checklist
Students Name: _____________________________________________________________
Initial and Date: Instructor(s) attest to the satisfactory completion of the element.
Element Date Initial
1. Basic GC/MS Course.
2. Fire Debris Training (ATF, NFSTC, FBI, etc.).
3. Philosophy of trace evidence examination.
4. Definitions of terms relating to Fire Debris Analysis.
5. Trace evidence transfer theory.
6. Operation of the oven.
7. Head space extraction.
8. Solvent extraction.
9. Head space vs solvent extraction.
10. Working with CS2.
11. HP GC/MS overview.
12. Using GC/MS and software.
13. GC/MS carousel.
14. Comparing samples (data analysis).
15. Overlaying samples.
16. Ignitable liquid worksheet.
17. Classification of ignitable liquids (ASTM).
18. Weathered samples and their analysis .
19. Target compounds for I. L. classification.
20. Flowchart for ignitable liquids.
21. Identifying ignitable liquids.
22. Note taking for casework.
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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 8 of 10 Training Protocol, version 1.1
23. Written reports.
A. Evidence description.
B. Reporting the examination and comparison process
procedure.
Element Date Initial
C. Examination results.
D. Examination conclusions.
E. Disposition of evidence.
24. Competency testing.
25. Reading.
A. GC/MS Guide to Ignitable Liquids. Newman, Gilbert &
Lothridge, CRC Press, 1998, Boca Raton.
B. 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.
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.
F. 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. 361-
370.
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.
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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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 9 of 10 Training Protocol, version 1.1
I. FBI Laboratory Analysis of Fire Debris Evidence course
book.
J. National Forensic Science Training Center, Advanced Fire
Debris Analysis Course student and reference manuals.
26. Conduct independent examinations and cosign reports.
27. Courtroom testimony principles.
28. Witness expert ignitable liquid court testimony (if possible).
29. Mock trial exercises.
30.
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.
B. 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.
2. 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.
3. After the new examiner has completed the second test sample, the assessor
and the new examiner will meet, preferably at the new examiners
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.
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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Dallas County Institute of Forensic Sciences Fire Debris and Ignitable Liquid
Forensic Laboratory 10 of 10 Training Protocol, version 1.1
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. Case approach principles.
2. Evidence examination principles.
3. Collection of trace evidence.
4. Examination of ignitable liquid evidence.
5. Appropriate conclusion development.
6. Final written report construction.
E. Review and update of the CHECKLIST by the assessor and new examiner.
F. A mock trial will be held prior to the new examiners first ignitable liquid testimony.
G. 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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Dallas County Institute of Forensic Sciences GC/MS Analysis / Training Procedure Manual, Version 2.1
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Dallas County Institute of Forensic Sciences
Trace Evidence Unit
Gas Chromatography / Mass Spectrometry
Analysis / Training Procedure Manual
Version 2.1
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Dallas County Institute of Forensic Sciences GC/MS Analysis / Training Procedure Manual, Version 2.1
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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 (capsaicinand 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 thisprotocol. 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.
2. Hands on experience using the interactive tutorials and training manuals
on the HP CD-ROM. Followed by the general test.
2. Thorough understanding of the general trace evidence procedures manualand clothing examination manual.
3. 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.
4. Working with an experienced analyst in the setup, calibration, QC and
general maintenance procedures of the GC/MS system.
5. Completion of a competency test where the analyst must set up theGC/MS, run any pertinent QC tests, and identify a chemical unknown
based on retention time and mass spectral data.
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 1618Test Mixture).
The type of analyte that can be detected will be dependant on two things: the solvent and
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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 requiredto 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.
2. Saferstein, R. (Ed.), Forensic Science Handbook, Vol II, Hall, Englewood Cliffs,
New Jersey, 1988, pp. 38-65 (David T. Stafford PhD., Chapter Author).
3. Jehuda, Y. (Ed.), Forensic Applications of Mass Spectrometry, CRC Press
Florida, 1995.
4. Jehuda Y. (Ed.), Forensic Mass Spectrometry, CRC Press, Florida, 1987.
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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 orrepair activities will be recorded in the GC/MS Logbook.
