SWIFS Trace Evidence Procedures Collection v2.3 (02.24.2009) - Re Formatted 330 Pages

This is an uncontrolled copy of a controlled document
Southwestern Institute of Forensic Sciences Criminal Investigation Laboratory
Trace Evidence Procedures Collection, Version 2.3 Effective 2/24/2009
Approved by: David Spence, Trace Unit Supervisor Timothy J. Sliter, Ph.D., Section Chief Karen Young, Quality Manager

Revisions & Corrections Log SOP: Trace Evidence Procedures Collection
Effective Date 3/15/05 12/29/2005 Description 2004 Trace Manuals were reviewed by Dr. Sliter All administrative & technical procedure manuals of the Trace Evidence Unit were reauthorized for use by Dr. Sliter Replace page 22 of 29 SEM/EDS Analysis of GSR Protocol Section 12.3.2 (Plano Std) Memo to replace SEM/EDS Analysis of GSR Protocol Section 12.3.2 (Plano Std) Revisions to Common Abbreviations (Added to section) Hardcopy procedures converted to electronic format (pdf). Hardcopy manual archived. Procedure for Housekeeping Version 1.0 replaced with Version 2.0 Individual procedures compiled into Trace Procedures Collection, Version 1.0 Version 1.0 archived and replaced by Version 2.0, with the following changes: Analytical Balance Procedure Version 1.0 replaced by Version 1.1 Bloodstain Pattern Analysis Procedures Version 1.0 replaced by Version 1.1 Fire Debris Procedure Manual Version 1.0 replaced by Version 1.1 Glass Analysis Protocol version 1.0 replaced by Version 1.1 GSR and Range Determination Procedure Manual Version 1.1 replaced by Version 1.2 Hair Procedures Version 1.0 replaced by Version 1.1 Housekeeping Procedure Version 2.0 replaced by Version 2.1 Primer Residue by AA Protocol Version 2.1 replaced by Version 2.2 SEM GSR Analysis Version 1.0 replaced by Version 1.1 Trace Recovery General Procedure Manual Version 1.0 replaced by Version 1.1 Common Abbreviations used in Trace Evidence Laboratory Version 1.0 revised by Memo Authorizing Individual Dempsey Dempsey
5/12/2006 10/18/06 4/3/2007 5/1/2007 8/7/2007 11/12/2007 1/22/08
Dempsey Dempsey Sliter Sliter Sliter Sliter Spence
Trace Evidence Procedures Collection, Version 2.2 Effective Date: 5/5/2008

2/28/2008 Changes from Version 2.0 to Version 2.1 Replacement of SEM/EDS Analysis of GSR Protocol Version 1.1 with Version 1.2 Changes from Version 2.1 to Version 2.2 1) Revisions to SEM GSR Analysis (Version 1.2 to Version 1.3): Revision: Revision to Section 5.3.1 and its subsections Revision: Revision to Section 6.2.1.5 Revision: Revision to Section 6.2.1.11 Revision: Revision to Section 6.2.2.5 Deletion: Deletion of Section 6.2.2.18 Addition: Addition of Section of 8.3 Addition: Addition of portable external hard drive to Section 3.3 Addition: Addition of appendix documents: o Class Library Definitions Original o Class Library Definitions Revised 5/5/2008 (revised to remove Silicon from the class definitions) 2) Revisions to Fire Debris and Ignitable Liquid Procedure Manual (Version 1.2 to Version 1.3) Addition of Appendix 5 - Archival of Digital Instrument Data and Sequence Files Addition: Fabric and Materials Damage Analysis, Version 1.0 (02.24.2008) Spence
5/5/2008
Spence
2/24/2009
Spence
Trace Evidence Procedures Collection, Version 2.2 Effective Date: 5/5/2008

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 15, 2008 Subject: Changes to the list of common abbreviations used in the Trace Evidence Laboratory
This memo will serve to document changes being made to the list of common abbreviations used in the Trace Evidence Laboratory. The following changes as follows: PLM or P.L.M. Polarized light microscope or Polarized light microscopy MSP Microspectrophotometer or microspectrophotometry ABS Apparent bloodstain(s) Agg or agg. Aggravated Asslt Assault Att or att. Attempted Cal or cal. Caliber Overd Over-range or Over-read Prof Proficiency C Control or control swab CC Cartridge case or carbon copy s/n or S/N Serial number or signal to noise ratio Comp Component or complainant Evid or evid. Evidence Fr or fr Front Hom Homicide Id or id Identified Num Numerous or number

Changes to the list of common abbreviations used in the Trace Evidence Laboratory
QC Quality Control LB Left hand back LP Left hand palm RB Right hand back RP Right hand palm RH Right hand LH Left hand Robb Robbery RSD Relative Standard Deviation Susp Suspect Und Undetermined Wit Witness dep Deposit def Defect w/i within - Positive - Negative, none, zero rxn(s) Reaction(s) Det. Detective Inv. Investigator DA or D.A. District Attorney Ignliq Ignitable liquid IL Ignitable liquid Flam Flammable DCDA Dallas County District Attorneys Office SO or S.O. Sheriffs Office PD or P.D. Police Department Man. Env. Manila envelope Man. Manila Env. - Envelope
January 15, 2008 Page 2 of 2
Dallas County Institute of Forensic Sciences Trace Evidence Unit
Trace Evidence Recovery Examinations General Procedures, Version 1.1
Evidence Recovery - General Procedures, Version 1.1 Page 1 of 8
Revisions & Corrections Trace Evidence Unit Trace Evidence Recovery Examinations General Procedures, Version 1.1 Effective Date 1/22/08 Description Changes from Version 1.0 to Version 1.1: Revision: Revision to Section III to add SEM sample stubs. Revision: Changes to Section III to include generic sticky notes and plastic bags: Deletion: In Section III, deletion of 5. Chemical Reagents and Knowns Sufficient for Presumptive Testing Revision: Revision to Section V to clarify information/documentation required in notes Deletion: Deletion of Section VI Packaging/Sealing/Labeling Deletion: Deletion of Section VI, subsection d., which required that lab coats be worn at all times while handling exhibits. Revision: Revisions of page numbers and section numbers. Authorized by Spence
Trace Evidence Recovery - General Procedures, Version 1.1 Page 2 of 8

TRACE EVIDENCE RECOVERY EXAMINATIONS - GENERAL I. OBJECTIVE / INTRODUCTION
The object of this protocol is to provide guidelines for procedures to collect, analyze, document, and preserve trace evidence. Trace evidence includes hairs, fibers, paint, glass, gunshot residue, and other substances capable of characterization, identification, and comparison by various microscopic, microchemical, or analytical techniques. Clothing examinations, damage assessment, and fabric impressions are also sometimes required prior to trace evidence evaluations. The primary function of the forensic scientist is to locate, isolate, identify, and compare evidence of unknown origin and determine possible origin or similarity to control samples of a known source. II. TRAINING
Training in trace evidence examination and collection is provided primarily by experienced examiners and by individual experience as part of basic microanalysis training. More specific information on examination and collection of trace evidence is covered in the separate manuals. III. 1. 2. TOOLS/EQUIPMENT Adequate-Sized and Ventilated Work Surfaces for the Examined Object Adequate Lighting 3. Visible Ultraviolet B Other, as needed
Magnification Magnifying lamp Stereoscope Hand lens
4.
Tools Probes Tweezers Transparent adhesive tape Glass slides and cover slips SEM sample stubs Ruler and tape measure Scraper Note-taking materials

5.
Sketching materials Sticky notes
Packaging Materials Envelopes Paper Plastic bags Boxes Petri-dishes Evidence/Security tape Paper bags
6.
Microscopes Stereomicroscope Polarizing Light Microscope Compound Microscope with phase contrast capabilities Comparison Microscope with epi-illumination and both bright field and dark field capabilities
IV. 1.
ANALYSIS/EXAMINATION Contact Requesting Agency/Detective for a Case History as needed a. Relationship of individuals to the crime b. Name of victim (all victims) Name of suspect (all suspects) Relationship (or not) between victim(s) and suspect(s) Other individuals associated with the incident
Scene(s) of crime Is the scene related to a victim or a suspect? If so, was the other (suspect or victim) ever there before? How long ago? If not, how did they get there? Vehicle involved?
c.
Sequence of events leading to incident Victims account Suspect(s) account Why this person is suspected of the crime Witness accounts

d.
Investigators suspicions (and basis)
In a homicide Cause of death Instrument of death (weapon?) Time of death Is autopsy report available? Photos
e. f. g. h.
How soon after the crime was evidence collected? How soon after the crime was suspect(s) apprehended? Did victim go to a hospital? How long after the incident? Do we have all necessary controls? For example, if a rape took place in a stolen car, we need hair control samples from usual users of that car.
i.
What are the elements of proof which laboratory work can address? The direction that the examination takes may be different from the first information request by the agency.
j.
What other physical evidence in this case has been collected? Latent prints? Medical or dental reports? Evidence which has been submitted to other labs? Is there a trial date? Is lab work needed before something else can be done?
2.
Decide on Approach to Case a. b. c. Does other work need to be done prior to trace recovery examination (gunshot residues, volatiles analysis, etc.)? Determine relative significance of the submitted items. Decide on best way to examine evidence - incorporate additional expertise, if necessary (multiple functional area approach). i. In order of importance of evidence submitted.

ii. d. If other laboratory sections should be involved.
Be aware of what is of primary interest - possibly look at control samples prior to performing clothing exam.
3.
Prepare Work Area Space is adequate and clean Lighting sources are available Clean paper is covering work surface; prevent contamination Sufficient tools are handy
Examination Examination of each evidence type will be covered by separate chapters of this manual. See specific chapters for techniques and examination procedures. V. 1. NOTE-TAKING Purpose To completely document observations, results, and thought processes in order to be able to reconstruct the analysis and support conclusions at a future date. 2. Minimum Contents a. b. Submittal Information Describe packaging/labeling/seals/evidence numbers, etc., for each item examined Description of evidence i. ii. iii. d. Be able to identify article at a later date - color, size, manufacturer, etc. Condition - wear, damage, etc. Note deposits (location), damage, etc.
c.
Briefly describe examination of evidence i. ii. Sequence of exams Alteration of evidence

e. Provide a general description of the collected trace evidence. Note what type of evidence is present, relative frequency of occurrence, colors, size, etc. Attach instrumental hard copies (spectra, charts) Disposition of trace evidence i. ii. How packaged (container) Where trace evidence can be located (i.e., with examined article, separately packaged, etc.)
f. g.
h. VI. 1.
Analysts initials and FL # on all pages
QUALITY ASSURANCE Ensure ability of analyst to adequately and accurately collect trace evidence. a. b. c. Adequate training Tests samples Proficiencies (incorporated into each sub-discipline)
2.
Insure analyst can recognize and attach proper significance to evidence associated with the examined evidence during training. a. b. Co-working/co-signing casework Reexamination/review of evidence by peers
3.
Insure analyst can properly recognize and preserve evidence for future analyses. a. b. Understanding and usage of methods outlined in this section Co-working/co-signing casework during training
4.
Ensure analyst takes proper precautions to prevent contamination and/or loss of evidence by understanding and utilizing the methods outlined in this section. Ability to reconstruct the examination and support conclusions. a. Proper note-taking procedures
5.
6.
b. Adequate peer review Ability of an analyst to prepare an accurate and thorough report.
a. b. 7.
Proper report writing procedures Adequate peer review
Insure that analyst remains current in techniques used for examination of evidence. a. b. c. d. Ongoing proficiency testing Reference library collection and maintenance Stay current on journals or texts regarding evidence examination In-house sharing of information and interesting case work
8.
Contamination control/prevention a. b. Laboratory exhibit lockers are kept as clean as possible No more than one case in an unpackaged state is allowed on any examination table at any one time The examination table is carefully cleaned between examinations of each exhibit Every precaution should be taken to prevent cross-contamination between suspect and victim evidence items including: i. Where possible, garments from any suspect(s) are examined on different examination tables or at least at different time intervals than garments from the victim(s) Exhibit tape lifts are examined as far away as possible from the examination area
c. d.
ii.
VII.
BIBLIOGRAPHY
A bibliography or reference list of reading material is provided at the end of each individual procedure and training manual.
Analytical Balance Procedure and Calibration Log, Version 1.1
Dallas County Institute of Forensic Sciences Forensic Laboratory
Analytical Balance Procedure & Calibration Log, Version 1.1 Page 1 of 6
Revisions & Corrections Trace Evidence Unit Analytical Balance Procedure and Calibration Log, Version 1.1 Effective Date 1/22/08 Description Changes from Version 1.0 to Version 1.1: Correction of a typographical error: The standard weight of 500 grams used for the monthly balance check was corrected to 100 grams Deletion: Quality Control / Quality Assurance The last line of the paragraph At that time a new antistatic bar is placed inside the chamber was removed. Revision: The 500 mg and 5g weights are weighed and logged before each use of the balance was changed to read: The 500 mg and 5 g weights are weighed and logged before each use of the balance unless the monthly calibration check was performed on that date. Authorized by Spence
ANALYTICAL BALANCE PROCEDURE AND CALIBRATION LOG

Principal & Scope The analytical balance is used in the preparation of chemical reagents required by other procedures in the Trace Evidence Unit. On occasion, the balance is used for weighing articles related to casework. Equipment Mettler AE163 analytical balance, Dallas County Property Tag # 49657, See diagram on page 5 Standards Certified weights of 500 mg and 5 g are used to check the calibration of the balance before each use unless the monthly calibration was performed on that date. Once a month during months of use, the balance is checked using outside calibrated weights of 0.01, 0.20, 1.0, 50 and 100 grams. Certificates of calibration are kept on file with the Quality Manager. Procedures For specific troubleshooting and procedures, refer to the balances Operating Instructions Manual. 1. 2. 3. With the side doors closed, turn on the balance by pressing downward on the control bar. Make sure the balance is level by checking the bubble in the spirit level. If the balance is not level, adjust the leveling screws. Once the balance has zeroed and is level, open one side door and place the 500 mg weight using tweezers on the metal plate. Notate the weight on the log sheet. Do the same for the 5 g weight. If both weights fall within tolerances (+/- 3 percent), continue with the procedure. If not, follow the instructions for recalibrating in the Operating Instructions Manual. Follow a recalibration by weighing the full set of outside weights. Make sure to notate the recalibration on the log sheet. Use the same procedure for the monthly check of the full set of weights. To weigh a sample, tare the balance (clear to zero) and then insert the weighing receptacle (boat, paper, beaker, etc.) on the metal plate. Close the side door and depress the control bar to tare the balance again. Add the sample to the receptacle until desired weight is reached. Be careful not to spill! Record the indicated weight. Carefully remove the receptacle and close the side door. Turn the balance off by lifting up on the control bar. Clean the area inside the balance chamber and the area surrounding the outside of the balance as needed.
4.
5. 6. 7. 8. 9. 10. 11.
Quality Control / Quality Assurance The full set of calibration weights is used once a month unless the balance is not used for that month and the findings recorded on the log sheet. The 500 mg and 5 g weights are weighed and logged before each use of the balance unless the monthly calibration check was performed on that date. The difference in values must be within +/- 3 percent measured on the balance. If the values do not fall within the above tolerance, the balance shall be retested. Should the balance still not fall within the above tolerance, the balance may be recalibrated in-house according to the recalibration procedure in the instrument manual. Should the balance still not fall within the above tolerance, the balance shall be taken out of service by placing documentation in the balance log book and by placing an Out Of Service sign on the instrument. Prior to placing the balance back into service, the balance shall be serviced by a qualified technician and tested to insure that the balance falls within the above tolerance. On a yearly basis, an external service provider services and calibrates the balance, as well as takes the full set of weights off-site for calibration and certification. Safety Universal precautions for handling biohazards and chemicals shall be observed. All chemicals and chemical solutions should be properly labeled. Care should be taken to clean up any chemical spill in accordance with the proper procedures outlined in the Health and Safety Manual.
METTLER AE163 ANALYTICAL BALANCE DC # 49657
ANALYTICAL BALANCE CALIBRATION LOG

BALANCE # AE163 DALLAS CO. # 49657 TRACE EVIDENCE UNIT
DATE INITIALS EXPECTED WEIGHT MEASURED WEIGHT OK/RECAL MONTHLY CHECK
Procedures for Bloodstain Pattern Analysis Version 1.1
Procedures for Bloodstain Pattern Analysis, Version 1.1 Page 1 of 15
Revisions & Corrections Procedures for Bloodstain Pattern Analysis, Version 1.1 Effective Date 1/22/08 Description Changes from Version 1.0 to Version 1.1 Corrections: Various nonsubstantive grammatical corrections Revision: Section 2.3.5.2 was changed to read In the event that an item is judged to be suitable for BPA, further screening for BPA will be performed by the bloodstain pattern analyst. Collection of bloodstains and presumptive testing of bloodstains will be performed by qualified staff of the Forensic Biology Unit (FBU). Revision: Section 2.4.3.3. was changed to read The administrative review of the report and case file will be conducted by another trained BPA analyst. Revision: Section 3.3.1 was changed to read The condition and appearance of significant bloodstain pattern(s) used for interpretation may be documented photographically, using a digital camera or film camera. Addition: Section 3.3.4 was added and states Specific areas and stains that are subjected to presumptive blood testing and sampling for species and DNA typing will be documented by the examiner performing the testing. The documentation will be either through diagrams or photographic documentation. Revision: In Section 3.4.2.1, the measurement for small stains was changed from 2 mm to 2 cm. Revision: In Section 3.4.2.2, ruler was changed to scale. Revision: Section 3.5.1 was changed to read Presumptive testing of visible, apparent blood stains will be conducted by examiners in the Forensic Biology Unit (FBU) at the direction of the bloodstain pattern analyst, and the results may be detailed in the Forensic Biology Report and/or summarized in the Authorized by Spence
bloodstain pattern analysis report. Revision: Section 3.5.2 was changed to read Presumptive testing for blood will be performed using the current Leucomalachite Green (LMG) testing procedure of the Forensic Biology Unit. Revision: Section 3.6.1 was changed to read Sampling of stains of interest will be conducted by examiners in the forensic biology unit at the direction of the bloodstain pattern analyst. In the event that additional serological and/or DNA testing is needed, examiners of the FBU may sample additional stains at their discretion. Reference to the Leucomalachite green (LMG) testing procedures used by the FBU were removed. Revisions: In Appendix 1, Terminology for bloodstain pattern analysis, compression transfer pattern was changed to contact transfer pattern. The definition for forward spatter was corrected to say blood which travels in the same direction Deletions: The Evidence Photography, Presumptive Testing for Blood, and the Worksheet for Blood Spatter Measurement appendices were removed. Revision: Revisions of page numbers. Addition: In Appendix 1, Terminology for bloodstain pattern analysis, The definitions Wet Applied Bloodstain and Soak-through bloodstain were added.
Introduction
This document describes the policies and procedures that apply to the analysis and interpretation of bloodstain pattern evidence as performed at the Southwestern Institute of Forensic Sciences (SWIFS). The geometric patterns of bloodstains produced during a violent event are large part due to two factors: the nature of the events that caused the dispersal of the blood, and the physical characteristics of the surface on which the blood was deposited. As a result, knowledge of the pattern and distribution of bloodstains associated with a crime scene can be used to reconstruct details of the events that occurred at that scene. This is the goal of Bloodstain Pattern Analysis (BPA). This manual reflects the standard operating protocol for the identification, collection, analysis, documentation and interpretation of bloodstain evidence at SWIFS. The variety of evidence materials that may be subjected to BPA is great, and may depending on the case include intact crime scenes, vehicles, objects, and items of clothing. Because at this time most of the items submitted to SWIFS for BPA consist of clothing items, the emphasis in this document will be on this sort of evidence material. However, the underlying principles of analysis may be applied more broadly as specific case requirements dictate. 2 2.1 Applicable Policies Organizational policies 2.1.1 Within the organizational structure of SWIFS, bloodstain pattern analysis (BPA) is performed as a subdiscipline of the Trace Evidence Unit (TEU) within the Physical Evidence Section (PES). Analysts performing BPA are not restricted to members of the TEU, but may include qualified staff from other units.
2.1.2
2.2
Qualifications of analysts 2.2.1 Prior to performing BPA at SWIFS, an analyst must successfully complete an approved basic course in bloodstain pattern analysis, which is to include a competency test. Approved courses will satisfy the basic course requirements of the International Association of Bloodstain Pattern Analysts (IAPBA). Analysts performing BPA at SWIFS must complete a technical proficiency test, either internal or external, once per year.
2.2.2
2.3
Conduct of analysis 2.3.1 2.3.2 Conduct of BPA casework will be performed in accordance with all applicable requirements of SWIFS=s Quality Management Program and the policies of the PES. All procedures performed as part of the BPA of an item will be conducted in such a manner as to avoid unnecessary modification of the bloodstain pattern, so as to permit reanalysis at a latter date. Any modifications made to the bloodstain pattern, such as the sampling of portions of the pattern for serological and DNA testing, are to be clearly indicated in the bench notes and in photographs.
2.3.2.1
2.3.3 2.3.4 2.3.5
All analytical results and observations will be documented in the form of worksheets, photographs and drawings. All conclusions regarding bloodstain patterns must be supported by sufficiently detailed analytic results and observations. Items of evidence submitted for BPA will be initially examined by an analyst to determine their suitability for BPA. Suitability of an item for BPA will judged on the basis of criteria such as the character of the substrate, and the presence of a sufficient number and character of stains that test positive for blood using a presumptive chemical test. In the event that an item is judged to be unsuitable for BPA, the item will be transferred to the Forensic Biology Unit (FBU) for routine evidence screening and sampling, if requested. In the event that an item is judged to be suitable for BPA, further screening for BPA will be performed by the bloodstain pattern analyst. Collection of bloodstains and presumptive testing of bloodstains will be performed by qualified staff of the Forensic Biology Unit (FBU).
2.3.5.1
2.3.5.2
2.3.6
In addition to items of physical evidence, BPA may include ancillary materials such as reports of autopsy findings, serology reports, DNA reports, crime scene photographs, witness statements, etc. The use of these materials are to be clearly indicated in the supporting case documentation.
2.4
Reports 2.4.1 The results of BPA will be communicated to the investigating agency in the form of a written report whose format and content conform to the general policies of the PES regarding reports. The original BPA report will be maintained in the official PES case file, together with complete supporting documentation in the form of photographs, worksheets, and
2.4.2
other documentation of analytical results that justify the conclusions of the analyst. 2.4.3 Prior to release of the finalized report, each report and supporting case file will be technically and administratively reviewed. The technical review of the report and case file will be conducted by a second examiner qualified in BPA. The technical review will be conducted to assure that the analysis has been accurately performed, that the documentation of the analytical results in the case file is complete and accurate, that the reported conclusions are fully justified by analytical results, and that the report is clearly and accurately written. The administrative review of the report and case file will be conducted by another trained BPA analyst. The administrative review will be conducted to assure that the report and case file comply with all applicable Institute and PES policies, and that the report is clearly and accurately written.
2.4.3.1 2.4.3.2
2.4.3.3 2.4.3.4
3 3.1
Procedures Initial screening of evidence 3.1.1 3.1.2 Items of evidence submitted for BPA will be assigned to a BPA analyst for initial visual screening to determine the suitability of the item for detailed BPA. In the event that the item is judged unsuitable for BPA, it may be submitted to the Forensic Biology Unit (FBU) for routine screening, if requested. A BPA report will be produced stating that the item was not analyzed, and giving the reasons for this.
3.1.2.1 3.1.3
In the event that the item is judged suitable for BPA, analysis will be conducted in accordance with the described procedures.
3.2
Detection of bloodstain evidence 3.2.1 All examinations of evidence items for the presence of bloodstain evidence will be done so as to avoid unnecessary modification of the evidence, with a view to maintaining the original condition of the evidence for later reanalysis. Items of evidence will be examined visually to determine the presence of apparent bloodstain evidence. Gross macroscopic examination will be done visually using appropriate lighting.
3.2.2 3.2.3
Macroscopic examination may be performed with the assistance of low-power magnifying lens. 3.2.4 As appropriate, macroscopic examination may be supplemented by microscopic examination using a binocular dissecting microscope with appropriate illumination.
3.3
Photographic documentation 3.3.1 The condition and appearance of significant bloodstain pattern(s) used for interpretation may be documented photographically, using a digital camera or film camera. Photographic documentation may consist of either hardcopies of digital color images, or standard color photographs. Photographs may be annotated as a guide to specific pattern features. Specific areas and stains that are subjected to presumptive blood testing and sampling for species and DNA typing will be documented by the examiner performing the testing. The documentation will be either through diagrams, notes, or photographic documentation.
3.3.2 3.3.3 3.3.4
3.4
Data collection on bloodstain patterns. 3.4.1 3.4.2 Basic bloodstain patterns will be described using the terminology in Appendix 1, which is an adaptation of IABPA-recommended terminology. Measurements of the size of blood stains will be made using appropriate metric measuring devices. Direct measurement of stains on evidence items may be made using metric rulers, divided into 1 mm increments. For small stains (less than 2 cm), magnifying devices with integrated measuring reticules may be used for direct measurement. Measurements of stains from photographs may be made only when the photograph includes a scale. For rulers laid out in units of 1 mm, measurements will be made to the nearest 0.2 mm. For devices laid out in units of 0.1 mm, measurements will be made to the nearest 0.1 mm.
3.4.2.1
3.4.2.2 3.4.3
Measurements will be made to an acceptable degree of precision.
3.4.3.1 3.4.3.2 3.4.4
Measurement of the size of stains will be an essential element of the case
documentation whenever interpretations are to be made regarding the categorization of spatter as originating from low, medium or high velocity impact events; or the angle of impact of spatter is to be calculated. 3.4.5 Whenever measurements are made of the size of blood stains, the stains should be clearly indicated and identified on photographs.
3.5
Presumptive testing for blood 3.5.1 Presumptive testing of visible, apparent blood stains will be conducted by examiners in the Forensic Biology Unit (FBU) at the direction of the bloodstain pattern analyst, and the results may be detailed in the Forensic Biology Report and/or summarized in the bloodstain pattern analysis report. Presumptive testing for blood will be performed using the current Leucomalachite Green (LMG) testing procedure of the Forensic Biology Unit.
3.5.2
3.6
Sampling of blood stains for further analysis 3.6.1 Sampling of stains of interest will be conducted by examiners in the forensic biology unit at the direction of the bloodstain pattern analyst. In the event that additional serological and/or DNA testing is needed, examiners of the FBU may sample additional stains at their discretion.
3.7
Data Analysis 3.7.1 Angle of impact of a stain will be calculated using the following formula:
Impact Angle = arcsin
Width Length
3.7.2
The point of convergence (POC) of a blood spatter pattern consisting of multiple stains will be established by projecting the long axis of well-defined bloodstains back to a common point or area. The point of origin (PO) of a blood spatter stain on a surface will be determined using the following formula:
Z = d tan
3.7.3
where Z is the elevation of point of origin from the surface, d is the distance of the stain
Dallas County Institute of Forensic Sciences Forensic Laboratory Procedures for Bloodstain Pattern Analysis, Version 1.1 Page 8 of 15
from the point of convergence of the pattern on the surface, and is the impact angle of the stain. 4 4.1 Report writing The results of BPA will be communicated in the form of a written report that describes the analysis in a concise, well-organized manner that is technically accurate and intelligible to the non-scientist reader. In general, 4.1.1 4.1.2 4.1.3 4.2 4.3 The report is to reflect the objective, unbiased opinion of the examiner regarding the evidence submitted. The opinions expressed in the report should be limited to the area of BPA. All opinions expressed in the report are to be adequately supported by factual observations and numerical data.
The report will conform to current report format policies of the PES. The major divisions of the report will consist of the Addressee and Case Information block, the Evidence Listing, the Results section, the Conclusions section and the Disposition of Evidence section. 4.3.1 The Evidence listing will enumerate all items of physical evidence examined. It will also include all ancillary documents and materials examined, such as medical examiner=s reports, autopsy photographs, serology and DNA reports, photographs of crime scenes, etc. The Results section of the report will concisely describe the observations made that form the foundation for the analyst=s conclusions. When multiple items/materials are part of the analysis, the results for each item should be detailed independently. For each item examined, the report should detail both the type of examination performed (e.g., visual examination, microscopic examination, chemical testing, etc.) Experiments conducted to address specific questions are to be detailed. Statements of conclusions will be clearly and concisely worded. All conclusions must be substantiated by information included in the body of the report. Where a range of interpretations of the data are possible, these should be clearly stated.
4.3.2 4.3.3 4.3.4 4.3.5 4.4 4.4.1 4.4.2 4.4.3 4.5
The Conclusions section will summarize the critical findings of the analysis.
The report should avoid the use of words and phrases that are excessively definitive or
excessively inconclusive. 4.6 Reports should avoid the use of language that implies a degree of probability for events that can not be supported empirically (e.g., words such as likely, more likely, probably, etc.) The Conclusions section may, when appropriate, include a disclaimer to the effect that the conclusions are based only upon the described information, and in the event that the conclusions may require modification if additional probative information becomes available. Case File Documentation All case records, including administrative and analytical documentation, relevant to a particular case will be maintained in the official case file. The case record will contain adequate information so that another competent BPA examiner can independently evaluate and interpret the data. 5.2.1 Components of the case record for BPA will include references to procedures used, handwritten notes, worksheets, photographs, drawings, records of case related conversations, evidence submittal and chain of custody documents, correspondence, peer review forms and other pertinent records. All pages of the case record will be identified with the analyst=s initials and the case FL#.
4.7
5 5.1 5.2
5.2.2
Appendix 1. Terminology for bloodstain pattern analysis Adapted with modification from: 1) Stuart H. James. Scientific and Legal Applications of Bloodstain Pattern Interpretation. CRC Press. 1999; 2) Herbert L. MacDonell. Bloodstain Patterns. Laboratory of Forensic Science. 1997.
Accompanying drop. A small droplet that forms between a larger drop and its blood source when the larger drop breaks away and falls free. Angle of impact. The acute or internal angle formed between the direction of a blood drop and the plane of the surface it strikes. Arterial spurting (or gushing) pattern. Bloodstain patterns resulting from blood exiting the body under pressure from a breached artery. Back spatter. Blood directed back toward the source of energy or force that caused the spatter. Back spatter is often associated with gunshot wounds of entrance. Blood. The fluid and its suspended formed elements that are circulated through the heart, arteries, capillaries and veins. Bloodstain. The resulting transfer when liquid blood has come into contact with a surface or when a moist or wet surface comes into contact with dried blood. Bubble rings. Rings in blood that result when blood containing air bubbles dries and retains the circular configuration of the bubbles as a dried outline. Cast-off pattern. A bloodstain pattern created when blood is released or thrown from a bloodbearing object in motion. Clot. A gelatinous mass formed as a result of a complex mechanism involving red blood cells, fibrinogen, platelets, and other clotting factors. Over time, the blood clot retracts, resulting in a clear separation of the mass from the more fluid, yellowish blood serum which remains at the periphery of the stain. (See serum stain.) Contact transfer pattern. A contact bloodstain pattern created when a wet, bloody surface contacts a second surface with minimal lateral motion. A recognizable mirror image, or at least a recognizable portion of the original surface, is transferred to the second surface. Directionality. The orientation of a bloodstain or pattern which indicates the direction the blood was traveling when it impacted the target surface. Directionality of the flight of a blood drop can usually be established from the geometric shape of its bloodstain. Directionality angle. The angle between the long axis of a bloodstain and a predetermined line on the plane of the target surface which represents 0o.
Direction of flight. The trajectory, or flight directionality, of a blood drop which can be established by its angle of impact and directionality angle. Drawback effect. The presence of blood in the barrel of a firearm that has been drawn backward into the muzzle. Drip pattern. A bloodstain pattern that results from blood dripping into blood. Drop. A volume of blood of sufficient weight to overcome its surface tension and fall free from the mass of blood from which it was formed; typically a volume of 0.05 ml. Droplet. A blood drop volume less than the typical volume of 0.05 ml that was produced by energy exceeding that of gravitational attraction alone. Expirated or exhaled blood. Blood that is blown out of the nose, mouth, or a wound as a result of air pressure and/or airflow, which is the propelling force. Flight path. The path of the blood drop as it moves through space from the impact site to the target. Flow pattern. A change in the shape and direction of a wet bloodstain due to the influence of gravity or movement of an object. Forward spatter. Blood which travels in the same direction as the source of energy or force causing the spatter. Forward spatter is often associated with gunshot wounds of exit. High-velocity impact spatter. A bloodstain pattern caused by an impact/force of approximately 100 ft/sec or greater such as that produced by a gunshot or high-speed machinery. It must be emphasized that blood does not spatter at the same velocity as the velocity of the wounding agent. This pattern is characterized by a mist-like dispersion which, due to the high surface area of small droplets, can only travel a short horizontal distance in its flight. The preponderance of individual spots of blood produced by these mist-like droplets are usually less than 1 mm in diameter, although some larger spots are also always produced. Impact pattern. Bloodstain pattern created when blood receives a blow or force resulting in the random disperson of smaller drops of blood. Impact site. The point on a bloody object or body which receives a blow. Often, impact site is used interchangeably with point of origin. Impact site may also refer to an area on the surface of a target which is struck by blood in motion. Low-velocity impact spatter. Bloodstains produced on a surface when the blood source has been subjected to a low-velocity force approximately 5 ft/sec or less to a blood source. Medium-velocity impact spatter. Bloodstains produced on a surface when the blood source has been subjected to a impact/force between approximately 5 and 25 ft/sec. A beating typically causes this type of spatter. The preponderance of individual spots of blood produced in this manner are usually 1-3 mm in diameter, but larger and smaller spots also occur.
Misting. Blood which has been reduced to a fine spray as the result of the energy or force applied to it. Parent drop. A drop of blood from which a wave castoff or satellite spatter originates. Passive drop. A drop of blood produced by the action of gravity on liquid blood, as is produced during bleeding from a wound. Pattern. A form, shape or outline that is recognized. If comprised of small spots there must be an adequate number to be classified as a pattern. Perimeter stain. A bloodstain that is comprised only of its peripheral outline. This stain forms when the central area has been removed by wiping after the blood has partially dried, or by its center flaking off after it has completely dried. Also referred to as a skeletonized bloodstain. Point or area of convergence. A point or area to which a bloodstain pattern can be projected on a two-dimensional surface. This point is determined by tracing the long axis of well-defined bloodstains within the pattern back to a common point or area. Point or area of origin. The point or volume in three-dimensional space from which the blood that produced a bloodstain pattern originated. This is determined by projecting angles of impact of well-defined bloodstains back to an axis constructed through the point or area of convergence. Projected blood pattern. A pattern created when blood is projected or released as the result of force. Ricochet or secondary splash. The deflection of large volumes of blood after impact with a target surface that results in staining of a second surface. Ricochet does not occur when small drops of blood strike a surface. Satellite spatter. Small droplets of blood that are projected around or beside a drop of blood upon impact with a surface. A wave castoff is also considered a form of satellite spatter. Scallop pattern. A bloodstain produced by a single drop which is characterized by a wavelike, scalloped edge. Serum stain. A clear, yellowish stain with a shiny surface often appearing around a bloodstain after the blood has retracted due to clotting. This separation is affected by temperature, humidity, substrate, and/or air movement. Skeletonized bloodstain. A bloodstain that consists only of its outer periphery, the central area having been removed by wiping after liquid blood has partially dried. A skeletonized bloodstain is also produced by the flaking away of the central portion of a completely dried stain. Also referred to as a perimeter bloodstain. Smear. A relatively large volume of blood, usually 0.5 ml or more, that has been distorted to such a degree that further classification is not possible. A smear is similar to a smudge, but a smear is a stain produced by a larger volume of blood.
Smudge. A bloodstain that has been distorted to such a degree that further classification is not possible. Soak-through bloodstain. A bloodstain that soaks through an object such as a piece of fabric. Spatter. The dispersion of small blood droplets due to the forceful projection of blood. Spine. The pointed edge characteristics that radiate away from the center of a bloodstain. Their formation depends upon impact velocity and surface texture. Splash. A bloodstain pattern created by a low-velocity impact upon a quantity of blood approximately 1.0 ml or greater striking a surface. Surface tension. The physical property of a liquid that its surface resists separation, due to molecular attractions within the surface layer. The formation of drops and droplets of blood from a mass of blood requires energy to overcome the surface tension of the blood. Swipe. The transfer of blood onto a surface not already contaminated with blood. One edge is usually feathered, which may indicate the direction of travel. Target. A surface upon which blood has been deposited. Terminal velocity. The maximum speed to which a free-falling drop of blood can accelerate in air, which is approximately 25 ft/sec. Transfer pattern. A contact bloodstain created when a wet, bloody surface contacts a second surface as the result of compression or lateral movement. A recognizable mirror image or at least a recognizable portion of the original surface may be transferred to the second surface. Viscosity. The internal friction within a liquid which is characterized as the resistance to changing the form of the liquid. Void or shadow. Absence of bloodstain in an otherwise continuous bloodstain pattern. Often the geometry of the void will suggest an outline of the object which has intercepted the blood, such as a shoe, furniture, person, etc. Wave castoff. A small blood droplet that originates from a parent drop of blood due to the wavelike action of the liquid in conjunction with striking a surface at an angle less than 90o. Wet Applied Bloodstain, A bloodstain that exhibits characteristics of a wet droplet of blood contacting a surface. Wipe. A bloodstain pattern created when an object moves through an existing bloodstain removing blood from the original stain and altering its appearance.
Appendix 2. Summary of interrelationships of forces acting upon a source of blood (from S.H. James, Scientific and Legal Applications of Bloodstain Pattern Interpretation. CRC Press. 1999.)
Fire Debris and Ignitable Liquid Procedure Manual, Version 1.2
Fire Debris & Ignitable Liquid Procedure Manual, Version 1.2 Page 1 of 36
Revisions & Corrections Trace Evidence Unit - Fire Debris and Ignitable Liquid Procedure Manual, Version 1.2
Effective Date 1/22/08
Description Changes from Version 1.0 to Version 1.1: Revision: Revision of wording throughout the document to clarify the procedure Revision: All references to the ASTM Method 138795 were changed to ASTM Method 1618-06 Revision: The classification scheme (and all references to ignitable liquid classes) was changed and added as Appendix 3 to reflect the classification scheme in ASTM Method 1618-06 Deletion: Since the purge and trap attachment to the GC/MS is no longer in use, the alternate method section was removed Correction: The 0.05 % volume sensitivity resolution check mix was changed to the correct 0.005 % volume in numerous locations Revision: Since the GC/MS is not always used on a monthly basis, the requirement to run the sensitivity check was changed to semi-annually or monthly as casework dictates Revision: Previously omitted items including carbon strips were added to the Equipment and Materials list. Revision: The Restek E1387 and E1618 test mix solutions were added as Critical Reagents Revision: The un-extracted DFLEX or carbon strip will no longer be frozen and stored, but will be returned to the investigating agency along with the item of evidence. The extracted DFLEX or carbon strip will be discarded once the analysis is complete Deletion: The reference to Retention Time locking of Decane was removed from the QA/QC section Revision: Changes to the Ignitable Liquid Worksheet include removal of the storage column, different abbreviations and removal of GC/MS parameters. A line was added to record the solvent Lot #. Revision: Instrument methods were moved to Appendix 4.
Authorized by Spence
Addition: The previously omitted blank method was added to Appendix 4. Additions/Revisions: Abbreviations were added/revised in the Abbreviations section Addition: The Data Analysis section was added to clarify the methods used for data analysis. Addition: The book Fire Debris Analysis was added to the Recommended Reading section Addition: Appendix 5 Archival of Digital Instrument Data and Sequence Files was added Subsequent changes tracked on Trace Procedures Collection, Corrections & Revisions Log.
I.
Introduction Examinations for ignitable liquids may provide probative evidence of the presence of an ignitable liquid in scene debris, clothing of suspect or victim or scene evidence using instrumental analysis. These techniques are well documented and are fully accepted in the forensic science community
II.
Abbreviations GC/MS DFLEX CS2 TIC + / Pos - / Neg ignliq/IGNLIQ Nap/par Isopar Resck/Reschk/Rescheck LPD MPD HPD Gas Chromatography/Mass spectrometry Diffusive Liquid Extraction Carbon Disulfide Total Ion Chromatogram Positive Negative Ignitable Liquid Naphthenic / Paraffinic product Isoparaffinc product Resolution check mixture (ASTM E1387 or ASTM E1618) Petroleum distillate light range Petroleum distillate medium range Petroleum distillate heavy range
III.
Equipment, Materials, Critical Reagents, and Reference Ignitable Liquids Samples A. 1. 2. 3. 4. 5. Equipment and Materials Gas chromatograph and mass spectrometer (GC/MS) Helium (Grade 5.0) Carbon Disulfide (CS2) Reagent grade or higher Methanol Reagent grade or higher DFLEX (Diffuse Liquid Extraction) or Activated Carbon Strips from Albrayco Technologies, Inc. 6. Lined cans with lids 7. Rubber mallet 8. Screwdriver 9. Glass pipets 10. Pipet bulbs 11. Glass vials with Teflon septum caps 12. Auto sampler vials with Teflon septum caps 13. Scalpel blades 14. Auto sampler limited volume vial inserts 15. Crimper tool 16. Vent hood