HP GC/Mass Spectrometer Maintenance Schedule
Daily/with use Tune (autotune)Refresh wash vialsCheck gases
As needed Change gas tanksReplace columnChange filamentChange septumChange linerChange gold sealCut columnsClean SourceClean split side armCheck autocal vialChange rough pump oil
MAINTENANCE OF THE HP6890 GC/5973 Series Mass Spectrometer
Maintenance activities should be consolidated to minimize instrument down time. Forexample, if it is time to change the gold seal and cut the column, it may be more prudent tochange the liner and septum at that time or hold off changing the gold seal until the linerand 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 tocompletion, 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 toavoid 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 freshKimwipe. 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. Oncemaintenance 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 andreplace the septum. Reinstall the top septum nut. These are not ultraclean parts butcare 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 recommendedthat liners be sonicated in solvent such as methylene chloride and dried in an oven priorto 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, wrench
Note: The gold seal is located at the bottom of the inlet. It is accessed through the nut inthe oven where the column comes out of the inlet.
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Use ultraclean technique at all times when handling the gold seal.
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 abovefor Changing the Liner and Septum.
3. Remove the column from the inlet. (Once the column is removed, the ferrule will need tobe replaced and the column cut.)
4. Remove the insulator cup (2 Phillips/Torx screws) to reveal the nut housing the goldseal.
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 asplitless 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 thecarrier 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, inch wrench
Any time a column is removed from the inlet or detector, the ferrule should be replaced andthe column should be cut.
The inlet end of the column may be cut several inches to remove active sites and restoreseparation capacity. The inlet ferrule should also be replaced.
1. Cool the inlet or detector to room temperature. This will minimize oxidation and preventburns.
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 cuttingcrystal and then snapping the column at the score.
b. Inspect this cut with a magnifying glass. This cut must be clean and containno 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. Cool the injector and detector.2. Turn off the carrier flow following the procedure in Changing the Liner and Septum.3. Loosen the column ferrules from the injector and detector and remove the column.4. Place a nut and ferrule on each end of the column. (The flat side of the ferrule goes
toward the nut.)5. Cut about inch from the inlet end of the column using techniques described in
Cutting the Column.6. Install the new column into the inlet only.
7. Use a plug to cap the detector entrance in the column oven. This step may not benecessary depending upon the type of column used. An MS column which has beendeveloped for use in a mass spec has extremely low column bleed and can beconditioned in the detector. Proceed to steps 9 and 10 before conditioning the columnin this case.
8. Condition the column. If conditioning is not done properly the column may be ruined.
a. Allow the carrier gas to flow through the column for approximately one hourwith the GC oven at room temperature.
b. Ramp the oven temperature at 10-15 degrees per minute to the finalconditioning temperature. The final conditioning temperature should be at
least 10 degrees higher than the maximum oven temperature to be used inthe method but may not exceed 10 degrees below the maximum operatingtemperature 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 causedeleterious 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. Tunesshould also be done before instrument operation after maintenance. For the 5973instrument 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. Low water and air - < 10%2. Correct mass assignments - +/- 0.2 amu (69, 219, 502)
3. Symmetrical, smooth mass peak shapes4. Consistent mass peak widths - +/- 0.1 units from target values.- 5973 peak width default is 0.60.
5. Appropriate EM voltage 1000 to 2800 electron volts. If the voltage is not withinthese limits, review the history of the electron multiplier or consult a supervisor.The EM voltage will increase over time as the source becomes dirty. Cleaningthe source should return the EM voltage to a normal operating level.
6. Isotope mass assignments should be 1 amu greater than parent peaks.7. Mass 69 abundance should be 200,000 to 500,000.8. Relative abundance:
- Mass 69 = 100%
- Mass 219 = 70 250 %- Mass 502 > = 3 %9. 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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Autotune:
Autotune maximizes instrument sensitivity over the mass range, using PFTBA masses69, 219, and 502. Use this tune for applications requiring maximum sensitivity that donot require traditional abundance ratios.