17. Oven 18. Kapak bags 19. Nylon arson bags 20. Glass jars with screw cap lids B. Critical Reagents 1. Restek E1387 Column Resolution Check Mix (2000g/mL) 2. Restek E1618 Test Mix (0.5 g/mL or 0.05% volume/volume each) C. Reference Ignitable Liquid Samples
Certified ignitable liquid reference samples are not required. A reference collection of ignitable liquids should be available for comparisons. These samples can be obtained from commercial and retail sources. Examples of reference ignitable liquids may include but are not limited to: Gasoline (unweathered and in various stages of weathering) Mineral Spirits (unweathered and in various stages of weathering) Some cigarette lighter fluids Some specialty solvents Automotive parts cleaners Some insecticide vehicles Blended products Single component products Kerosene (unweathered and in various stages of weathering) Lamp oils Some camping fuels Some paint thinners Xylenes Laquer thinners Jet fuels Toluene-based products Diesel fuel (unweathered and in various stages of weathering) Turpentine products Some charcoal starters Paint and varnish removers Specialty cleaning solvents Industrial solvents Aviation gas Fuel additives
IV.
Sample & Reference Ignitable Liquid Requirements The identification of ignitable liquids is dependant on the analysts ability to recognize patterns of ignitable liquids in a Total Ion Chromatogram (TIC) as well as to identify significant compounds contained within the TIC. A reference collection of ignitable liquids is crucial to being able to identify samples. The samples from the reference collection of ignitable liquids should be analyzed by GC/MS. The GC/MS data from the ignitable liquid reference collection may be kept in a folder on the GC/MS computer. Also, the ignitable liquid reference sample data may be printed and retained in a binder of reference samples. A Mass Spectral Database Library, such as the NIST 98, may be used for comparison and identification of individual compounds. A laboratory produced database library can also be utilized. Certified ignitable liquid reference samples are not required for ignitable liquid identification.
V.
Safety Care must be taken to prevent injury from exploding cans. If enough pressure has developed inside a can, the lids can pop off with tremendous force; therefore, cans with bulging lids should only be opened inside the vent hood with the sash down as far as possible. Adequate ventilation should be utilized when working with any chemicals, especially carbon disulfide. Appropriate personal protective equipment (PPE) shall be worn while preparing samples for analysis.
VI.
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 as described in ASTM E1618. For specific operating instructions, refer to the instrumentation manuals. An acceptable sensitivity range is 0.005 volume percent in CS2 (10:1 dilution of the E1618 Test Mix). Before each sequence of casework samples is run, an autotune is performed. Refer to Gas Chromatography / Mass Spectrometry Analysis / Training Procedure Manual. A sequence begins with at least one blank carbon disulfide injection (blank method) followed by a Resolution Check Mix (E1387 or E1618) being analyzed on an ignitable liquid method. A blank solvent sample is then analyzed after the Resolution Check Mix sample. Between each case sample, a blank sample is analyzed to insure no carryover has occurred. The blank and ignitable liquid methods utilized in fire debris analysis are located in Appendix 4. The 0.005 % volume/volume (0.05 microliters/milliliter) Test mixture solution is run semi-annually or on a monthly basis as casework dictates.
VII.
Procedure 1. 2. Evidence is received and inventoried. Document the containers and conditions of the evidence seals on the Ignitable Liquid worksheet (Refer to Appendix # 1). If the material (non-liquid) to be tested is not already in a sealed lined can, glass jar, Kapak, or nylon arson bag, place the material in a suitable sealed container as soon as possible. Document any repackaging of evidence on the Ignitable Liquid Worksheet. Open each container. Notate a brief description of the contents and any obvious ignitable liquid odor. Add a DFLEX (diffusive liquid extraction) carbon strip or hang an individual carbon strip inside each container. Reseal the container as quickly as possible. Place the DFLEX identification sticker (if applicable) on the side of the container and record the DFLEX serial number on the Ignitable Liquid worksheet. Notate the time and date of the insertion of the DFLEX / carbon strip on the Ignitable Liquid Worksheet. Heat the container overnight (~16 hours) in a 60oC oven.
3.
4.

5. 6. 7. 8. 9. 10. 11. Allow the container to cool slowly in the oven. On the Ignitable Liquid Worksheet, document the time and date that the heating cycle is completed. Once the container has completely cooled, open the can and remove the DFLEX / carbon strip. Reseal the evidence container. Cut the DFLEX / carbon strip in half using a clean scalpel blade and place each half in separately labeled glass vials. Add carbon disulfide to one vial. Add enough carbon disulfide to cover the DFLEX / carbon strip. Make sure the vial is tightly capped. Allow the carbon disulfide vial to sit at least 30 minutes before analyzing. Prepare auto sampler vials by adding the FL#, item #, and initials with indelible ink. Insert a vial insert into the auto sampler vial. Pipette the sample extract into the vial insert. Cap the vial. Repeat for each sample. If the case sample is in a liquid form and you are unsure of the sample suitability for GS/MS analysis, first check its solubility in carbon disulfide by adding 1-2 drops of the unknown liquid to approximately 0.5 mL of carbon disulfide. If the sample is soluble in carbon disulfide, dilute the sample to an appropriate concentration, typically 1:100 for neat samples, and fill an auto sampler vial/ insert with the sample/solvent mixture and continue with the procedure. If the analyst has reason to suspect the sample is a water mixture with a portion being soluble in carbon disulfide, then the carbon disulfide extract can be separated from the aqueous layer and analyzed by GC/MS. The aqueous layer or an insoluble sample should not be analyzed by GC/MS. Run a sequence on the GC/MS. The order of the sequence shall include one or more solvent blanks, a Resolution Check Mix (reschk), solvent blank, case sample. Solvent blank samples will be run before each case sample to insure that there is no carryover from the previous sample. At least one reschk solution will be run per sequence batch. Run each case sample using one of the ignitable liquid methods (Appendix 4). Seal the glass vial containing the un-extracted portion of the DFLEX / carbon strip in a heat sealed pouch and return to the submitting agency with the evidence. The un-extracted portion of the DFLEX strip is assigned a sub-exhibit item number and documented on the chain-of-custody form. The extracted DFLEX / carbon strip is not retained.
12.
13. 14.
NOTE: Kapak and Nylon arson bags are acceptable containers for fire debris. The same extraction procedure is used as with cans. A small incision is made at the top of the bag. After the DFLEX / carbon strip is inserted into the bag, the opening is then heat sealed closed. The same is done once the DFLEX / carbon strip is removed.
VIII. Increased Sensitivity Method If the analyst believes the sample is so dilute that it cannot be adequately detected by the ignitable liquid (ignliq.m) method, an ignitable liquid method with increased sensitivity can be utilized. These methods operate at lower split ratios or split-less injection settings allowing more analyte to be injected onto the column. Increased sample volume is
Dallas County Institute of Forensic Sciences Forensic Laboratory Fire Debris & Ignitable Liquid Procedure Manual, Version 1.2 Page 7 of 36

another possibility to aid in increasing sensitivity but should be used cautiously. Too much sample and/or analyte can overload the column. Sample volumes in excess of 2 l should be used cautiously, as column overloading may result. Any changes in sample volumes should be noted in the bench notes. IX. Data Analysis Classification of ignitable liquids is done using one or more of the following techniques: pattern recognition, extracted ion profiling, single compound identification and target compound analysis. Pattern Recognition Compare TIC(s) of questioned sample(s) to TIC(s) of reference ignitable liquid samples. Comparison of TICs may be performed using software overlay methods or direct overlay of printed TICs. Extracted Ion Profiling (Mass Chromatography) Extracted Ion Profiling (EIP) is performed by comparing EIPs from questioned samples and reference samples. The TIC and EIP profiles for a sample may be obtained by running a macro program (arion2.mac, Appendix # 2) on each non-negative questioned sample. This macro includes a printout of the TIC and extracted ion profiles (EIPs). These profiles are: alkane profile (57, 71, 85, 99), aromatic profile (91, 105, 119), cycloparaffin profile (55, 69, 83) and naphthalene profile (128, 142, 156). Compare the printed TIC and EIP profiles from questioned samples and reference samples by direct comparison. Single Compound Identification Select relevant peaks from a TIC or EIP to search in the Mass Spectral Database Library (NIST 98) or in-house reference collection to identify the compound. If a compound cannot be identified through the use of the NIST 98 or in-house reference collection, additional reference samples may be analyzed as needed. If a suitable comparison sample cannot be located, then the sample cannot be confirmed. Target Compound Analysis (TCA) Target compound analysis uses key specific compounds to characterize an ignitable liquid. Target compound lists for common ignitable liquids may be found in tables 3-5 in ASTM E1618. While target compounds provide much useful information, a TCA should not be the sole basis for the identification of an ignitable liquid residue. Also, not all target compounds listed in tables 3-5 in ASTM E1618 are present in all ignitable liquids of the same class. IX. Quality Assurance & Quality Control The autotune is checked for any evidence of leaks or other instrumental problems. Refer to the Gas Chromatography / Mass Spectrometry Procedure Manual for autotune parameters and corrective actions.
A Resolution Check Mix containing a known mixture of hydrocarbons (E1387 or E1618) is run with every sequence of case samples. The dilution for the E1387 resck mix is 20:1 in CS2. A 10:1 dilution of the Sensitivity resck mixture (E1618 Test Mix) is also analyzed (0.005 % volume/volume) semi-annually or on a monthly basis as casework dictates. The Sensitivity resck sample should be run for each month that case samples are analyzed. Log the preparation of the resck mixtures into the Standard/Reagent logbook. Indicate in the logbook whether or not the resck samples performed as expected. The resck samples do not need to be prepared fresh daily. The compounds specified in ASTM E1618 section 6.4 for the test mixture should be resolved and identified in an accepted resolution check mix. If any of the compounds cannot be resolved or identified, the analyst should check the system for leaks, remake the resolution check mix, and/or perform any other maintenance necessary. The data from 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 casework 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 described in the GC/MS Procedure Manual. A suitable solvent blank should exist prior to samples being analyzed. Any maintenance should be recorded in the GC/MS logbook. X. Notes The notes should reflect a description of the material being tested, date and time(s) of DFLEX / carbon strip insertion, heating and results. In addition to the Ignitable Liquid Worksheet (Appendix # 1), bench notes may also be documented in other formats. The type of matrix/material being tested may be important when interpreting the spectra. Make note of any apparent odors of ignitable liquids but do not rely on them entirely. XI. Report and Reporting Guidelines The attached ignitable liquid classification system from the ASTM Method E1618-06 (Appendix # 3) is used to classify any ignitable liquid detected in a sample. In reporting results, give a class name and range (light, medium, or heavy), as well as examples of that class for positive results. A comparable chromatogram from the reference collection should be included with case notes. When no ignitable liquid is detected, possible reasons should be included on the report. These reasons could include no ignitable liquid having been used, the ignitable liquid having been consumed in the fire, or the ignitable liquid having been washed away during firefighting efforts. The analyst will print out the mass spectra for compounds specifically identified and relied upon for the identification of an ignitable liquid from the Total Ion Chromatogram (TIC). These mass spectra will document the identification of specific peaks relied upon for the interpretation of results. The identification of ignitable liquids is based on pattern

matching against known reference materials and/or identification of specific compounds within a pattern. The use of a target compound checklist is one tool that may be utilized. Lists of target compounds can be found in ASTM E1618. XII. Continuing Education For continuing development as an ignitable liquid examiner, each scientist will be required to complete at least one annual proficiency test. The examiner should also peer review casework for/by other examiners, stay current with forensic literature, and seek to attend outside courses/seminars involving ignitable liquid examination. XIII. Recommended Reading 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. 412423. Chemical Markers in Weathered Gasoline, Ronald Coulombe, Journal of Forensic Sciences, 40(5), September 1995, pp. 867-872. Turpentine in Arson Analysis, Michael Trimpe, Journal of Forensic Sciences, 36(4), July 1991, pp. 1059-1073. 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. 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. FBI Laboratory Analysis of Fire Debris Evidence course book. National Forensic Science Training Center, Advanced Fire Debris Analysis Course student and reference manuals. Fire Debris Analysis, Stauffer, Dolan, and Newman, Elsevier, 2008.

Appendix # 1
IGNITABLE LIQUID WORKSHEET

FL # __________________ Solvent _______ Solvent Lot #____________ Received from ___________________ on ___________ Analyst _______________ Resolution Check Mix Lot # __________ Agency # ________________________________ Date __________________ Item # Container Description of Contents DFLEX in DFLEX # Heating - 60 C GC/MS Results
GC/MS: HP 6890/5973 Abbreviations: CS2 - Carbon Disulfide Ignliq - Ignitable Liquid
Appendix # 2: Arion2 Macro

Appendix 3: Ignitable Liquid Classification Chart from ASTM E1618-06 CLASS
Gasoline all brands, including gasohol Petroleum Distillates (including De-Aromatized)
LIGHT (C4-C9)
Petroleum Ether Some Cigarette Lighter Fluids Some Camping Fuels Aviation Gas Some Specialty Solvents Some Paint and Varnish Removers Some Automotive Parts Cleaners Xylenes, Toluene-based products Cyclohexane based Solvents/Products Solvents Pentane, Hexane, Heptane Alcohols, Ketones Some Lacquer Thinners Fuel Additives Surface Preparation Solvents
MEDIUM (C8-C13)
Fresh gasoline is typically in the range C4-C12 Some Charcoal Starters Some Paint Thinners Some Dry Cleaning Solvents Some Charcoal Starters Some Paint Thinners Some Copier Toners Some Automotive Parts Cleaners Specialty Cleaning Solvents Some Insecticide Vehicles Fuel Additives Some Charcoal Starters Some Insecticide Vehicles Some Lamp Oils Some Candle Oils Some Copier Toners Some Lacquer Thinners Some Industrial Solvents Metal Cleaners/Gloss Removers
HEAVY (C8-C20)
Kerosene Diesel Fuel Some Jet Fuels Some Charcoal Starters Some Commercial Specialty Solvents Some Insecticide Vehicles Industrial Cleaning Solvents
Isoparaffinic Products
Aromatic Products
Naphthenic-Paraffinic Products Normal-alkanes Products
Some Insecticide Vehicles Some Lamp Oils Industrial Solvents Some Candle Oils Carbonless Forms Some Copier Toners
Oxygenated Solvents
Appendix 4: Ignitable Liquid Methods
Appendix 5: Archiving of Digital Instrument Data and Sequence Files

The HP 6890/5973 GC/MS instrument stores analysis data in the following data path: C:\HPCHEM\1\DATA\(current folder)\. Additionally, the instrument stores the sequence file in the following path: C:\HPCHEM\1\SEQUENCE\(current sequence file). When the analysis and review of a complete casework analysis data set and sequence file have been completed, the data set and sequence file will be uploaded to the Dallas County server on a monthly basis as casework dictates. If no casework is performed in a particular month then no data archival is required.
Gunshot Residue and Range Determination Procedure, Version 1.2
GSR & Range Determination Procedure, Version 1.2 Page 1 of 18
Revisions & Corrections Gunshot Residue and Range Determination Procedure Manual, Version 1.2 Effective Date 1/22/08 Description Changes from Version 1.1. to Version 1.2 Revision: Revision of Section II to delete Certified ACS grade requirements. Revision: Revision of Section III to delete measurements for 15% acetic acid and 5% hydrochloric acid solutions. Revision: Revision of Section V to clarify safety concerns. Revision: Revision of Section VI to add abbreviations. Revision: Revision of Section VIII to clarify storage of processed photographic paper sheets. Revision: Revision of Section IX to clarify storage of nitrite swabs. Revision: Change of Section X, XI, XII to clarify the testing processes and safety procedures and to reduce documentation required on pressouts and their storage envelopes. Revision: Change of Sections X, XI, XII, XIII, XIV, and XVII to allow for release of pressouts with evidence to investigating agency. Revision: Revision of Section XV to clarify documentation required on evidence items, to delete requirement for photographs, and to clarify wording in reference to ammunition for test firings. Revision: Revision to Section XVII to clarify when sodium rhodizonate solution should be prepared. Addition: Addition of updated Gunshot Residue, Test Firings, Shotgun Test Firings, and other worksheets. Deletion: Deletion of outdated Gunshot Residue and Test Firings Worksheets. Deletion: Deletion of references (moved to Gunshot Residue and Range Determination Training Manual). Revision: Revisions of page numbers. Authorized by Spence
I.
Introduction This manual is not intended to serve as a textbook, nor is it intended to be a substitute for the proper training that is the prerequisite for conducting gunshot residue (GSR) examinations. GSR examiners following this procedure should have received the proper training and passed all necessary competency tests required to perform the examinations covered by this manual. The analyst shall follow the Institute of Forensic Sciences= procedures regarding analyses requested, casework documentation, collection, security and preservation of the evidence and report format. The forensic examination of clothing and other objects for gunshot residue uses visual, microscopic and chemical techniques in an effort to provide an estimated range of fire (muzzle to object distance). These techniques are well documented and are fully accepted in the forensic science community.
II.
Equipment, Materials & Reagents Stereomicroscope, vent hood, ruler, spray bottles, glacial acetic acid, desensitized photographic paper, iron, cheesecloth, cotton swabs, sulfanilic acid, alpha naphthol, sodium nitrite, sodium bitartrate, tartaric acid, rhodizonic acid (sodium salt), concentrated (12 M) hydrochloric acid, methanol, 100% ethanol, dithiooxamide, concentrated ammonium hydroxide, potassium chloride, muslin and miscellaneous fabric squares, Benchkote paper and pencil.
III.
Preparation of Chemical Solutions Numerous chemical reagents are used in the analysis of gunshot residue. Below are the recipes for making up the various solutions required. All chemicals should be handled with caution and all chemical safety procedures should be followed. 1. 15% Acetic Acid - Dilute the glacial acetic acid to a 15% solution using deionized water. Store in an uncontaminated, sealed glass container. Sodium Rhodizonate Solution - Partially fill a small plastic spray bottle with deionized water. Add a small amount of rhodizonic acid to saturate the solution to approximately the color of strong tea. Make enough of the solution for immediate use. Do NOT store the solution.
2.

3. Bitartrate Buffer - Dissolve 9.5 grams of sodium bitartrate and 7.5 grams of tartaric acid in 500 mL of deionized water. Store in an uncontaminated and sealed glass container. 5% Hydrochloric Acid - Dilute the concentrated (12M) hydrochloric acid to a 5% solution using deionized water. Care should be taken to insure proper ventilation is maintained. Store the solution in a clean, sealed container. 0.2% Dithiooxamide (DTO) solution - Dissolve 0.2 grams of dithiooxamide in 100 mL of 100% ethanol. Store this solution in a tightly sealed container to prevent the evaporation of the ethanol. 50% Ammonium Hydroxide - Dilute 50 mL of concentrated ammonium hydroxide with 50 mL of deionized water. Always use concentrated ammonium hydroxide in a well ventilated hood. Store the solution in a tightly sealed container. Potassium Chloride Buffer - Prepare a 0.2M potassium chloride solution (KCL) solution by dissolving 0.75 grams of KCL in 50 mL of deionized water. Next, prepare a 0.2M hydrochloric acid (HCL) solution by diluting 5.0 mL of concentrated HCL (12M) in 295 mL of deionized water. Combine 25 mL of 0.2M KCL with 67 mL of 0.2M HCL to make a buffer with pH 1.0. Store the solution in a tightly sealed container.
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Sample & Standard Requirements The ability to identify gunpowder is dependent on the examiners ability to identify numerous types of burned and unburned gunpowder particles. Comparative samples of gunpowder knowns are useful for reference and review. Also, known distance patterns from varying firearms can also be used for comparative and instructive purposes. A lead source (i.e. lead bullet core) is needed to test the reactive capability of the sodium rhodizonate solution. Nitrite test swabs are used to test the sensitivity and reactiveness of the treated photographic paper. A copper jacketed bullet can serve as a standard for the dithiooxamide test. Knowledge of basic firearms terminology and functionality is another requirement.