Standard Spectra Tune:
Standard Spectra Tune ensures standard response over the full mass range. This tunemay 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 accuratemass assignment. Only the mass axis, peak widths, and EM voltage are adjusted; thelenses 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 noteof any error messages generated by the Chemstation Software, and check all sourcesof leaks for tightness. Re-evaluate the instrument, and monitor the instrument throughthe manual tune functions of the software. Once the problem is corrected, an Autotuneand Standard Spectra Autotune shall be performed, and technical information andtroubleshooting performed written in the GC/MS Logbook. If further assistance isneeded, 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
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Users may begin using the chemstation by clicking on the top icon (namedGC/MS Instrument # 1) located on the desktop. There are several ways to move aroundin the chemstation software. The following instructions are a guideline in which to followand will not represent all of the ways that may be possible. The primary method ofmovement from one screen to another in the chemstation software is through the viewmenu item. If you are in the top level, instrument control or data analysis, the viewmenu 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 methodsand 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 instrumentparameters such as injector, inlet, column parameters, oven parameters, mass spectemperatures, and electron multiplier voltages. The user can also edit, load, save andprint methods from this screen. This screen enables the user to monitor instrumentparameters 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 thelocation 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 MassSpectrometer Chemstation there are three key areas of storage.
Data is stored in C:\hpchem\1\data. Data consists of data.ms files containing total ionchromatograms and their spectra, pre_post.ini files containing information on the status
of theinstrument during the run of the indicated file, and log files containing informationregarding the sequence that was run.
Methods are stored in C:\hpchem\1\methods. Methods contain all of the informationrequired to execute a run. Methods contain the required macros and instrumentparameters such as oven ramp parameters, pressure and flow parameters, injectionparameters, and instrument temperatures as well as other information.
Sequences are stored in C:\hpchem\1\sequence. Sequences contain the informationrequired to complete a series of injections utilizing the autosampler tower and tray. Theinformation 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 selectedsequence in the instruments memory. Proceed toEdit sequence section to edit the sequence orRunning a sequence section to run the loadedsequence.
Edit sequence
Once the desired sequence has been loaded you may want to edit the sequence. Fromthe 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 previouslyloaded. 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 othersequences.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 thehighlighted line for all other information.
Cut will delete the highlighted line (will hold it in memory for paste function untilanother cut or a copy is executed).
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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 thecurrent 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 tothe running sequence. If the sequence is running the menu items will not be availableand the user must select the edit sample log tbl button from the center screen. At thistime, the edit sequence screen will appear.
Saving a sequence
After the user has loaded and edited a sequence, hemust 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 andrun 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 auser specified location within the current sequence. To begin a sequence from the toplevel:
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 toselect the overwrite existing data files. Select the appropriate option on thebarcode mismatch section.
5. Type the correct path for the storage of data. The default path isC:\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 thedefault 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 selectionsto 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 positionwithin a sequence before the above screen appears.
Using Keywords
The chemstation allows the use of keywords within a sequence. These keywords allowthe user to perform certain functions within the sequence such as running a commandor macro, tuning the instrument, pausing the sequence and more. The most commonkeyword used is pause. The pause command will allow the user to pause thesequence after the current injection and method are complete. To use a keyword thesequence 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 rungreyed out.
3. Select the next line to be run, copy and paste so there are two identical lines.4. Select the
keywordcommand in thetype box.
5. This will promptthe user to typethe keyword that
is to be used.Select thekeyword in thekeyword box.
6. Select ok.When the current method iscomplete the keywordcommand will be executed.
II. Methods
The method in the chemstation software is the location of all of the instrumentparameters and data analysis parameters that will take place during the execution of amethod in a sequence. Methods should only be created or modified by those withknowledge 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 selectmenu items from either the top level screen or
the instrument control screen. From eitherscreen:
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 createyour new method.
4. Select the save menu item to savethe method.
Editing an existing method
If the user needs to edit a method or check the contents of a method, he can access themethod 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 youhave 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 iconon the desktop, from the top level screen during the execution of a sequence, or fromthe 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 identifiedcompounds in the chromatogram. To load a chromatogram:
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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 thatwas specified when the sequence was started. The default location is C:\HPC
Reviewing Data
Once the chromatogram has been loaded it will appear in window 2. It will appear asthe total ion chromatogram (TIC) with peaks representing detector response tocompounds 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 forspecific ions, comparing unknown spectra to known libraries, generating reports, andprinting spectra.
The TIC will be normalized on the largest peak. This means that the largest peak willbe completely visible from the top of the peak to the baseline. Large peaks in a TICmay make smaller peaks not visible when looking at the normalized chromatogram. Ifthe user wishes to look at the smaller peaks he can zoom in on the peak. To do this leftclick and hold the mouse, drag a box around the area to be analyzed and release. Thiswill 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 mousebutton at the point of interest. This will generate a mass spectrum of the area that wasclicked 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 foruse (see searching libraries for instructions on changing). To compare the generatedspectrum 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 shownfirst. This comparative spectrum is generated in window 24.