V. Safety
Gunshot residue examinations can employ chemicals and reagents that are known carcinogens and hazardous substances. Appropriate personal protective equipment (PPE) should be worn to reduce the risk of exposure to blood borne pathogens. Examples are masks, gloves, lab coat, plastic apron, face shields and/or safety glasses. The examiner should be familiar with basic firearms safety. VI. Abbreviations BD - bullet defect BS - bloodstain(s) BW - bullet wipe compl - complainant ent. entrance FB or FBU Forensic Biology Unit FMJ full metal jacket GR - "grease ring" GSR Gunshot Residue GSW - gunshot wound JHP jacketed hollow point L left LW - lead wipe LR long rifle LRN lead round nose MG or mod griess - Modified Griess N/A or NA - No analysis or not applicable VII. Training Before an analyst can begin independent forensic examination of gunshot residue evidence, a thorough training program must be completed. Refer to the Gunshot Residue and Range Determination Training Manual for a detailed outline. VIII. Processing of Desensitized Photographic Paper 1. 2. 3. Make a solution of 1.5g of sulfanilic acid in 300 mL of distilled water. Make a solution of 0.84g of alpha-naphthol in 300 mL of methanol. Combine both solutions and pour into a non-reactive tray. Dip individual sheets of desensitized photographic paper (previously desensitized) into the solution until well coated. Remove each sheet and allow to dry. Place the sheets in an appropriate container, such as a manila envelope or other suitable container and store until ready for use.
NaRh - Sodium Rhodizonate P or PP - gunpowder particle(s) PPP Gunpowder particle pattern Pb - Lead pwdr powder R - right S - soot s/n or sn - serial number SGW - shotgun wound SRT sodium rhodizonate test Vis. Visible VL - vaporous lead w/ - with w/o - without WTB - white Tyvek bag + Positive -/ - Negative
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Preparation of Nitrite Swabs 1. 2. Make a solution of 0.6 grams of sodium nitrite in 100 mL of distilled water. Soak cotton-tipped swabs in the solution. Set the swabs aside to dry and then store in a foil-covered container.
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Modified Griess Test 1. Test the four corners of the treated photographic paper using a nitrite test swab soaked in 15% acetic acid. An orange colored reaction indicates the paper is sensitive and reactive. Positive test corners may be cut off at the examiners discretion; this step is not required. Record these QC results on the worksheet. Mark each test paper with the FL#, item #, date, and examiner=s initials. Place your sample, questioned side down, onto the photographic paper. Notate on the paper any defects or other distinguishing features for future reference. Soak a piece of clean cheesecloth in a beaker of 15% acetic acid and wring it out. Place it over the questioned area (underside). Press the cheesecloth/sample/photographic paper Asandwich@ with an iron set on a cotton setting. Separate the Asandwich@ and notate any nitrite reactions (orange colored) on the GSR worksheet (Appendix 1). On occasion the fabric will react and form an orange pattern on the photographic paper. A positive nitrite reaction will be in the form of dots or a dense halo close to the hole. Allow the photographic paper to dry. Place the dry pressouts in a new manila envelope. Label the envelope as containing GSR pressouts, and mark the envelope with the FL #, item #, date, and examiners initials. Seal the envelope and initial the seal. After packaging, the envelope should then be documented on a chain of custody and released to the appropriate agency. If a lifting method is warranted, spray the 15 % acetic acid onto an appropriately sized piece of Benchkote paper. Press the Benchkote paper onto the questioned area. Remove the Benchkote paper and continue with the procedure, using the Benchkote paper as the questioned item. All chemicals and procedures using chemical solutions should be handled wearing appropriate personal protective equipment and following SWIFS Health
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and Safety Procedures. XI. Reverse Modified Griess Test 1. 2. Attach a piece of filter paper to the back of a sheet of treated photographic paper. Test the four corners of the photographic paper as described in the Modified Griess test. Mark each test paper with the FL #, item #, date, examiner=s initials, and defect identification (such as Hole A). Wipe the emulsion side of the photographic paper with a piece of cheesecloth soaked in 15% acetic acid. Place the photographic paper on the questioned surface with the acetic acid coated emulsion (shiny) side down. Notate on the paper the location of any defects or distinguishing features for future reference. Apply an iron set on a cotton setting to the filter paper attached to the photographic paper. Separate the layers and notate any findings on the GSR worksheet. Allow the photographic paper to dry. Place the dry pressouts in a new manila envelope. Label the envelope as containing GSR pressouts, and mark the envelope with the FL #, item #, date, and examiners. Seal the envelope and initial the seal. After packaging, the envelope should then be documented on a chain of custody and released to the appropriate agency.
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9. All chemicals and procedures using chemical solutions should be handled wearing appropriate personal protective equipment and following SWIFS Health and Safety Procedures.
XII.
Sodium Rhodizonate Test 1. Using a lead bullet core, mark a piece of cloth, paper, or paper towel. Using a plastic spray bottle, spray the area with 15 % acetic acid and treat the area using the procedure below to check for reactiveness of the sodium rhodizonate solution. Record these QC results on the worksheet. Using a plastic spray bottle, coat the area surrounding the defect (which should still be damp with acetic acid from the Modified Griess test) with the sodium rhodizonate solution.
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3. Spray the same area with a bitartrate buffer solution. Lead and a few other metals which may be present will turn a pink color. Follow the buffer solution with a coating of 5% hydrochloric acid. If the pink color turns a blue-violet color, then lead is indicated. Record findings on the GSR worksheet. If a pattern is not readily visible (i.e. dark colored material, heavy blood deposition), blot the area surrounding the defect with an appropriately cut piece of Benchkote paper to transfer a positive reaction. Allow the Benchkote paper to dry. Mark each test paper with the FL#, item #, date, examiner=s initials, defect identification. Document the reaction pattern (as the color will fade with time) on the GSR Worksheet. Place the dry pressouts in a new manila envelope. Label the envelope as containing GSR pressouts, and mark the envelope with the FL #, item #, date, and examiners initials. After packaging, the envelope should then be documented on a chain of custody and released to the appropriate agency. All chemicals and procedures using chemical solutions should be handled wearing appropriate personal protective equipment and following SWIFS Health and Safety Procedures.
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XIII. Dithiooxamide Test The Dithiooxamide Test (DTO) is used independently and/or in conjunction with other tests in range determination. The DTO test utilizes a color chemistry reaction to indicate the presence of copper. The DTO test reacts with copper to produce a dark greenish-gray to nearly black color reaction. It should be noted that the DTO test will also react with cobalt, leaving an amber color reaction and nickel, leaving a violet color reaction. In the event the examiner feels the circumstances are warranted, the DTO test can be performed along with the Sodium Rhodizonate and Modified Griess Tests. NOTE: The order of the test performed is crucial as well as the use of a potassium chloride buffer instead of a bitartrate buffer during the Sodium Rhodizonate Test. The order is as follows: 1st - Modified Griess 2nd - Dithiooxamide 3rd - Sodium Rhodizonate (using KCL buffer) 1. Using a copper jacketed bullet, mark a piece of cloth or paper towel. Using a plastic spray bottle, spray the area with 15 % acetic acid and then treat the area using the procedure below to check for the reactivity of the DTO solution. Record these QC results on the worksheet. Saturate the questioned area with 50% ammonium hydroxide using a spray bottle. Allow the item to sit for one minute.
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With another spray bottle filled with 0.2% DTO solution, saturate the area. A green color, ranging from forest green to army green/gray is a positive reaction for the presence of copper. The color may develop immediately or may require approximately five minutes to develop. Allow the item to air dry for five minutes before proceeding to the next test. If the Sodium Rhodizonate Test is to be performed, follow the same procedure but use the KCL buffer instead of the bitartrate buffer. If a lifting method is warranted, spray the 50% ammonium hydroxide solution onto an appropriately sized piece of Benchkote paper. Press the Benchkote paper onto the questioned area. Remove the Benchkote paper and continue with the procedure, using the Benchkote paper as the questioned item. Allow the Benchkote paper to dry. Mark each test paper with the FL#, item #, date, and examiner=s initials. Place the dry pressouts in a new manila envelope. Label the envelope as containing GSR pressouts, and mark the envelope with the FL #, item #, date, and examiners. Seal the envelope and initial the seal. After packaging, the envelope should then be documented on a chain of custody and released to the appropriate agency.
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8. All chemicals and procedures using chemical solutions should be handled wearing appropriate personal protective equipment and following SWIFS Health and Safety Procedures. XIV. Shotgun Related Evidence 1. Process item(s) as mentioned above with the exception that the Modified Griess Test is not necessary unless a close range of fire is suspected. Make notations of the diameter of the central defect and/or pellet hole pattern. A circular grid is useful. Also, examine the area visually and microscopically for the presence of filler material and gunpowder particles especially if a close range is suspected. Spray the area with 15% Acetic Acid and then perform the Sodium Rhodizonate Test. Record findings on the Gunshot Residue Worksheet (Appendix 1). Record findings of shotgun test firings on the Shotgun Test Firings Worksheet (Appendix 3). When performing test firings for comparison, use blotter board or similar material. Properly package the pressouts and/or test firing (as stated in previous
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sections), label the packaging as containing pressouts and/or test firings, and mark the envelope with the FL #, item #, date, and examiners initials. Seal the package and initial the seals. After packaging, the package/envelope should then be documented on a chain of custody and released to the appropriate agency. XV. Procedures for Gunshot Residue Examinations 1. Inventory articles in item. Label articles with FL#, item #, and examiners initials. Evaluate which articles have defects or possible areas of gunshot residue and document findings. Notate any visible soot, gunpowder particles or other residue. Microscopically search area surrounding defect or area of suspected residue for soot, gunpowder particles or other residue. Chemically test suspect area for nitrites (Modified Griess Test). Chemically test suspect area for lead (Sodium Rhodizonate Test). Notate all residue detected. Photographs may be taken of any distinctive nitrite or lead residue patterns, but are not required. If requested and an associated firearm is available, consult with the Firearms Unit to have the firearm test fired using evidence ammunition or similar ammunition from laboratory stock. Using muslin cloth squares or similar material, discharge the weapon at varying distances in an attempt to duplicate the residue pattern found on the evidence item or determine at what distance the weapon and ammunition stop depositing residue on the target. Analyze the test cloths microscopically and chemically using the same procedure as used for the article in the submitted item and notate findings on the Gunshot Residue Test Firings Worksheet (Appendix 2). Compare gunshot residue patterns from test cloths to gunshot residue patterns from the submitted item. Summarize conclusions and make report.
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XVI. Additional Procedures

Dallas County Institute of Forensic Sciences Forensic Laboratory GSR & Range Determination Procedure, Version 1.2 Page 10 of 18
For materials that are thick or non-porous, the Reverse Modified Griess Test can be used to analyze for nitrite residue. If a dark colored article, an immovable object, a heavy blood soaked area or non-porous object is to be tested, the analyst can use a Alifting@ method for the Sodium Rhodizonate Test. A similar Alifting@ method can be used for the Modified Griess Test and DTO Test (see below) where the Alift@ is treated as the questioned material. Lifting method 1. Prepare a piece of Benchkote paper to fit the area to be tested plus a surrounding portion as a blank. If the questioned area is hydrophobic, moisten the Benchkote paper with 15 % acetic acid solution and then spray the test area on the object with the 15 % acetic acid solution. Immediately press the moistened Benchkote paper on to the object and Ablot@. Remove the Benchkote paper and spray the paper with sodium rhodizonate solution, bitartrate buffer and then with 5% HCl.
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XVII. Quality Assurance & Quality Control Careful documentation of defects and residue detected can be crucial for later comparisons and review. The sodium rhodizonate solution should be made fresh daily, as needed for casework, and tested its reactivity using a scratch test with a lead bullet core. A similar scratch test can be used to test the quality of the DTO test reagents using a copper jacketed bullet. The nitrite test swabs are soaked in 15% acetic acid and then swiped across the four corners of each treated photographic paper immediately prior to its use. Any test firing cloths, Modified Griess test papers, positive Benchkote paper or transfer sheets will be packaged, sealed and initialed, and labeled with the FL #, analysts initials and date. They will then be documented on a chain of custody and released to the appropriate agency. XVIII. Notes The examiner should take detailed notes on the questioned article(s), the visual and microscopic findings and the chemical analyses. The chemical results are especially important since the color reaction for the presence of lead will fade, sometimes very quickly. When test firings are made, make sure the pertinent weapon and ammunition information (from evidence or laboratory stock) is recorded. The location of defects and residue detected will be important. XIX. Reporting
Dallas County Institute of Forensic Sciences Forensic Laboratory GSR & Range Determination Procedure, Version 1.2 Page 11 of 18
The written report should accurately reflect the items examined, the basic procedures used in the examination, and the conclusions reached as a result of the analysis. The conclusions reached must be supported by information available in the notes. XX. Continuing Education
For continuing development as a gunshot residue 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 gunshot residue examination.

Appendix 1

Appendix 2

Appendix 3

Appendix 4

Appendix 5

Appendix 6
Glass Analysis Protocol, Version 1.1
Dallas County Institute of Forensic Sciences Forensic Laboratory Page 1 of 22
Revisions & Corrections Glass Analysis Protocol, Version 1.1 Effective Date 1/22/08 Description Changes from Version 1.0 to Version 1.1: Change: The changes made by memo to the Quality Assurance/Quality Control Section on August 7, 2002, were incorporated into the current version of this protocol. Deletion: The Thermometer with 0.1C resolution was removed from the Tools/Equipment section. Revision: Item 1 under Analysis/Examination was reworded to clarify that control glass from the incident should be collected from all sources of broken glass when feasible. Note: The collection of control glass from the crime scene is out of the control of the laboratory. Revison: Section 4 SAFETY to clarify safety concerns. Revision: Appendix 4 to include additional worksheets to be used for bench notes. Addition: Section 8, QUALITY ASSURANCE/QUALITY CONTROL, subsection 2, Peer Review, The following wording was added: When additional glass examiners in the Trace Evidence Unit are trained and qualified, peer review will be performed in-house. Deletion: Appendix 2: Density Comparison Sink/Float Method, subsection 3, the wording Document the size and shape of all glass particles being used for density comparison for future identification, was deleted. Revision: Appendix 3: Refractive Index Determination - Monochromatic Light and Temperature Control, number 14, a typographical error (lot # C 01 1958) was corrected to read (lot # C 04 1958). Deletion: The Bibliography section was removed. Revision: Revision of page numbers. Authorized by Spence

1. OBJECTIVE / INTRODUCTION This manual is not intended to serve as a textbook, nor is it intended to be a substitute for the proper training that is the prerequisite for conducting glass examinations. Glass examiners following this procedure should have received the proper training and passed all necessary competency tests required to perform the examinations covered by this manual. The analyst shall follow the Institute of Forensic Sciences= procedures regarding analyses requested, casework documentation, collection, security and preservation of the evidence and report format. The presence of glass fragments on clothing corresponding to glass from a known source is frequently accepted in the courts as important evidence to link a suspect with a broken glass object. Glass breakage may occur as a result of a forced entry burglary, a hit-and-run accident, or an assault where a bottle is used as a weapon. The following glass analysis procedures are recommended guidelines for the examination of physical evidence for the transfer of glass fragments, the recovery of glass fragments, and the subsequent comparison with possible sources of said glass. 2. TRAINING A new glass examiner should complete training on all aspects of this glass analysis protocol to the satisfaction of the section supervisor. A general listing of the steps involved in training are: 1. Completion of a basic microscopy course, taught either in-house or as a class taught by outside laboratory microscopy consultants. This instruction or course should include basic theory and application of microscopes and microscopic methods of examination. In-house training should be given by an experienced forensic glass examiner who shall monitor the progress of the trainee and report to the supervisor on a regular basis. Completion of the training program includes: a. b. c. Trainees will be familiar with select glass analysis articles. Practical training in recovery and analysis of glass fragments. Instrumental accuracy attained by the trainees shall be assessed through practice samples. Glass recovery rates can be measured using Adoping@ of clothing exhibits. The number of practice samples worked will be decided jointly by the
Glass Analysis Protocol, Version 1.1 Page 3 of 22
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trainee, instructor and the supervisor. d. Period of co-signed/second opinion casework with an experienced examiner. The length of this time frame will be determined by the Supervisor. Completion of written tests, projects, and/or mock trials.
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3. TOOLS/EQUIPMENT 1. Tools/Supplies G G G G G G G 2. Tools for trace evidence (See General Trace Evidence) Slides and cover slips compatible with a Mettler Hot Stage Brushing implements Refractive index liquids (Cargille 1.50 and 1.53) Glass refractive index standards Density liquids (Bromoform and Chloroform) Jacketed glass water column
Equipment G G G G G G Ultraviolet light source (254 nm) Stereomicroscope Polarizing compound microscope Phase contrast microscope Filters (486 nm, 589 nm, and 656 nm) for the phase contrast microscope light source Mettler hot stage and controller
4. SAFETY Glass examinations can employ chemicals that are known carcinogens and hazardous substances. Therefore, the examiner should follow the Dallas County Institute of Forensic Sciences Environmental Health and Safety Manual. All chemicals and chemical solutions should be properly labeled and worked with under a vented hood. All examiners should have knowledge of blood-borne pathogens and the risks involved in routine casework. Appropriate personal protective equipment (PPE) should be worn while processing evidence for glass analysis. Additionally, the Mettler hot stage is capable of temperatures of 300C; therefore, care should be taken to avoid burns.
5. ANALYSIS/EXAMINATION 1. Glass from the incident (hereafter referred to as control glass) should be collected from all sources of broken glass when feasible. Sufficient control glass should be included to be representative of the source. Contact requesting agency/detective as needed (See General Trace Evidence). Questions Specific to glass analysis: G G G G How many glass sources were broken? Were they single or multiple-pane windows? Where was the control glass recovered from? Was the inside/outside surface of the control glass marked? How much time elapsed between the incident occurring and the collection of the physical evidence?
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Appropriate general methods of collection and preservation of recovered trace evidence (See General Trace Evidence). Visual examination, presumptive testing, and microscopic examination of clothing (See General Clothing Examination). Recovery of glass fragments is usually achieved by hand-picking or brush-down/shakedown (See General Clothing Examination). When examining shoes, collecting evidence separately from soles, uppers and inners, is recommended because different significance may be attributed to the glass fragments recovered from each location. Prior to repackaging each item, the packaging itself should be examined and any debris removed to a labeled, sealable container. Any removed debris is searched with a low-power microscope and suspected glass fragments are removed. A glass fragment is identified as such by its conchoidal fracture, amorphous structure, and isotropism. Testing sorts out particles that may be confused with glass: a. b. Plastic can be eliminated by testing for indentation with a needle point. Most mineral grains (such as quartz or sand) can be identified by observations in polarized light. Under the microscope, using crossed polarized light, the particle (stage) is rotated; glass and isotropic minerals remain dark, whereas other
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crystals, which are called birefringent or anisotropic, refract light in more than one direction and Alight up@ during the rotation. c. Minerals (such as table salt, garnet, fluorite and diamond) can be distinguished from glass by their respective physical and microscopic characteristics.
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Control glass and recovered glass needing a detailed comparison should be subjected to the following minimum characterization and comparisons, where applicable: a. b. c. d. e. Thickness. Color. Fluorescence when irradiated by short wave ultraviolet light (254 nm). General degree of transparency. Matching of fracture contours - (See Appendix 1). An excellent review of this topic, as well as glass analysis in general, exists in Forensic Science Handbook, Chapter 4: Forensic Glass Comparisons by Elmer T. Miller. f. g. h. Form - whether tempered, wired, patterned, etc. Surface material - such as dust, paint, adhering fibers, etc. Density - (See Appendix 2). Glass density measurement is done by a comparative sink/float method as outlined in Forensic Science Handbook Chapter 4, Forensic Glass Comparisons Elmer T. Miller. Differences of 0.00005 g/cc or less may be observed using this method. Since variation across a glass product may exceed 0.00005 g/cc, a false rejection of the actual source can result from sink/float comparison. i. Optical dispersion of refractive index - Monochromatic Light and Temperature Control - (See Appendix 3). The method involves using a phase contrast microscope equipped with a Mettler hot stage and wavelength filters for 486 nm, 589 nm, and 656 nm. An excellent

review of this topic, as well as glass analysis in general, exists in Forensic Science Handbook, Chapter 4: Forensic Glass Comparisons by Elmer T. Miller. The following further modifications are suggested: I. The performance of the instrument at the time of analysis is determined by measuring the optical dispersion of refractive index of a glass standard (i.e., a glass sample for which the manufacturer has provided refractive index data to at least five decimal places). Whenever possible, analysis of glass fragments should be made without prior washing treatment. If necessary, cleaning may be performed by a method such as using dilute sulfuric acid wash, followed by successive water and acetone or methanol washes. The refractive index at the surface of float glass can be different from the bulk. Bulk control glass and control glass from the float and non-float surfaces are obtained by marking the surfaces with two colors of ink, crushing the sample, and selecting only those fragments which are uninked as bulk and only those fragments which are appropriately inked as float and non-float surfaces. Glass fragments mounted in refractive index oil must be remounted if there is any reason to suspect that changes have occurred in the oil which may affect the refractive index measurements.
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6. NOTE-TAKING General guidelines for notes on trace evidence should be followed (See General Trace Evidence). Notes should include the reported source of submitted glass, the collection of glass fragments from clothing items, any sample treatment or preparation steps taken, results of visual and microscopic observations, and any data from optical dispersion of refractive index and density measurements. The worksheets in Appendix 4 as well as other suitable forms of documentation including photographs, sketches or other bench notes may be used for documentation. 7. PACKAGING General guidelines for packaging of trace evidence should be followed (See General Trace Evidence).
Dallas County Institute of Forensic Sciences Forensic Laboratory Page 7 of 22 Glass Analysis Protocol, Version 1.1

Return items in their original packaging. If this packaging is not secure, place in an appropriate sealable package. Seal and mark with initials, laboratory number, date and item number. Unmounted glass fragments and debris collected in the laboratory should be sealed in a secure package and labeled as to what item it was collected from, the laboratory number, initials, and date. 8. QUALITY ASSURANCE/QUALITY CONTROL 1. Proficiency Testing a. Each glass analyst will be required to examine at least one glass proficiency case per year. Records of each examiner=s results will be maintained by the quality control manager.
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Peer Review Inasmuch as only one examiner is fully trained and qualified to perform glass analysis at the Southwestern Institute of Forensic Sciences, the Department of Public Safety Laboratory in Garland has agreed to perform peer reviews on glass analysis cases. When additional glass examiners in the Trace Evidence Unit are trained and qualified, peer review will be performed in-house.
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Continuing Education For continuing development, the examiner should stay current with the forensic and manufacturing literature, peer review casework for/by other examiners, seek to attend outside courses/meetings involving glass analysis, tour local production facilities, and conduct independent projects.
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Contamination Refer to the General Trace Evidence and General Clothing Examination sections.
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Calibration The calibration of the Mettler Hot Stage is verified quarterly and at the time of analysis by using calibrated immersion oils and by analyzing glass standards whose refractive index is known to at least five decimal places. Appendix 3 details the procedure. The results of analysis of the standard glass samples are then compared against the known

refractive index values of the glass standards. Re-calibration of the Hot Stage may be required if the refractive indices of the known glass sample exceed 0.0004 Nc, 0.0002 Nd, 0.0004 Nf. If a re-calibration of the Hot Stage is required, follow the calibration procedure as outlined in the operating manual for the Mettler Hot Stage. It should be noted that the refractive index values for the known glass sample must fall within the allowed tolerances prior to performing any refractive index measurement on case samples. Should the calibration still fail to meet the listed tolerances for Nc, Nd, and Nf, the Hot Stage should be removed from service by placing an out of service notice on the instrument and by documentation in the Logbook. The instrument should then be serviced by a qualified technician and retested prior to being placed back into service. When the instrument is placed back into service, the instrument must be rechecked by performing the calibration check. When the instrument passes the quality control check, the instrument will be placed back into service by documentation in the Logbook. 9. REPORTS The written report should accurately reflect the items examined, the basic procedures used in the examination, and the conclusions reached as a result of the analysis. The conclusions reached must be supported by information available in the notes.
10. APPENDIX 1 Fracture Match and Sequence of Impact Significance: Broken glass at the scene of a burglary, traffic accident or other crime scene can sometimes be physically compared to pieces of glass recovered in the possession of a suspect. A fracture match between glass at a crime scene and glass from a suspect=s possession can make a positive association between the two. Also, when a glass surface such as a car windshield or an architectural window is struck by a number of solid objects such as by bullets or rocks, the fracture patterns developed in the glass can often be examined to determine the sequence of impacts and the direction of travel of the projectiles. This information can be used to reconstruct a sequence of events. Principle: Glass is amorphous and brittle, and is not stretched nor distorted by breakage, and it can be reconstructed to its original shape. Because it is amorphous, no two glass objects will break the same way. Further, the ridges and hackles formed on the broken edges of the glass can be examined to aid in determining the direction of force applied to a pane of glass. Also, the patterns of radial and concentric cracks developed on a pane of glass that has been subjected to a bullet impact can be examined to determine the sequence of bullet impacts. Procedure: 1. Examine the submitted glass object and determine if a sequence of impact analysis needs to be performed. If the glass object is suitable for a sequence of impact analysis, photograph or sketch the object. a. b. c. Label the inner and outer surfaces of the glass object. Macroscopically examine the patterns of radial and concentric cracks to determine the total number of impact points. Examine the radial cracks and determine the sequence of impacts by evaluating where the radial cracks end. (note: radial cracks will terminate at the intersection of a previously formed crack). Label the impact points as P1, P2, P3, etc.. P1 is the first impact, P2 is the second impact etc. (Label on the diagram or photographs)
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Examine the hackle marks on the radial and concentric cracks to determine the direction of force for each point of impact. [Note: Four R rule: Ridges on Radial cracks are at Right angles to the Rear (side opposite to impact)]. It is however, not always possible to determine the side from which glass is broken. Exceptions are: a. b. c. Tempered or toughened glass, because it Adices@ without forming ridges. Very small windows held tightly in a frame, because they cannot bend or bulge appreciably. Windows broken by heat or explosion, because there is no Apoint of impact@.
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Determine if any of the recovered glass particles are suitable for a mechanical fit comparison. Perform any mechanical fit analyses prior to performing any destructive examinations. A mechanical fit may preclude the necessity of performing any further analyses such as density and refractive index.

11. APPENDIX 2 Density Comparison - Sink/Float Method Significance: Density is a specific physical characteristic of glass specimens and can be used in differentiating specimens. This procedure determines variation in densities of large and small pieces of glass evidence. Principle: Density is a constant property for glass. The difference in density between two or more specimens is determined through the use of the sink/float method. The sink/float method involves mixing a solution of bromoform/chloroform in a water-jacketed glass tube. When the density of the solution exactly matches the density of a known specimen of glass, the glass sample will be suspended in the solution. When a questioned specimen of glass is compared to the known glass, any difference in densities will be noted by the sample sinking or floating in the solution.
Procedure: 1. Clean the glass particles as needed. Remove aluminum coatings from headlight reflector lenses using a dilute acid. Thoroughly dry samples. Crush a portion of the control glass in a pin mortar, select particles for density comparison which approximate the size and shape of one or more of the unknown-source particles. If appropriate, select samples from various parts of the known specimen to determine variation within the specimen. Using a water-jacketed density column, fill the column to approximately two inches using bromoform. (See Figure 1)
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Figure 1
4.
Allow the temperature of the bromoform and density column to equilibrate. Add one of the control (known-source) glass fragments to the bromoform (glass will float). Slowly add chloroform with frequent mixing to lower the density of the solution until the density of the solution matches that of the glass sample. Allow the solution of bromoform and chloroform to equilibrate with the glass sample. Additional bromoform or chloroform may have to be added dropwise to achieve the density match. The glass sample should be suspended near the middle of the solution at the equilibrium point. Insert the questioned-source glass sample into the bromoform/chloroform solution. Mix thoroughly and allow the solution to achieve thermal equilibrium with the glass samples. The control and questioned glass samples will be suspended at or near the same height in the column if their densities match. If the questioned sample is more dense, it will settle to the bottom. If the questioned sample is less dense, it will rise to the surface. (Caution: If the glass sample floats at the surface, make sure that it is not being held at the surface by the surface tension of the liquid solution).
5.
6.
7.
8.
9.

10. Document the results of the density determination on the glass examination worksheet.

12. APPENDIX 3 Refractive Index Determination - Monochromatic Light and Temperature Control Significance: Refractive indices are specific for individual glass specimens. This procedure determines the refractive indices of glass specimens at wavelengths of 656 nm, 589 nm and 486 nm. It can be used for large as well as small pieces of glass evidence. The technique is precise to +/- 0.0004 refractive index units at the Nc and Nf lines and to +/- 0.0002 refractive index units at the Nd line. Principle: Refractive index is a physical property of glass very sensitive to small changes in chemical composition. This property is determined by mounting a small sample of glass in a liquid of known refractive index, heating the sample and observing the disappearance of the Becke line while viewing the specimen in light of 656 nm, 589 nm and 486 nm. The temperature of Becke line disappearance is a function of the wavelength of light and refractive index. The refractive indices Nc, Nd and Nf for the glass samples are then extracted from data tables supplied with the Cargille Immersion Liquids.
Procedure: 1. Crush a portion of each sample into the appropriate sizes (~ 80 - 100 mesh) for refractive index determination using a pin mortar. (See Figure 2)
Figure 2
Dallas County Institute of Forensic Sciences Forensic Laboratory Page 15 of 22 Glass Analysis Protocol, Version 1.1
2.
Determine the appropriate immersion liquid for refractive index determination (Cargille 1.50 oil or Cargille 1.53 oil). Generally, headlamp glass will be immersed in 1.50 oil and all other glass samples will be immersed in 1.53 oil. The refractive index of the immersion oil should be slightly greater than the refractive index of the glass sample at ambient room temperature. Immerse glass particles in the immersion oil on a glass slide (~ 76 x 19 x 1mm), cover with cover glass (~ 18 x 18 x 0.17mm). Turn on the Microscope lamp to 10.5V or 12V. Adjust phase and illumination according to directions provided in the AO Series 20 Reference Manual, if needed. Turn on the Mettler Hot Stage. (Switch at right rear of main unit) Insert slide into the Mettler hot stage on the phase microscope. Focus on a bright edge of a glass fragment (10X objective), avoiding thick 90 edges or thin feathered edges. (Place the glass specimen at the center of the field of view in the microscope). Rotate the Nc (656, red) filter into position (position AA@, upper filter wheel) on the microscope. Set the starting temperature on the Mettler FP82HT Hot Stage to 35C and allow to equilibrate. Raise the temperature of the hot stage at a rate of 1C/min, observe the Becke line on the glass sample and record the temperature at which the Becke line disappears (match point, refractive index of glass = refractive index of oil). Rotate the Nd (589, yellow) filter into position (position AB@). Continue to raise the temperature at a rate of 1C/min.. Record the temperature of the match point. Rotate the Nf (486, blue) filter into position (position AC@). Continue to raise the temperature at a rate of 1C/min.. Record the temperature of the match point. Repeat Steps 9-11 at least three times and determine the match point temperature for each wavelength. Record each match point temperature into the Glass Analysis Worksheet (Appendix 4).
3.
4.
5. 6. 7.
8.
9.
10.
11.
12.
13.
Determine the refractive indices (Nc, Nd, Nf ) for each glass sample. The refractive indices can be determined directly from the refractive index data tables for the Cargille 1.50 and 1.53 immersion oils. (Refractive index data tables are corrected for the dN/dT correction factor for each oil as supplied on the Manufacturers data sheets). By repeating steps 2-13, perform a quality control check by determining the refractive indices of either the Cargille 1.49 glass (lot # B 04 1958) or the 1.52 glass (lot # C 04 1958) depending on which oil was used as the immersion liquid for the questioned samples. Compare the known refractive indices of the Cargille glass to the experimental values of the refractive indices. The actual refractive indices of the Cargille glass samples will be determined directly from the data sheets provided with the glass samples. All quality control data must be documented and retained with the case folder. Also, the quality control data must be documented in the log book for the Mettler hot stage and AO Series 20 phase microscope. The refractive indices of glass samples should have an error factor of: Nc and Nf of +/- 0.0002 and Nd +/- 0.0001 when comparing the same glass sample. Nc and Nf of +/- 0.0004 and Nd +/- 0.0002 when comparing two glass samples.
14.
15.

13. APPENDIX 4
Hair Procedures Manual, Version 1.1
Dallas County Institute of Forensic Sciences Trace Evidence Unit Page 1 of 23
Revisions & Corrections Hair Procedures Manual, Version 1.1 Effective Date 1/22/08 Description Changes from Version 1.0 to Version 1.1: Revision: Revision of the wording throughout the document to clarify the procedure. Deletion: Deletion of the Training section. Deletion: Deletion of Table of Contents Addition: Addition to Reagents and Supplies to include polarized light microscope, other suitable mounting medium, digital camera, microscope camera adapter, microfuge tubes lens cleaner, lens paper, two stage micrometers with 0.01mm divisions. Revision: Revision to Safety to clarify safety concerns. Addition: Addition of Equipment Calibration and Maintenance section Revision: Revision to Collection of Hair Evidence to clarify the collection process. Revision: Revision to Collection of Hair Evidence to delete reference to the General Trace Evidence Recovery Examination and Clothing Examination procedures. Revision: Revision of Hair Comparison Analysis to change documentation required on slides. Revision: Revision of Hair Comparison Analysis to delete the requirement of using Permount. Revision: Revision of Section Non-Comparative Examinations number 4, letter C, to add Catagen to the wording. Revision: The Reporting section was renamed Reporting Guidelines. Wording was included to detail the reporting guidelines. Deletion: Deletion of the Hair Examination Worksheet. Addition: Addition of new worksheets for hair analysis bench notes. Revision: Revisions of page numbers and section numbers. Authorized by Spence
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I. Principle: This manual is not intended to serve as a textbook, nor is it intended to be a substitute for proper training that is the prerequisite for conducting hair examinations. Hair examiners following this procedure should have received the proper training in microscopic hair comparison analysis and passed all necessary competency tests required to perform the examinations covered by this manual. The analyst shall follow the Institute of Forensic Sciences= procedures regarding analyses requested, casework documentation, collection, security and preservation of the evidence and report format. II. Introduction: The forensic examination of hair uses macroscopic and microscopic techniques as the primary methods of characterization and comparison of samples. These techniques are well documented and are fully accepted in the forensic science community. III. Scope: This procedure details the collection, preservation and comparison of hair evidence as it relates to casework. Prior to an analysis of evidentiary material, an initial assessment of the evidence and its relevance should be made. When case circumstances warrant a trace evidence analysis, items of interest should be processed prior to other examinations such as serology, fingerprints or firearms. This processing must be done in such a manner as to not compromise or contaminate the remaining evidence. IV. Reagents and Supplies: Microscopes Stereoscope Bright Field Incident or Reflected light Comparison Polarized light Micro tools for handling trace evidence (tweezers, dissecting needles, etc.) Slides, cover slips (various sizes) Mounting medium Xylene Permount Other suitable mounting media Polaroid black and white film coater Ruler
Dallas County Institute of Forensic Sciences Trace Evidence Unit Hair Procedures Manual, Version 1.1
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Evidence tape Fingernail polish Petri dishes Manila coin envelopes Sticky/Post-It style notes (various sizes) Scraper Fingerprint or equivalent tape for tapelifts Acetate sheets 8 2 x 11 Gloves Digital Camera Microscope Camera Adapter Microfuge tubes Lens cleaner Lens paper Stage micrometer with 0.01mm divisions Ocular with reticule
V.
Safety Appropriate personal protective equipment (PPE) shall be worn when processing hair evidence or while preparing microscope slides. Appropriate PPE includes wearing gloves and a lab coat or plastic apron when processing hair evidence or while preparing microscope slides. PPE is not required while performing microscopic examinations of microscope slides.
VI.
Equipment Calibration and Maintenance: 1. Maintenance
To assure the precision, reliability, and performance of microscopes, the following procedures for the maintenance of the microscopes should be performed on an as needed basis. A. Clean the optics of dust, oil, and dirt. Lens cleaner or alcohol on lens paper is sufficient to clean most optics. Never use Kimwipes, facial tissue, or other rough surfaced paper or cloth. Pressurized canisters of air may be used to remove dust. B. C. D. Clean the external surfaces. Check the optical alignment and realign if necessary to establish Khler illumination. Record all repairs and annual maintenance in the appropriate equipment
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logbook. If the microscope cannot be cleaned or aligned properly, call for service.
E. 2.
Calibration Check of the Ocular Scale Magnification of the comparison microscope should be checked periodically. Calibration of the ocular scale should be performed for each objective of each microscope so accurate measurements may be obtained. A. B. C. D. E. Adjust the microscope for Khler illumination. Place the stage micrometer on the microscope stage. Adjust the focus of the reticule eyepiece to focus on the eyepiece reticule lines. Using the lowest powered objective, focus on the stage scale and arrange the stage scale lines parallel with the lines of the ocular scale. Align one of the lines of the ocular scale with one of the stage scale lines. Then determine how many ocular scale divisions (osd) exactly equal some whole number of divisions on the stage scale, expressed in m. To make the comparison as accurate as possible, a large part of each scale must be used. Determine how many ocular scale divisions equal how many stage scale divisions (ssd). For example 38 osd = 600 m; therefore, 1 osd = 600 m/38 = 15.8 m. Repeat this process for each objective. Record the ocular stage scale calibration for each magnification in the logbook.
F. G.
H. I.
3.
Calibration Check of the Comparison Microscope Magnification of the comparison microscope should be checked periodically. Calibration of the microscope should be performed for each objective on each microscope to verify that the two sides of the microscope operate at equivalent magnifications. A. Once the magnification for each objective has been checked for each side of the comparison microscope, the two objectives of similar magnification should be checked against each other. Place a stage micrometer on each microscope stage. Adjust the focus of the reticule eyepiece to focus on the eyepiece reticule lines. Align the two stage scale micrometers such that they are in a vertical arrangement with respect to each other.
B. C. D.
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E. F. G. H. I. J. Using the lowest powered objective on each microscope, focus on the stage scales. Adjust the split screen prism so that both stage scales are visible simultaneously. Arrange the stage scale lines of one parallel with the lines of the other stage scale. The lines of one stage scale should align with the lines of the other stage scale. To make the comparison as accurate as possible, a large part of each scale must be used. The two stage scale micrometers should align without any noticeable differences. If noticeable differences are observed, arrange for the microscope to be adjusted by an appropriate microscope service provider. Repeat this process for each objective combination.
K.
VII.
Collection of Hair Evidence:
Preface: Hair evidence, including questioned and reference standards, should be collected and preserved in a manner that maximizes both hair comparisons and biological typing of root sheaths and other biological material. Appropriate methods for collection and preservation of trace evidence, including hair and fiber evidence, from evidence items submitted should be utilized. 1. Check out evidence from registrars according to accepted policies and procedures. Verify that the Forensic Laboratory Number (FL#) and each corresponding item number is correct and reflects those items submitted for hair examination on the submission sheet. Open the item packaging taking care not to destroy the integrity of previously sealed areas when possible. Precautions are taken to avoid biological contamination of the evidence. Appropriate personal protective equipment (PPE) should always be worn when examining items for hair evidence. Remove item from container and check for loose hairs in the container. Examine the item for hair evidence. Note the location where hairs are recovered from an item when feasible. Pictures, diagrams or notes may be taken to
2.
3.
4.
5. 6.
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document location of recovered hairs. 7. Trace evidence will be recovered by one or more of the following practices: physically picking the hair evidence off of the item using tweezers or a gloved hand, tape lifting the items and adhering the tape lift to acetate sheets, tape lifting onto sticky notes, shaking the item over white paper, or scraping the item over white paper. Sticky notes may be used to hold the hair evidence while it is stored in adequately labeled and sealed, coin envelopes, or suitable containers. When trace evidence such as hairs, fibers or other debris are collected from an exhibit, these sub-exhibits will be given sub-exhibit item numbers. Notes will include the FL#, analysts initials and date. The bench notes should also include a description of the evidence and evidence container(s) and condition of seals. The evidence container and evidence are marked by the examiner for future identification purposes. Where applicable, the FL#, date, item # and examiner=s initials are inscribed on the item away from areas such as blood or semen which may be useful in subsequent analyses. Return the item to the original container when possible and seal with evidence tape. Initial the tape seal. Repeat steps 3-12 for all examined items. Upon completion of analyses, return evidence to evidence registrars for release to agency or transfer to the appropriate lab section for subsequent analyses. Document the transfer of evidence including sub-exhibits on the chain of custody form. Any hair evidence not retained by the laboratory for further evaluation will be returned to the appropriate agency. Any hair evidence which will be retained by the laboratory for further evaluation will be stored by the analyst according to Institute policies.
8.
9.
10.
11.
12.
13. 14.
15.
16.
VIII. Hair Comparison Analysis
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Preface: The analysis of human hair involves the examination of the questioned and reference samples to determine macroscopic and microscopic characteristics. The questioned hairs may then be compared to the reference samples. Human head hair is only suitable for comparison with human head hair. Human pubic hair is only suitable for comparison with human pubic hair. The minimum length requirement for microscopic comparison analysis is 1 cm. Human hairs from somatic origins, other than the head or pubic region, are of limited value for microscopic comparison analysis. Any hair which is unsuitable for comparison analysis may be evaluated for its DNA potential, as determined by the examiner. Microscopes which should be available to the hair examiner include transmitted and incident light stereomicroscopes and comparison microscopes with magnification ranges of at least 100X - 400X and equipped with light polarization capabilities. 1. Prior to hair comparison analysis, adequate head and or pubic hair standards should be obtained from the complainant(s), suspects and any individual who may normally have deposited hairs in the questioned area, when possible. An adequate head hair standard consists of human head hair taken from the front, top, both sides, and back of the human scalp. These hairs should be full length with intact roots (pulled). An adequate pubic hair standard consists of hair from the pubic region above the sex organs and below the waist of humans. These hairs should also be full length with intact roots (pulled). Adequate hair standards generally include between 25 and 50 hairs pulled hairs with roots. In the absence of primary hair standards, secondary hair standards such as hairs from a victims hair brush may be temporarily substituted for comparison purposes during an investigation. Hair standards should be collected within five years of the time of the offense. Due to the potential changes in an individuals hair over time, hairs collected beyond five years may or may not be comparable to hairs shed previously. Extreme caution should be exercised when comparing hairs that exceed the five year time frame. If at any time the examiner determines that the hair/hairs are unsuitable for further examination/comparison, the analysis may be halted and a report may be issued documenting the work performed. Groups of hairs from a single exhibit which exhibit similar macroscopic characteristics may be sampled for a representative sample at the examiners discretion. Hairs selected for comparison/examination are chosen at the discretion of the examiner.
2.
3.
4.
5.
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6.
Hairs less than 1cm in length are not considered as suitable candidates for microscopic comparison. The questioned and reference hairs may be examined visually and/or with a stereo microscope. Some of the characteristics which may be noted during this examination are the presence of apparent blood, type of root and tip, length, reflected color, diameter variations, cosmetic treatments, and degree of curl, among other characteristics. The macroscopic and low power microscopic examinations may be used to exclude or include hairs for further microscopic examination. Hairs may be excluded for further microscopic comparison based on differences in color, racial origin, somatic origin and other gross macroscopic features. The questioned and reference hair(s) are mounted in a suitable mounting media on separate, properly labeled glass microscope slides. The slides are labeled with the FL#, item #, examiner=s initials and date. The number of hairs per slide will vary with the examiner=s experience and preference. The comparison must be thorough and careful using different magnifications to compare the microscopic characteristics. Macroscopic and microscopic examinations consist of a comparison between the questioned and reference hairs for internal structure and external characteristics. Some useful comparison characteristics are listed on the Hair Examination Worksheet (Appendix 2). Individual hairs on glass slides may be marked by marking the slide or coverslip with indelible ink to ensure easy identification of a single hair. Additionally, the individual slide may be photocopied, sketched, or photographed to aid in the documentation in the bench notes. The comparison analysis is conducted and the significant discriminatory features documented in the bench notes. The bench notes may include the use of any of the forms listed in Appendix 2 in addition to typewritten notes, photographs, sketches, photocopies or other forms of appropriate documentation. At the completion of the macroscopic and or microscopic examination/comparison of the hairs, the hairs should either be demounted from the microscope slides or the glass slides should be protected by packaging and sealing in slide mailers/containers that adequately protect the slides from breakage.
7.
8.
9.
10.
11.
12.
13.
14.
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IX.
Non-Comparative Examinations:
Preface: Hair evidence which is submitted to the laboratory without adequate reference standards for comparison can yield useful information. Common analyses that fall into this group are: human vs. animal, somatic origin, racial origin and possible DNA content. 1. Is the hair human or animal? A. Animal hairs are usually distinguished from human hairs in color, shape, medullation, cuticle structure, and the appearance of the root. The cuticle of the hair can be studied as a dry mount or a cast can be made using Polaroid film coater, clear fingernail polish, or lacquer. The cast is made by applying a thin film of the coater, polish or lacquer to a clean glass slide and pressing the hair specimen into the thin film before it dries. After the slide is dry, the hair is removed from the film and the cast is compared to reference animal hair casts. The examiner should use caution when identifying species of animal as many animal hairs have similar characteristics. The use of a reference collection is strongly recommended.
B.
2.
If human, is it head, pubic, beard or a body hair? A. Somatic origin determination of a questioned hair should be limited to head, pubic, beard or body. A body hair can be limb, chest, back or transition hairs. General Observations of length and shape along with some microscopic characteristics such as medullation, texture, taper, and tip may assist in determining somatic origin. In some instances, the determination of the somatic origin may not be possible; therefore, the somatic origin will be considered as undetermined.
B.
C.
3.
If human, what is the racial origin? A. Racial indicators of human hair are poorly defined and must be used with a great deal of caution. It should be stated that a hair exhibits certain racial characteristics. It should never be stated that a hair originated from a certain racial group. A hair classified as exhibiting Caucasian, Negroid, or Mongoloid racial characteristics should be
B.
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typical of hair within these racial groups. In some instances, the racial characteristics may not be clearly within a single racial group. Some hairs exhibit characteristics of more than one racial group. If the racial group is not clearly defined, the hair may be described as originating from an undetermined racial origin. C. The simplest of characteristics are the most useful in grouping hairs by race. These include color, longitudinal shape, cross-sectional shape and pigment granule distribution.
4.
If human, what about DNA? A. DNA from hairs comes in two forms, Mitochondrial DNA and Nuclear DNA. Depending on the presence or absence of a root and the type of root, the hair analyst may suggest the best approach at obtaining the most probative DNA evidence allowed by the questioned hair. For hair fragments measuring at least 1cm in length with no roots or hair with Telogen roots which have no sheath material, Mitochondrial DNA sequencing of the shaft may be suggested. For hair with Anagen roots or hair with Catagen or Telogen roots supplying ample sheath material, Nuclear DNA typing of the root may be suggested.
B.
C.
X.
References Standards: A collection of reference hair samples (human and lower animals) should be maintained. The reference hair collection may include human hairs of different races, somatic origin, chemical treatment, and physical damage. Animal hairs in the collection should at least represent the most common types of animals encountered in routine casework.
XI.
Conclusions: In order to conclude that a questioned hair is consistent in macroscopic and microscopic characteristics with a known hair sample from a particular person, it must first be determined that there are no forensically significant differences in these characteristics or their arrangements. Since no two hairs will ever be exactly the same in all minute details, it is important to determine what differences are significant. It must first be determined that the characteristics exhibited by the questioned hair fall within the range of characteristics presented in the known sample. After that, the ideal situation for the hair examiner is to find one or more hairs in the known sample that correspond in all respects (no significant differences) with the questioned hair. Depending on the characteristics
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involved and the circumstances surrounding the case, it may sometimes be possible to utilize several hairs from the known sample to locate characteristics that correspond to those of a questioned hair. However, the duplicate hair criterion for a match should be the ultimate goal. (Proceeding of International Symposium on Forensic Hair Comparisons).
XII.
Reporting Guidelines: The written report should accurately reflect the items examined, the basic procedures used in the examination, and the conclusions reached as a result of the analysis. The conclusions reached must be supported by information available in the notes.
1. Animal Hair Conclusions The genus or species of a questioned animal hair may be reported if the characteristics of the hair are distinctly typical of a certain genus or species of an animal. Otherwise, they should only be reported as an animal hair if identified as such. 2. Human Hair Conclusions A. If no significant differences are found, it can be stated that the questioned hair and the known hair sample exhibit the same microscopic characteristics and, accordingly, are consistent with originating from the same source. The questioned hair exhibits both similarities and differences to the known hair sample, and accordingly, no conclusion can be reached as to whether or not the questioned hair originated from the source of the known hair. The questioned hair is microscopically dissimilar to the known hair sample and, accordingly the questioned hair could not have originated from the source of the known hair sample. Other Conclusions: 1. The presence of an anagen root indicates that the hair was forcibly removed and should be reported when probative. The presence of individual characteristics should be reported when they may be important to an investigation.
B.
C.
D.
2.
E.
Disclaimers 1. A disclaimer accurately describing the limits of a particular conclusion