The spectrum for the unknown compound is located on top and the spectrumfor the best match is located on the bottom. The library that the best matchspectrum came from is listed in the PBM Search Results box.
3. To print the comparison select the print button located in the PBM SearchResults box.
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The user may also want to print the TIC or the unknown spectrum without using thecomparison method. To do this:
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1. Load chromatogram and generate spectrum.2. Select the file menu item.
3. Select the print menu item.4. The user will be prompted to enter the windowthat he wants to print. Enter the number of thewindow that you wish to print: 1 = spectrum, 2 =TIC.
Searching for specific ions
When a specific ion needs to be isolated so the user mayseparate coeluting compounds or find a compound with aweak response, the chemstation can search for specific ions within a TIC. To do this:
1. Select the chromatogram menuitem.
2. Select the extract ionchromatograms menu item
3. This will prompt the user to enterthe ion or ions that thechemstation will look for and the
retention time windows in which tolook.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 ina different color. Full spectrum may be generated by double clicking the right mousebutton 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 ishidden 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 userwould look for the ions in the compound of interest by a manual search or by searchingfor extracted ions. Once the compound is found the full spectrum may have ions fromthe baseline included in the ions for the compound. The chemstation allows the user tosubtract one spectrum from another to clean up or clarify a spectrum. To subtract aspectrum:
1. Obtain a spectrum of the compound (with theinterfering ions).
2. Move the cursor to a location, usually just beforeor 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 secondobtained spectrum removed from the first obtainedspectrum. When the subtract menu item is selected it willsubtract the current spectrum in window 1 from theprevious spectrum that was in window 1 and show thedifference of the two in window 1.
Printing reports
There are many ways to print reports and a number of reports are available in thechemstation software. The most common way to print a report for a designated methodis 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 asequence.
The user may also want to use the options available under the quantitate and toolsmenu items.
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Using the quantitate menu item the user will be limited to the chemstation report formatand any custom reports will not apply.
The tools menu item allows the user to reprocess quantitative and qualitative reportsand are linked to custom reports found in the deuser.mac macro associated with eachmethod.
Searching Libraries
There are many different libraries that are available in the chemstation ranging from in-house 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 automaticallysearched 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 spectrumto a library spectrum.
Once a spectrum is obtained in window 1, the user can also search specific libraries byselecting 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 compoundsbased 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 automaticallyand perhaps manually. The user will be trained on an individual basis regardinginterpretation 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 referencecollection found near each instrument.
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Revisions & Corrections
Glass Analysis Training Protocol Version 1.0
Effective
Date
Description Authorizing
Individual
1/23/2008 Revisions described in memo of 1/18/2008 Spence
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SOUTHWESTERN
INSTITUTE OF FORENSIC SCIENCES
AT DALLAS
Trace Evidence Unit5230 Medical Center Drive
Dallas, Texas 75235
Interoffice Memorandum
To: Tim Sliter, Ph.D., Chief of Physical Evidence
From: DavidW. 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 Gunshot Residue and Range Determination
Forensic Laboratory Training Manual, Version 1.1
Page 1 of 9
Dallas County Institute of Forensic Sciences
Trace Evidence Unit
Gunshot Residue and Range
Determination Training Manual
Version 1.1
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Dallas County Institute of Forensic Sciences Gunshot Residue and Range Determination
Forensic Laboratory 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 Authorized by
Changes from Version 1.0 to 1.1:
Revision: Revision of section IX.: change of title toIndependent Casework and clarification of
documentation required to complete training
Revision: Revision of section III.: to add/clarifytraining topics
Revision: Revision of section X.: to add references. Revision: Revisions of page numbers
Spence
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Forensic Laboratory 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 performcasework 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 gunshotresidue and range determinations. Lists of required and recommended readings can be
found at the end of this training manual.
LecturesB 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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Test Firing Procedures. Range of Fire Estimations. Interpretation of Results.