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will be reported whenever a positive association significant to the case is determined. A statement equivalent to the following is adequate: It is pointed out that the hairs do not possess a sufficient number of unique individual microscopic characteristics to be positively identified as having originated from a particular person to the exclusion of all others. 2. Some hairs will not exhibit sufficient microscopic characteristics upon which to base an association. These hairs would be categorized as unsuitable for comparison. When the time between the shedding of the questioned hair(s) and the collection of the known hair standards is (5) five years or more apart, any comparisons shall include the following disclaimer or equivalent in the examiners report. Due to the time span of five years or more between the shedding of the questioned hair(s) and the collection of the hair standard(s), the value of the hair comparison involving these hairs is limited to screening for DNA analysis and/or investigative leads.
3.
XIII. Continuing Education: For continuing development as a hair examiner, each scientist will be required to complete hair proficiency tests, peer review casework for/by other examiners, stay current with forensic literature, and seek to attend outside courses/seminars involving hair examination.
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Appendix 1: Recommended Reading
This is not an all inclusive list. 1. Saferstein, R. (Ed.), Forensic Science Handbook, Hall, Englewoods Cliff, New Jersey, 1982, pp. 184-221 (Bisbing, R. E., Chapter Author). Proceedings of International Symposium on Forensic Hair Comparisons, 1985, FBI Academy, Quantico, Virginia. Hicks, J. W. , AMicroscopy of Hair: A Practical Guide and Manual,@ Federal Bureau of Investigation Issue 2, Washington, DC, 1977. Kirk, Paul L., AHuman Hair Studies,@ Journal of Criminal Law and Criminology, Vol.31, 1940-1941, pp. 486-496. Petraco, N., Fraas, C., Callery, F. X., and De Forest, P. R., AThe Morphology and Evidential Significance of Human Hair Roots,@ Journal of Forensic Sciences, JFSCA, Vol. 33, No. 1, Jan. 1988, pp. 68-76. Linch, C. A., Smith, S. L., Prahlow, J. A., AEvaluation of the Human Hair Root for DNA Typing Subsequent to Microscopic Comparison,@ Journal of Forensic Sciences, JFSCA, Vol. 43, No. 2, 1984, pp. 305-314. Kirk, Paul L., (Thornton, J. I., Ed.), ACrime Investigation,@ Interscience Publishers, Inc., New York, New York, 1974, pp. 151-166. Gaudette, B. D. and Keeping, E. S., AAn Attempt at Determining Probabilities in Human Scalp Hair Comparison,@ Journal of Forensic Sciences, JFSCA, Vol. 19, No.3, July 1974, pp. 599-606. Gaudette, B. D., AProbabilities and Human Pubic Hair Comparisons,@ Journal of Forensic Sciences, JFSCA, Vol. 21, No. 3, July 1976, pp.514-517.
2.
3.
4.
5.
6.
7.
8.
9.
10. Gaudette, B. D., ASome Further Thoughts on Probabilities and Human Hair Comparisons,@ Journal of Forensic Sciences, JFSCA, Vol. 23, No. 4, Oct. 1978, pp. 758-763. 11. Gaudette, B. D., AA Supplementary Discussion of Probabilities and Human Hair Comparisons,@ Journal of Forensic Sciences, JFSCA, Vol. 27, No. 2, April 1982, pp. 279-289.
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Appendix 2:
Hair Examination Worksheets
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Primer Residue/Handwiping Protocol By Graphite Furnace Atomic Absorption Spectrophotometry, Version 2.2
Primer Residue/Handwiping Protocol by GFAAS, Version 2.2 Page 1 of 14
Revisions & Corrections Trace Evidence Unit Primer Residue/Handwiping Protocol, Version 2.2 Effective Date 1/22/08 Description Changes from Version 2.1 to 2.2 Revision: Revision of Section I to remove extraneous information Revision: Revision of Section III to clarify pipettes and standards used in protocol Revision: Revision of Section IV to clarify personal protective equipment requirements Revision: Revision of Section V; to add 2% Nitric Acid to the solution list, to add units (g) to the standard value table and to correct QC1 values listed in that table Revision: Revision of Section VII to clarify use of new tubes, to change the rinse solution used and to delete reference to the Standard Operating Procedure provided by the Toxicology Unit Revision: Revision of Section VIII; to clarify case information needed on handwipings worksheet, to clarify how caps should be placed on tubes when heating, to change references to 1 ml diluted samples or extracted solutions to ~ 1 ml diluted samples or extracted solutions Revision: Change of Section X to allow stock standards and QC stock standards to be from different lots/batches instead of exclusively from different manufacturers Revision: Revision of Section XI to add HWAA and HW/AA to list of abbreviations Addition: Addition of Appendix 1 (Handwiping Worksheet) Addition: Addition of Appendix 2 (Instrument Parameters) Revision: Revision of page numbers Authorized by Spence
Dallas County Institute of Forensic Sciences Page 2 of 14 Forensic Laboratory
Primer Residue/Handwiping Protocol, version 2.2

I. Principle This manual is not intended to serve as a textbook, nor is it intended to be a substitute for proper training that is the prerequisite for conducting handwiping examinations by Graphite Furnace Atomic Absorption Spectrophotometry (GFAAS). Examiners following this procedure should have received the proper training in atomic absorption spectrometry and passed all necessary competency tests required to perform the examinations covered by this manual. II. Introduction The forensic examination of handwipings uses Graphite furnace atomic absorption spectrophotometry as a method of measuring the quantity of the ammunition primer elements of antimony, barium and lead. This technique is well documented in the forensic science literature. III. Reagents and Supplies Atomic Absorption Spectrophotometer, Graphite Furnace High Purity Argon gas High Purity Nitric Acid Polypropylene culture tubes with snap caps (12mm x 75mm) Methanol (for cleaning graphite furnace) Centrifuge Vortex Oven Pipettes (i.e. 100 L 1000 L, 20 L 200 L, repeater pipette) and corresponding tips Polypropylene sampling cups Individual Atomic Absorption standards (1000 mg/L) of Antimony, Barium and Lead Partitioned graphite tubes Hollow cathode lamps for each element Antimony, Barium and Lead Johnson & Johnson cotton swabs, plastic shafts Nickel Modifier 1000 ppm in 0.1 % HNO3 Triton X or similar surfactant IV. Safety Appropriate personal protective equipment (PPE) shall be worn while handling evidence and preparing samples for analysis. Appropriate PPE includes gloves, lab coat and eye protection. V. Preparation of Chemical Solutions and Standards 5 % Nitric Acid - To make 1 liter solution, add 50 mL of concentrated Nitric acid to 950 mL of Millipore water. Mix thoroughly. Store in a large Nalgene bottle until ready for use.
Dallas County Institute of Forensic Sciences Page 3 of 14 Forensic Laboratory Primer Residue/Handwiping Protocol, version 2.2
2 % Nitric Acid - To make 1 liter solution, add 20 mL of concentrated Nitric acid to 980 mL of Millipore water. Add one drop of Triton X or similar surfactant for each liter of solution. Mix thoroughly. Store in a large Nalgene bottle until ready for use. Stock standard - In a 100 mL volumetric flask, add 1 mL Barium standard, 2 mL Lead standard and 0.1 mL Antimony standard. Fill to the mark with 5% Nitric acid. Mix thoroughly. This is a Critical Reagent. Standard swab (S3) - Place the two cotton swab tips in an appropriately labeled culture tube. Add 0.100 mL stock standard and 0.100 mL 5 % Nitric acid. Dry the swabs in uncapped tubes in the oven at 80C for two hours. Remove from the oven and allow to cool. Next, cap the tubes and set aside until time for analysis. QC Stock standard - In a 100 mL volumetric flask, add 0.8 mL Barium standard, 1.6 mL Lead standard and 0.08 mL Antimony standard. Fill to the mark with 5% Nitric acid. Mix thoroughly. This is a Critical Reagent. Make sure these purchased standards are from different lots / batches as those used for the Stock Standard. QC swabs - Place the two cotton swab tips in appropriately labeled culture tubes. Following the table below, add the corresponding amount of QC stock standard and 5 % Nitric acid. Dry the swabs in uncapped tubes in the oven at 80C for two hours. Remove from the oven and allow to cool. Next, cap the tubes and set aside until time for analysis. QC STD. QC1 QC2 QC STOCK STD. (mL) 0.000 0.100 5% NITRIC ACID (mL) 0.200 0.100
The S3 standard swab will be used as the high standard which the instrument will self dilute to create the calibration curve. The calculated amount of analyte measured for each standard is listed in the table below. Also included in this table are the standard values used to make the calibration curve and used as the QC values. These values take into consideration the dilution of the standard swabs.
STD.
ANALYTE Sb (g)
ANALYTE Ba (g)
ANALYTE Pb (g)
STD. VALUE Sb (g)
STD. VALUE Ba (g)
STD VALUE Pb (g)
S0 S1 S2 S3 QC 1 QC 2
0 0.025 0.050 0.100 0 0.080
0 0.250 0.500 1.000 0 0.800
0 0.500 1.000 2.000 0 1.600
0 0.0125 0.025 0.050 0 0.040
0 0.00625 0.0125 0.025 0 0.020
0 0.0125 0.025 0.050 0 0.040
VI.
Instrument Parameters Attached are the instrument parameters (Appendix 2) for the Antimony, Barium and Lead methods. These methods are used as guidelines. Either linear or quadratic algorithms are acceptable for forming the calibration curve. A fifty sample tray is utilized. If a cartridge case swab is being analyzed, this sample is run at the end of the batch with a blank sample of 5% Nitric Acid after each cartridge case sample. The dilution factor for Barium and Lead is 40X and 2X for Antimony. With cartridge case swabs, the dilution factor is 160X for Barium and Lead and 40X for Antimony. Three replicates are run for each sample; however, if the %RSD is less than 7 after two replicates, the third replicate will not be performed. If the absorption for a sample is 1.5 times the highest calibrator, the sample will be auto diluted using 1 L of sample and 19 L of blank. The sample will then be injected and the instrument will then continue to the next sample.
VII.
Maintenance Partitioned graphite tubes are used for the analysis of all three elements. Before each run, the graphite furnace should be cleaned. (Refer to the instrument operating manual.) If any pitting or abnormalities appear on the contact electrodes, they may need to be replaced. Other regular maintenance includes checking the water level in the recirculator, Argon gas pressure, rinse solution (2% Nitric Acid with a small amount of Triton X) and periodic emptying of the waste bottle.
VIII. Procedure

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Inventory evidence. Transfer case information (including FL #, item #, analysts initials) to the handwipings worksheet (Appendix # 1). Label corresponding tubes. If swabs have come in their own tubes, do not use those tubes; use the culture tubes from the laboratory. Visually inspect each swab and notate any gunpowder, debris or excessive blood. Also, notate on the worksheet how wet and dirty each swab is. Cut the tips off of each pair of swabs and place them in the corresponding tube. Dry the swabs in the uncapped tubes in an 80C oven for 2 hours. Remove the rack of tubes from the oven. Add 2 mL of 5% Nitric Acid to each tube. Vortex each tube to attempt to loosen the cotton from the shaft of the swab. Heat the tubes for another 2 hours in an 80C oven (with loose caps). Remove the rack of tubes from oven and allow tubes to cool. Vortex each tube to attempt to remove the cotton from the shaft of the swab. Centrifuge each tube. For the analysis of Barium and Lead, label a set of corresponding tubes. Dilute the extracted solution by combining 0.1 mL of extracted solution and 1.9 mL of 5% Nitric Acid. Thoroughly vortex the sample. Remove ~1 mL of the diluted sample and place in a corresponding sample cup in the autosampler tray. For the analysis of Antimony, remove ~1 mL of extracted solution and place in a corresponding sample cup in the autosampler tray. (Note: sample cups are to be precleaned and deactivated by soaking in 5 % HNO3 for 24 hrs then rinsed with deionized water and dried). For the extraction of cartridge case swabs, examine the swab as to whether it has been used. If the cartridge case swab does not appear to have been used, follow the procedure for the other swabs. If the cartridge case swab appears to have been used, follow the regular extraction method and the following dilution protocol: A. For Antimony, dilute 0.1 mL of the extracted solution with 1.9 mL of 5 % Nitric Acid. Vortex sample. Place ~1.0 mL of diluted sample into a corresponding sample cup in the autosampler tray. For Barium and Lead, dilute 0.05 mL of extracted solution with 3.95 mL of 5% Nitric Acid. Vortex sample. Place ~1.0 mL of diluted sample into a corresponding sample cup in the autosampler tray.
11.
12.
B.
IX.
Reporting Guidelines In order to conclude the characteristics of gunshot residue are present in a set of handwipings, all three elements (Antimony, Barium and Lead) should meet or exceed an established threshold level on the same part of the hand. The threshold levels are 0.05 g for Antimony, 0.50 g for Barium and 1.0 g for Lead. The presence of gunshot residue on handwipings is consistent with the person: 1. Discharging a firearm 2. Handling a firearm (or firearm component) which has recently been fired or an unclean firearm 3. Having the hand(s) close to a discharging firearm

The absence of gunshot residue on handwipings is consistent with the person: 1. Not discharging a firearm 2. Discharging a firearm that does not deposit significant residue 3. Washing or wiping the hands X. Quality Assurance & Quality Control A high standard is auto-diluted (using 0, 5, 10 and 20 L) and used to develop a calibration curve on each element for each batch of samples. QC samples of known concentrations are analyzed periodically during the run (approximately every 40 firings). QC 1 is a blank sample for the purpose of checking for carryover and swab contamination. The QC values, sometimes designated by the symbol ~, should be less than the first standard value. The QC 2 values must be within 20 % of the expected value. If the QC sample fails, the method is set up to flag and continue. The calibration curve is deemed acceptable if the correlation coefficient meets or exceeds 0.990. A recalibration will occur if the correlation coefficient criteria is not met. At the end of the analysis, the examiner is responsible for reviewing the data, calibration curve, correlation coefficient and all QC values. If any of the values are not within acceptable ranges, the samples must be re-analyzed. The purchased standards used to make the Stock Standard and QC Stock Standard must be from different lots / batches or manufacturers to insure the reliability of each standard solution. When a new set of standard and QC swabs are made, a set of new swabs is analyzed as samples using a set of the old swabs as calibrators. The concentrations for the new swabs must be 20 % of the expected value. If this fails, these new swabs are discarded and another new set is made and tested. XI. Abbreviations HW - Handwipings Sb - Antimony Ba - Barium Pb - Lead Ppm - Parts per million (mg/L) HWAA or HW/AA - Handwipings analysis by Atomic Absorption Spectrometry GSR - Gunshot Residue %RSD Percent Relative Standard Deviation C Control LB Left hand back LP Left hand palm RB Right hand back RP Right hand palm CC Cartridge Case
XII.
References Primer Residues Deposited by Handguns, Cooper, Guileyardo, Stone, Hall and Fletcher, American Journal of Forensic Medicine and Pathology, 15(4), 1994, pp. 325327. Barium and Antimony Distributions on the Hands of Nonshooters, Havedost, Peters and Koons, Journal of Forensic Sciences, 1990, pp. 1096-1114. A Survey of Gunshot Residue Analysis Methods, Singer, Davis and Houck, Journal of Forensic Sciences, March 1996, pp. 195-198. A Reevaluation of the Aerospace Corporation Final Report on Particle Analysis. When to Stop Searching for Gunshot Residue (GSR)?, Anthony Owens, Journal of Forensic Sciences, 35(3), May 1990, pp. 698-705. Analysis of Gunshot Residue Test Results in 112 Suicides, Reed, McGuire and Boehm, Journal of Forensic Sciences, 35(1), January 1990, pp. 62-68. FBI Academy Primer Residue School Notebook.

Appendix # 1 Handwiping Worksheet
Lab #_________________________________________ Agency #_________________________________________ DCME # _________________________________________
Item # Locatio n Clean Slight Moderate Heavy Wet Damp Dry Blood Gunpowder Other Ba(g) Pb(g) Sb(g) Ba/Sb
C LB LP RB RP C LB LP RB RP
KIT TYPE:
___ Criminal Research Products ___ Kinderprint ___ Lynn Peavey Co. ___ Sirchie ___ Tri Tech ___ Other ___________________
SHAFT:
___ Wood ___ Paper ___ Plastic
CONTAINERS:
___ Plastic bags ___ Plastic tubes (___used ___ Glass ___ Paper ___ Other ___returned)
Weapon:___________________________________________________________________________________________________ Ammunition:_______________________________________________________________________________________________ Number of shots fired: Environment: Shooting: Sample: Subject 1: Name:___________________________________ Activity:___________________________________ ___________________________________ ___________________________________ Sealed:__________________________________ ___ Right Handed ___ Left Handed _____ ___Inside ___Outside Shooting: Sample: Subject 2: Name:________________________________________ Activity:________________________________________ ________________________________________ ________________________________________ Sealed:________________________________________ ___ Right Handed ___ Left Handed _____ ___Inside ___Outside Subject 2 ________________________ Subject 2 ________________________
Subject 1 _____________________ Subject 1 _____________________
Remarks:____________________________________________________________________________________________________ ____________________________________________________________________________________________________________ ____________________________________________________________________________________________________________ __________________ Prepared by: ________________________ Date: ___________________________________

Appendix # 2 Instrument Parameters
Trace Evidence Unit SEM/EDS Analysis of GSR Protocol, Version 1.3
Dallas County Institute of Forensic Sciences Trace Evidence Unite Page 1 of 48
SEM/EDS Analysis of GSR Protocol, Version 1.3 Effective date: 5/5/2008
Revisions & Corrections Trace Evidence Unit SEM/EDS Analysis of GSR Protocol, Version 1.X Effective Date 1/22/08 Description Changes from Version 1.0 to Version 1.1: Revision: Revision of Section 1 to remove extraneous information and clarify the scope. Revision: Revision of Section 2 to remove ASTM E 1588-95. Deletion: Deletion of the Summary of Practice and Significance of Use sections Revision: Revision of Section 3 to add lint free cloth gloves. Revision: Revision of Section 4 to clarify safety concerns. Addition of Section 5 Standards/Calibration/Controls; quality assurance/quality control information is contained within this section. Deletion of Quality Assurance/Quality Control section. Addition of negative batch control use. Change Section 5.2; calibration of amp time on EDAX detector changed from monthly to semi-annually. Addition of the requirement to collect an image and EDS spectrum of the 5 m particle on the Plano stub to verify that the instrument is capable of identifying the elements Sb, Ba, and Pb Addition of QC testing of carbon rods. Addition: Addition of Section 6 Procedure; all procedural and sample prep information was simplified and condensed under this single heading. Deletion of Sample Handling/Preparation, Procedure (General), and Procedure (Detailed) sections. Changes made by a memo dated 10/18/06 were incorporated into this section. Revision to Section 7 to detail the procedure for an analyst to override the particle classification assigned by the automated software classification scheme. Revision: Revision of Section 7 to reflect changes in definition and classification of GSR particles described in ASTM E 1588-07. Authorized by Spence
Revision: Changes to Section 8; maintenance schedules for the mechanical pump oil and power supply air filter were changed. Deleted reference to the Erlenmeyer flask and use of an air can to clean the instrument. Clarified wording referring to replacement and cleaning of tungsten filament and Wehnelt, respectively. Addition: Addition of Appendix 9.7 Philips XL30 ESEM Maintenance Chapter 6 Addition: Addition of SEM/EDS Worksheet. Addition: Addition of Carbon Coater Logbook Sample Loading Table Worksheet. Addition: Addition of the Carbon Coating Procedure from the SEM/EDS Training Manual as an appendix. Revision: Revisions of page numbers and section numbers. Revision: Revision to Section 6.1.5
Subsequent changes are tracked on the Trace Procedures Collection Revisions & Corrections Log

1 Scope Gunshot residue (GSR) particles can be detected and identified, based on morphology and elemental composition, using automated Scanning Electron Microscopy/Energy Dispersive Spectrometry (SEM/EDS) analysis. This method is a sensitive, non-destructive technique used to detect the primer residue component of gunshot residue. Particles characteristic of or consistent with GSR detected during the automated analysis are then confirmed by the examiner. This manual is not intended to serve as a textbook, nor is it intended to be a substitute for the proper training that is the prerequisite for conducting gunshot residue (GSR) examinations by SEM/EDS. 2 Related Documents None 3 3.1 Equipment & Materials Philips XL30 ESEM Scanning Electron Microscope w/tungsten gun and 5-axis motorized stage (100 mm X 100 mm X 60 mm), secondary electron (SE) detectors, backscatter electron detectors (BSD), CCD detector. EDAX Falcon processor with EDAX Genesis software and EDAX Sapphire Energy Dispersive X-ray detector w/Super Ultra Thin Window (SUTW). Ultrasonic cleaner Gunshot Residue Evidence Collection kits with pin stubs w/ carbon tape adhesive Pin stubs with carbon tape adhesive Pin stub forceps Liquid nitrogen X-ray detector/backscatter electron detector (BSD) calibrator stub (copper and titanium on aluminum) GSR reference standard stub (PLANO GSR Standard stub) Carbon coater Denton Vacuum DV-502 Carbon rods critical reagent Lint free cloth wipes Cotton swabs Soft Scrub or equivalent cleaner Solvents (methanol, isopropanol and acetone) Lint free cloth gloves Powder-free gloves Edwards Ultra Grade 19 pump oil
SEM/EDS Analysis of GSR Protocol, Version 1.3 Effective date: 2/28/2008 Page 4 of 48
3.2
3.3
Dallas County Institute of Forensic Sciences Trace Evidence Unite

Portable external hard drive 4 4.1 Safety During sample preparation of SEM sample stubs, gloves and a lab coat or plastic apron must be worn. When handling liquid nitrogen, a lab coat, Cryo-gloves and a face shield must be worn. When carbon coating, a tinted face shield (welders helmet or equivalent) must be worn. Others present in the lab at the time of coating must be warned not to look at the carbon coater. Standards / Controls / Calibration The calibration of the microscope and EDAX micrometers is beyond the capabilities of analysts in the Trace Evidence Unit; however, the calibrations can be checked simply by imaging a specimen of known dimensions (such as the central 5 m simulated GSR particle on the Plano Standard stub). The measurement of the specimen should closely resemble the actual measurement of the specimen. Also, the same specimen should be imaged and measured using the imaging tab in EDAX Genesis. The measurement in Genesis should also closely match the known measurement of the specimen. The magnification check should be performed at a minimum of 2500X. These measurements shall be performed at least semi-annually and documented in the maintenance logbook. Should the calibration of either the microscope or EDAX unit vary more than five percent, the appropriate vendor should be contacted for service. The amplification (amp.) times used for X-ray analysis including the 100 s amp. time should be calibrated semi-annually. The calibration is performed as specified in the Genesis Spectrum Users Manual Chapter 4 (4.3.3 Automatic Calibration). The x-ray detectors resolution should not exceed 150 eV at 100 s amp. time. If the calibration test indicates that the detector exceeded the 150 eV maximum resolution at the 100 s amp. time, optimize the microscope beam and recalibrate. If after several attempts the calibration continues to fail, contact EDAX for service. The calibration results are to be logged into the EDAX X-ray Detector Calibration Log (Appendix 9.3) and retained with the log book. Prior to running a GSR analysis run, a known simulated GSR sample (PLANO STANDARD SPS A521-1) will be run. The Plano Standard will be analyzed at the same magnification and analysis
4.2
4.3
5 5.1
5.2
5.3
5.3.1

parameters as the actual sample run. The Plano standard is to be located in the instrument at the same time as the actual case samples and run just prior to the actual case sample run with the same beam settings. When run at 236X, a grid of 3X4 fields will be analyzed (different magnifications will require different grid sizes). The analysis at 236X and 3X4 grid size should include the 5 m particle located in the upper right quadrant of the Plano standard stub (Appendix 9.2), and include the closest 1 m particle and three 2 m particles located near the 5 m particle as indicated on the particle map of SPS A521-1. Slight variations in the particles located and identified may be due to variations in the positioning of the 3X4 grid with respect to the grouping of particles. Each of the particles described above should be located when the instrument is focused sharply and is running optimally. Also, during the automated analysis, these particles should auto-classify as GSR 3 Comp. Should the above particles not be resolved or auto-classify as GSR 3 Comp., the focus, backscatter calibration and all analysis parameters should be checked and the QC analysis re-run. If after repeated attempts at optimizing the instrument and running the Plano standard, the particles still cannot be resolved and or classified as GSR 3 Comp., no further analysis will be performed until the instrument has been serviced and deemed suitable for analysis. 5.3.2 The x-ray spectrum of one of the 5 m particles on the Plano stub will be imaged and the x-ray spectrum for this particle will be collected and printed. The printed image and spectrum of this analysis will be included with each case packet to document that the detector is capable of detecting the elements Sb, Ba, and Pb. The carbon rods used for carbon coating will be tested prior to use in casework. The carbon rods will be tested by SEM/EDS to determine the presence of detectable levels of Sb, Ba, and Pb. Also, the carbon rods will be used to coat blank (unused) sample stubs and will be tested by Automated SEM/EDS for the presence of gunshot residue particles. The results of these analyses will be documented in the Critical reagent logbook. With every batch of sample stubs, a negative control stub will be utilized and treated like those samples being analyzed. The results of the negative control stub analysis will be documented in the case packet. The negative control stub does not need to be retained. If GSR particles (characteristic or consistent with, sections 6.2.2.14 and 6.2.2.15, respectively) are detected on the negative control stub, those findings will be documented in the lab report. Procedure Sample Handling/Preparation The sample preparation area will be cleaned according to the Housekeeping Protocol
5.3.3
5.4
6 6.1 6.1.1

when preparing GSR samples for SEM/EDS analysis. 6.1.2 Preparation of SEM stubs shall be performed in such a manner as to eliminate or minimize the potential for sample contamination. Any sample handling is performed while using only clean utensils and while wearing clean/powder free gloves. The evidence containers will be properly labeled with the laboratory number, item number, analyst initials and date. Once the evidence seal is broken, care should be taken so that no object touches the surface of the collection stub and that the specimen stub is not left uncovered any longer than is reasonable for transfer or mounting. Document details of the case and evidence packaging condition on the SEM/EDS GSR Worksheet (Appendix 9.5). Summary results of analysis will be documented on this worksheet post-analysis. Worksheets will be retained with the case file. The SEM stub containers will be labeled in such a manner that they are distinguishable from other specimen stubs. Use of uniquely numbered stubs (from Tri-Tech, Inc.) is recommended. The sample stub container shall be labeled with the laboratory case number, item number, unique stub number (if present), analysts initials and date. Also, insure that the stubs sampling location (i.e. right back (RB), right palm (RP), left back (LB) and left palm (LP)) is marked on the stub container. Sample collection from items of clothing The evidence submission form will be reviewed to determine the requested analysis. The submitting agency and or detective may be contacted to clarify any analysis requests. The submitting agency may also be contacted to determine if they have any specific reasons to sample specific areas of a garment such as a certain pocket or side of the shirt or garment such as the waistband of a pair of pants. The examiner will prepare the workbench surface for analysis by pre-cleaning with 10% bleach. The work surface will then be covered with a clean sheet of bench paper. The examiner will wear a clean lab coat or fresh disposable lab apron, clean gloves and eye protection while performing the analysis. The examiner will then inventory the item of evidence and then insure that the evidence container is adequately marked with the case number, item number, and analysts initials. Upon opening the evidence container, each item within the container will then be inventoried and the examiner will verify that the item is marked with the case number, item number and analysts initials whenever possible. If the item is unsuitable for marking with the analysts initials, lab number and item number, the analyst will document that in the bench notes.
6.1.3
6.1.4
6.1.5 6.1.5.1 6.1.5.2
6.1.5.3
6.1.5.4
6.1.5.5
Only outer layer garments will be sampled for the presence of primer gunshot residues unless specific circumstances exist such as at the direction of the submitting agency due to an indication that a shot was fired from under a coat or that a subject placed a firearm or fired firearm component in an inside pocket or in the waistband of a pair of pants. The examiner will visually and or microscopically examine the garment for the presence of bullet defects and or areas of apparent soot. Bullet holes and areas of apparent soot will be sampled using uniquely numbered conductive carbon coated aluminum pin stubs (D stubs from Tri-Tech, Inc.). Other areas of a garment to be sampled for GSR include cuffs of long sleeve shirts, jackets, sweaters, etc. At least one sample stub will be collected from each cuff area on long sleeve garment. Also, the front upper left quadrant, front lower left quadrant, front upper right quadrant and front lower right quadrant will also be sampled using at least one D stub per quadrant. The rear of a shirt, sweater, jacket etc. will not routinely be sampled for GSR unless the area has been specifically identified as a probative area either by direct observation of a bullet defect or area of soot or by communication from the submitting agency. The analyst may sample other areas as deemed necessary by the examiner. Short sleeve or no sleeve garments will be sampled in the front upper left quadrant, front lower left quadrant, front upper right quadrant and front lower right quadrant using D stubs from Tri-Tech, Inc. Additional areas of the garment may also be sampled as deemed necessary by the examiner. Examination of other garments such as pants, shoes, caps, etc. will be sampled for primer GSR only when specifically requested by the submitting agency or when an analyst has reason to believe that their sampling will be probative to a case. Examples of reasons that a pair of pants or another garment should be sampled include but are not limited to observations of soot or apparent bullet defects in the garment or statements from witnesses or communications with the submitting agency indicate that a weapon or fired cartridge case was placed in the pocket or waistband of the garment or that a shot was fired in close-proximity to the garment. Sample collection from bedding material The submitting agency and or detective may be contacted to clarify any analysis requests. The submitting agency may also be contacted to determine if they have any specific reasons to sample specific areas of an item.
6.1.5.6
6.1.5.7
6.1.5.8
6.1.5.9
6.1.5.10
6.1.6 6.1.6.1