III. 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 togunshot residue analysis.
2. A proper and complete understanding of all information and procedures neededprior to the execution of any gunshot residue analyses which includes:
a. Checking out evidence and establishing an official chain of custody.
b. Utilizing Field Agent and Medical Examiner=s reports as supplemental
information.
c. Following universal precautions for blood borne pathogens, contamination
and integrity of evidence at all times.
d. Solution preparation, quality control and quality assurance for the
Modified Griess, Sodium Rhodizonate, and Dithiooxamide (DTO) tests.
e. Proper etiquette when speaking to investigators, attorneys, etc.
3. Basic firearms knowledge and ballistics training is necessary to understand thesources of gunshot residue. Time spent with a firearms examiner is useful. Areas
to be covered should include:
a. Firearms safety.
b. Pertinent firearms terminology.
c. Study, observe, draw and describe gunpowder knowns (burned and
unburned).
d. Become familiar with various types of firearms (automatic, semi-
automatic, revolvers, shotguns, rifles) and ammunition.e. Components and firing process of the cartridge.
f. Actions of residues before, during and after discharge as they travel
toward and deposit on the target.
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g. Various shot sizes and other shotgun ammunition as well as generalArules
of thumb@ for shotgun distances.
h. 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. Inventorying the evidence.
b. Defect location, visual observation and comprehensive note taking.
c. Microscopic examination for the presence of gunpowder and gunshot
residues
d. Modified Griess test for gunpowder residue.
e. Sodium Rhodizonate test for lead residue.
f. Dithiooxamide test for copper and nickel residue (as needed).
g. Test firing and how to make a justifiable range of fire estimation.
h. Proper packaging of press-outs and appropriate release of evidence.i. Photography of significant defect and/or residue patterns, as needed.
5. Following the analysis of the evidence the trainee should understand how tointerpret the results and prepare a report as to those findings.
6. Observation of court testimony in the area of gunshot residue analysis is anecessary 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 asknowledge 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 anexperienced 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. Thisis 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 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 Date Initial
1 Evidence handling and documentation
2 Firearms terminology and safety
3 Modified Griess test
4 Sodium Rhodizonate test
5 Dithiooxamide test
6 Shotgun and rifle evidence
7 Test firings
8 Handgun practical exercises
9 Rifle practical exercises
10 Shotgun practical exercises
11 Interpretation/Results
12 Report writing
13 Testimony observation
14 Written test
15 Competency test
16 Mock trial
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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 forLead in Gunshot Residues, John Dillon, AFTE Journal, 22(3), July 1990, pp.
251-256.
4. Gunshot Wounds: Practical Aspects of Firearms, Ballistics, and ForensicTechniques, 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 DistanceDetermination, 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 DistanceDeterminations, John Dillon, AFTE Journal, 23(1), January 1991.
5. Characterization of Smokeless Powder Flakes from Fired Cartridge Case andfrom 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 inthe 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 andBarrel 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 PatternsProduced 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 GSRPatterns on Bloody Garments, L.C. Haag, AFTE Journal, 23(3), p. 808-815.
14.Forensic Applications of Infrared Imaging for the Detection and Recording ofLatent Evidence, Lin, Heish, Tsai, Linacre and Lee. Journal of ForensicSciences, Vol. 52. No. 5. p. 1148-1150.
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Dallas County Institute of Forensic Sciences Hair Training Protocol, version 1.1
Forensic Laboratory 1 of 11
Dallas County Institute of Forensic Sciences
Trace Evidence Unit
Hair Training Protocol, Version 1.1
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Revisions & Corrections
Trace Evidence Unit Hair Training Protocol, Version 1.1
Effective
Date
Description Authorized by
Changes from Version 1.0 to 1.1:
Revision: Revision of Section II to delete duplicateentries 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 addde-mounting of hairs to lecture list.
Revision: Revision to Section II, subsection E toclarify types of reference samples to be examined and
to delete chemotherapy hairs.
Revision: Revision of section ordering to allow forbetter flow in training process.
Deletion: Deletion of Second Opinion Caseworksection and duplicate entry of Competency Test
section.
Revision: Addition of Section IX: IndependentCasework
Revision: Revision of Appendix 1 Hair TrainingProgress Checklist to delete crime scene processing
and wigs from the training topics and to re-order
sections.
Revision: Revisions of page numbers and sectionnumbers.
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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 isnot 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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LecturesB A series of explanations/discussions is pr