6.1.6.2 The examiner will prepare the workbench surface for analysis by pre-cleaning with 10% bleach. The work surface will then be covered with a clean sheet of bench paper. The examiner will wear a clean lab coat or fresh disposable lab apron, clean gloves and eye protection while performing the analysis. The examiner will then inventory the item of evidence and then insure that the evidence container is adequately marked with the case number, item number, and analysts initials. Upon opening the evidence container, each item within the container will then be inventoried and the examiner will verify that the item is marked with the case number, item number and analysts initials whenever possible. If the item is unsuitable for marking with the analysts initials, lab number and item number, the analyst will document that in the bench notes.
6.1.6.3
6.1.6.4
Only outer layer bedding will be sampled for the presence of primer gunshot residues unless specific circumstances exist such as at the direction of the submitting agency due to an indication that a shot was fired from under a layer of bedding material. The examiner will visually and or microscopically examine the bedding material for the presence of bullet defects and or areas of apparent soot. Bullet holes and areas of apparent soot will be samples using uniquely numbered conductive carbon coated aluminum pin stubs ( D stubs from Tri-Tech, Inc.).
6.1.6.5
6.1.6.6
6.1.6.7
At least one sample stub will be collected from each area of the bedding material suspected of having primer gunshot residues using at least one D stub per area. The analyst may sample other areas as deemed necessary by the examiner. Sample collection from auto parts The submitting agency and or detective may be contacted to clarify any analysis requests. The submitting agency may also be contacted to determine if they have any specific reasons to sample specific areas of an item. The examiner will prepare the workbench surface for analysis by pre-cleaning with 10% bleach. The work surface will then be covered with a clean sheet of bench paper. The examiner will wear a clean lab coat or fresh disposable lab apron, clean gloves and eye protection while performing the analysis. The examiner will then inventory the item of evidence and then insure that the evidence container is adequately marked with the case number, item number, and analysts initials. Upon opening the evidence container, each item within the
6.1.7 6.1.7.1
6.1.7.2
6.1.7.3

container will then be inventoried and the examiner will verify that the item is marked with the case number, item number and analysts initials whenever possible. If the item is unsuitable for marking with the analysts initials, lab number and item number, the analyst will document that in the bench notes.
6.1.7.4
Only outer layer auto parts will be sampled for the presence of primer gunshot residues unless specific circumstances exist such as at the direction of the submitting agency due to an indication that a shot was fired from an underlying area such as from under a seat. The examiner will visually and or microscopically examine the material for the presence of bullet defects and or areas of apparent soot. Bullet holes and areas of apparent soot will be samples using uniquely numbered conductive carbon coated aluminum pin stubs (D stubs from Tri-Tech, Inc.). At least one sample stub will be collected from each suspected area of auto parts suspected of having primer gunshot residues using at least one D stub per area. The analyst may sample other areas as deemed necessary by the examiner. Sampling of miscellaneous items for GSR The submitting agency and or detective may be contacted to clarify any analysis requests. The submitting agency may also be contacted to determine if they have any specific reasons to sample specific areas of an item. The examiner will prepare the workbench surface for analysis by pre-cleaning with 10% bleach. The work surface will then be covered with a clean sheet of bench paper. The examiner will wear a clean lab coat or fresh disposable lab apron, clean gloves and eye protection while performing the analysis. The examiner will then inventory the item of evidence and then insure that the evidence container is adequately marked with the case number, item number, and analysts initials. Upon opening the evidence container, each item within the container will then be inventoried and the examiner will verify that the item is marked with the case number, item number and analysts initials whenever possible. If the item is unsuitable for marking with the analysts initials, lab number and item number, the analyst will document that in the bench notes. Only outer layer of the item will be sampled for the presence of primer gunshot residues unless specific circumstances exist such as at the direction of the submitting agency due to an indication that a shot was fired from an underlying area of the item.
6.1.7.5
6.1.7.6
6.1.7.7
6.1.8 6.1.8.1
6.1.8.2
6.1.8.3
6.1.8.4
6.1.8.5
The examiner will visually and or microscopically examine the material for the presence of bullet defects and or areas of apparent soot. Bullet holes and areas of apparent soot will be samples using uniquely numbered conductive carbon coated aluminum pin stubs (D stubs from Tri-Tech, Inc.). At least one sample stub will be collected from each suspected area of the item suspected of having primer gunshot residues using at least one D stub per area. The analyst may sample other areas as deemed necessary by the examiner. Many GSR samples on carbon adhesive SEM stubs will contain fibers or other debris which may charge while being analyzed in the SEM. In order to reduce or eliminate the charging, the samples may require carbon coating prior to analysis. Should the sample still exhibit significant charging which interferes with the analysis of GSR, the sample may then be recoated with carbon. When carbon coating is performed, a negative control stub will be coated with those stubs. (Appendix 9.6) Sample stubs, including the negative control stub, will be loaded into the SEM chamber and their locations recorded on the SEM Stage Sample Loading Table (Appendix 9.4) for tracking purposes during the analysis. The loading table does not need to be retained. After loading samples into the chamber, pump the SEM chamber down to operational vacuum. Upon completion of analysis, the sample stubs will be returned to their containers. The outer containers are sealed and initialed. Analytical Procedures PLANO Standard Run Insure that the electron beam is optimized at 25 keV. Allow to stabilize for at least 15 minutes. Obtain sharp focus using PLANO stub. Perform backscatter detector (BSD) calibration using the calibration stub. Calibration of the BSD is performed at 236x magnification. Set the minimum particle size threshold to 0.49m or less and the maximum particle size threshold to 100 m.
6.1.8.6
6.1.8.7
6.1.9
6.1.10
6.1.11
6.2 6.2.1 6.2.1.1
6.2.1.2 6.2.1.3 6.2.1.4 6.2.1.5

6.2.1.6 6.2.1.7 Center beam on upper 5 m particle on PLANO stub. Obtain sharp focus. Enter stub location and description for the PLANO standard using the EDAX software. Verify that detector is set to backscatter detector (BSD), that magnification is at 236x, and that the instrument scan control is set to external XY. Initiate the automated analysis run of the PLANO standard using an image resolution of 2048x1600 and a 3x4 grid. Start the PLANO standard run by depressing the MULTI-STUB button; name the analysis run using the following format: YYMMDDX where X is A for the first run of the day, B is for the second run of the day, etc. Press OK to start the run. 6.2.1.11 Verify that the particles referenced in section 5.3.1 were resolved and auto-classified as GSR 3 Comp. during the automated PLANO run. The PLANO jobsummr.txt file, the PLANO stubxx.csv file, and a printout of the stub-view image of the twelve fields showing the positions of each detected particle will be printed. These data sheets will be initialed and dated by the examiner. The original or a copy will be placed in each affected case packet. Sample Analysis Run Insure that the electron beam is optimized at 25 keV. Allow to stabilize for at least 15 minutes. Obtain sharp focus using one of the sample stubs. Perform backscatter detector (BSD) calibration using the calibration stub. Calibration of the BSD is performed at 236x magnification. Set the minimum particle size threshold to 0.49 m or less and the maximum particle size threshold to 100 m. Obtain sharp focus on the negative control stub.
6.2.1.8
6.2.1.9
6.2.1.10
6.2.1.12
6.2.2 6.2.2.1
6.2.2.2 6.2.2.3 6.2.2.4 6.2.2.5
6.2.2.6

6.2.2.7 Enter stub location and description for the negative control stub using the EDAX software. Record the location of the stub on the SEM Stage Sample Loading Table. The SEM Stage Sample Loading Table does not need to be retained. (Appendix 9.4) Repeat steps 6.2.2.6 and 6.2.2.7 for each sample stub. Verify that the detector is set to backscatter detector (BSD), that magnification is at 236x, and that the instrument scan control is set to external XY. Initiate the automated analysis run of the sample stubs using an image resolution of 2048x1600 and a 15x20 grid. Start the sample run by depressing the MULTI-STUB button; name the analysis run using the following format: YYMMDDX where X is A for the first run of the day, B is for the second run of the day, etc. Press OK to start the run. 6.2.2.12 Verify that no GSR (characteristic or consistent with) particles are present on the negative control stub. Review the stubxx.csv files. From the stubxx.csv files, print at least a representative sample of particles of interest for each sample stub. Also print the jobsummr.txt file for the batch analysis. These data sheets will be initialed and dated by the examiner. The original or a copy of the jobsummr.txt document will be placed in each affected case packet. The original printed pages of the stubxx.csv document will be placed in the corresponding file. The examiner must manually verify/confirm up to five characteristic GSR (Sb, Ba, and Pb) particles for each sample stub. If five or more characteristic GSR particles (containing Pb, Ba, and Sb) are found, then at least five particles must be confirmed. If fewer than five characteristic GSR particles (containing Pb, Ba, and Sb) are identified then each of the particles must be confirmed. If no characteristic GSR particles are confirmed, the examiner must attempt to manually verify up to five particles consistent with GSR for each sample stub. Particles consistent with GSR include the following elemental profiles: antimony, barium (with no more than a trace of iron or sulfur) barium, aluminum (in the absence of sulfur) lead, barium
6.2.2.8 6.2.2.9
6.2.2.10
6.2.2.11
6.2.2.13
6.2.2.14
6.2.2.15

If fewer than five particles consistent with GSR are found, each of the particles must be confirmed. 6.2.2.16 To verify/confirm a particle, relocate the particle identified during the automated sample run. If needed for imaging and x-ray analysis purposes, view the particle at a magnification higher than 236x. Print a photomicrograph of the particle and the EDS spectrum with key element peaks (i.e. Sb, Ba, and Pb) labeled. If the analyst performing the manual review determines that a classification made during the automated portion of the analysis is inaccurate, then the analyst may upgrade or downgrade the classification of the particle by examining the EDS spectrum. During manual review of the particle, additional elements may or may not be detected; therefore, the analyst is responsible for accurately classifying the particle. The analysts classification of a particle supercedes the classification made by the computer during the automated analysis run. The upgraded or downgraded classification of a particle should be documented in the bench notes. Retain these documents with the case file. The number of confirmed characteristic GSR particles or particles consistent with GSR will be documented on the SEM/EDS GSR Worksheet. The absence of GSR particles will be documented on the SEM/EDS GSR Worksheet and will be stated in the report.
6.2.2.17
Reporting Guidelines The following are examples of common reporting formats; however, due to the wide variety of circumstances and results, the analyst is not limited to these reporting formats.
7.1
Interpretation of Characteristic GSR Findings (Number of characteristic particles detected ) particles characteristic of primer gunshot residue particle(s) were confirmed on the back of the left hand (___ particle(s)) and back of the right hand (___ particle(s)) of test subject name (item ___). These particles consist of the elements antimony, barium and lead and are considered to be characteristic of gunshot residue. The presence of these particles on an individuals hands could be due to the individual/deceased either: 1. 2. 3. Firing a firearm Handling a firearm or firearm component that has been fired Being in the proximity of a firearm when it was fired
7.2
Interpretation of Findings Consistent with GSR

(Number of particles consistent with GSR detected ) particles consistent with primer gunshot residue particle(s) were confirmed on the back of the left hand (___ particle(s)) and back of the right hand (___ particle(s)) of test subject name (item ___). These particles consist of the elemental profiles (list of consistent with elements) and are considered to be consistent with gunshot residue; however, some environmental sources can produce similar particles. 7.3 Interpretation of Negative GSR Findings Primer gunshot residue particles were not found on item ___. The absence of primer gunshot residue (GSR) particles on an individuals hands could be due to the individual/deceased: 1. 2. 3. 8 8.1 Not discharging a firearm Discharging a firearm/ammunition that does not deposit or produce significant characteristic or consistent with GSR primer particles on the firing hand Washing or wiping the hands after discharging or handling a firearm
Instrument Maintenance Philips XL30 ESEM The routine operational maintenance of the microscope shall be performed on an as needed basis as described below. Additional maintenance will be performed as needed per chapter 6 of the Operating Instructions manual (Appendix 9.7).
8.1.1
Cleaning the sample chamber The instrument sample chamber should be wiped clean as needed using a clean lint free cloth.
8.1.2
Changing the pump oil The oil in mechanical pumps HVP-1 and HVP-2 should be changed at least twice a year using Edwards Ultra Grade 19 pump oil.
8.1.3
Exchanging the Filament and Wehnelt cap (As needed) Follow the directions per section 6.3 of Appendix 9.7
8.1.4
Cleaning the Wehnelt cap


8.1.4.1 8.1.4.2 Remove the Wehnelt Assembly and Filament as per section 6.3 of Appendix 9.7 Using a cotton swab and Soft Scrub, clean and polish the inside of the Wehnelt cap and area around the aperture. Rinse with water. Clean for about 15 minutes in an ultrasonic cleaner using water. Rinse the Wehnelt cap with water. Clean the Wehnelt cap for about 15 minutes in an ultrasonic cleaner using Isopropanol. Dry the Wehnelt cap using clean compressed air. Replacing the power supply air filter (Twice yearly) Remove the front cover from the electron microscope desk console. Remove the air filter from the power supply by pulling the tab on the filter. Replace the filter with a new filter. Replace the front cover to the electron microscope desk console
8.1.4.3 8.1.4.4 8.1.4.5 8.1.4.6
8.1.4.7 8.1.5 8.1.5.1 8.1.5.2 8.1.5.3 8.1.5.4
8.2
EDAX Falcon/Sapphire X-ray detector The 10 liter liquid nitrogen Dewar is designed to hold liquid nitrogen for 7 days; fill the Dewar as needed. Should the detector performance start to decline, the possibility of detector icing should be considered. If detector icing is suspected, allow the liquid nitrogen to run dry and acclimate to room temperature for several hours prior to refilling with liquid nitrogen. This cycling to room temperature will allow the icing to dissipate from the detector crystal; thus restoring the detector to it=s original performance.
8.3 8.3.1
Archival of Digital Instrument Data The entire electronic data analysis folder and its contents for each completed automated GSR casework date analysis set will be automatically saved to the EDAX Falcon processor computer at the completion of each data analysis run.

8.3.2 Due to the significant size of the electronic data files, the data files for each completed data analysis set will be temporarily downloaded to an external hard drive on a monthly or more frequent basis as casework dictates. Upon successful transfer of the electronic data analysis folders from the EDAX computer system to the portable hard drive, the original data files on the EDAX Falcon processor computer will be deleted in-order to free memory space on the EDAX computer hard drive. The data from the portable external hard drive will be uploaded to a secure Dallas County server from a networked computer on a quarterly or more frequent basis as hard drive storage space dictates. The data from the external hard drive will be deleted from the portable hard drive upon successful transfer to the secure Dallas County server. The archived data stored on the secured Dallas County server will be archived for a minimum of three years from the date of analysis. At the end of the three year period, the electronic data files may be deleted.
8.3.3
8.3.4
8.3.5 8.3.6

9 9.1 Appendices Plano Standard Certificate

9.2 Plano Standard Map including Upper 5 m particle
The boxed in area represents the approximate area of the Plano stub analyzed prior to sample runs.
9.3
EDAX X-ray Detector Calibration Log
Trace Evidence Unit EDAX X-Ray Detector Calibration Log A calibration will be performed and recorded semi-annually for each amp. time used for analyses, including the 100 micro. sec amp. Amp. Time Peak 1 Actual Peak 1 Ref. Peak 2 Actual Peak 2 Ref.
Date
Analyst
Resolution (eV)

9.4 SEM Stage Loading Worksheet
SEM STAGE SAMPLE LOADING TABLE

Date Loaded:______________________ Loaded By:__________________________ Date Unloaded:____________________ Unloaded By:_________________________
Stage Location 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Reserve d 15 Reserve d 16
FL#
Item #
Unique Stub S/N
Sample Location
Description
Calibration Standard
Plano GSR Performance Sample

9.5 SEM/EDS GSR Worksheet
Lab #________________________
SOUTHWESTERN
INSTITUTE OF FORENSIC SCIENCES

AT DALLAS
Agency #_____________________ DCME #_____________________ Analyst______________________
TRACE EVIDENCE SECTION
SEM/EDS GSR Worksheet
Date ________________________
Item # Subjects Name Subjects Status Homicide Complainant Homicide Suspect Suicide Complainant Suicide Witness Assault Complainant Assault Suspect Other
Type of Weapon Type of Ammunition Date / Time Shooting Date / Time Stubs Collected Type / Condition of Container / Seal Condition of Stubs Negative Control S/N Results (# of particles confirmed) Characteristic Consistent Consistent Sb, Ba, Pb Pb, Ba Sb, Ba
Item/ Serial Number Negative Control
Location
Consistent Ba, Al
N/A

9.6 Carbon Coating Procedure Denton Vacuum DV-502 The interaction of the electron beam and samples not mounted on conductive adhesive sample stubs may result in sample charging. Sample charging results from static charge build up on the surface of non-conductive surfaces such as those of fibers, hairs and minerals. By grounding a sample through the use of carbon coating, the electron charging can be reduced or eliminated thus improving the analysis of a sample. Carbon coating is a process where a very thin film of carbon is deposited on the surface of a sample thus providing a path to ground for electrons from the electron beam. Carbon is chosen for GSR analysis because it does not interfere with the elements of interest that are found in GSR particles. A. Start Up of Cold System All valves are closed and all switches are off. 1. 2. 3. Turn on water and main switch (toggle circuit breaker). Turn on mechanical pump switch. Turn on thermocouple gauge control to position #1 (tube reading is in manifold near mechanical pump). Open backing valve. Evacuate diffusion pump and system below the main valve to about 50 microns. Close backing valve. Open roughing valve and evacuate bell jar to about 50 microns. At this point you have pumped all parts of the evaporator to 50 microns or below, and you know the evaporator does not have any gross leaks or contamination. 6. Close roughing valve. Open backing valve. Make sure that cooling water is on (200 cc/min). Turn on diffusion pump switch. It will take about 10 minutes for the diffusion pump to reach operating condition. With the diffusion pump now at operating temperature, close backing valve, open roughing valve. Re-pump bell jar down to about 50 microns. This will only take a few seconds. Close roughing valve, open backing valve. Turn thermocouple gauge control to position to position #2 (reading in bell jar). Open main valve. You are now in high vacuum pumping.
4.
5.
7.
8.
9. 10.
Fill dewar with liquid N2. When thermocouple #2 indicates bell jar pressure below 5 microns, turn on cold cathode discharge gauge. a. b. Turn range selector switch to zero, wait 30 seconds for tube to warm-up. Press meter read switch. This is a momentary switch that energizes the high voltage supply. If bell jar pressure is above 1 micron, relay will disconnect the high voltage. Wait a few seconds and press meter read switch again. Turn range selector switch to right until a reading above 1 is obtained on meter. Pressure will be reading obtained times scale designation; i.e., a reading of 5 on the 105 scale indicates a pressure of 5 x 105 Torr. Return range selector switch to zero position and adjust needle to zero on meter. Turn off discharge gauge. Leaving discharge gauge on during coating will destroy the gauge.
c.
d.
e.
11.
To Carbon Coat: a. b. c. d. Prepare carbon rods. Enter the chamber (Section B: 1-3). Place specimens and negative control stub onto the sample stage. Insert carbon rods into carbon rod apparatus on the right post in the chamber. Center specimen under rods and put in piece of white paper (partially covered with microscope cover slip) to monitor carbon coating. Coating test strip does not need to be retained. Carefully replace bell jar. Make sure that dewar is filled with liquid N2. Pump down into high vacuum (Section C: 1-6).
e.
f. g. h.
i.
Turn selector switch to desired pair of electrodes. Right electrode is used for carbon coating. Turn Filament / Glow selector switch to Filament. Turn filament toggle switch on. Turn stage rotator switch to ON. Turn stage rotator control to desired speed. While wearing a welding helmet or equivalent tinted safety shield and watching the specimen, slowly increase voltage with filament adjust switch until carbon rods begin to spark. Decrease voltage slightly and hold until an adequate coat of carbon is laid down to meet your needs. Turn filament adjust switch to off. Turn off filament current switch. Close main valve. Slowly open chamber vent. Carefully remove bell jar. Close system and return to high vacuum (Section C: 1-6).
j. k. l. m. n.
o. p. q. r. s. t. B.
To Open Up System When Operating 1. 2. 3. With backing valve open and roughing valve closed. Close main valve. Turn off discharge gauge if on. Open air inlet valve to vent bell jar.
C.
To Operate When Diffusion Pump is Hot 1. Place bell jar on base plate making certain gasket and plate are clean. Close air inlet valve (chamber vent). Close backing valve.
2.
3. 4. 5. 6. D.
Open roughing valve; allow system to pump to below 50 microns. Close roughing valve. Open backing valve. Open main valve and proceed as in instructions in Section A-10.
To Close System Down 1. If system is open to air, place bell jar on base plate and rough down to ~ 100 microns or below. Pump to high vacuum as above if time permits. (Bell jar should always be left under high vacuum when not in use.) Turn off diffusion pump. Close main valve. Allow 10 to 20 minutes for diffusion pump to cool. Close backing valve. Turn off all switches, main switches, and main circuit breaker. Close diffusion pump cooling water valve. Remember that when closed down the bell jar should be in place and under vacuum. All valves should be closed and switches off.
2. 3. 4. 5. 6. 7.

9.7 Philips XL30 ESEM Maintenance Chapter 6
66
Dallas County Institute of Forensic Sciences Trace Evidence Unite SEM/EDS Analysis of GSR Protocol, Version 1.3 Effective date: 2/28/2008 Page 29 of 48
Trace Evidence Unit
Procedure for Housekeeping, Version 2.1
Trace Evidence Housekeeping Procedure Ver. 2.1
Revisions & Corrections Trace Evidence Unit Trace Evidence Housekeeping Procedure Version 2.1 Effective Date 1/22/08 Description Revision of Equipment/supplies section to remove detergent Revision of Appendix 2 to change presumptive testing and cleaning procedures; (Hot Zone microscopes) to add paper wrap as a viable material for covering the microscopes Revision of Appendices 3 and 4 to correspond with revisions of Appendix 2 Authorized by Spence
Trace Evidence Housekeeping Procedure Ver. 2.1 Page 2 of 11
Principle This document describes the procedures used by the Trace Evidence Unit (TEU) in regard to housekeeping. The Trace Evidence Unit is physically divided into an office area and a laboratory area (See Appendix 1). The office area is designated as a clean area where paperwork and other related office duties will be performed. The lab area is designated as a biohazard area where all physical and chemical analyses will be performed. The two areas are separated by a single door. All lab coats and evidence will be restricted from entering the office area. Personal Protective Equipment: Gloves, lab coat or plastic apron, shoe covers and eye protection. Equipment/supplies: 10% bleach (made fresh daily), spray bottle, squirt bottle, paper towels, bench paper, floor wax, mop handle, disposable mop pads (wet pads and dry pads), compressed air, lens cleaner, lens paper, water, foil, plastic wrap, tacky mats, sterile cotton swabs, presumptive blood testing reagents (leucomalachite green (LMG) solution or phenolphthalein (PHT) solution) and foaming disinfectant cleaner. Definitions Morgue Clothing Clothing evidence submitted from the morgue for the purpose of gunshot residue or trace evidence analysis (excluding ignitable liquid residue analysis). Hot Zone Pre-defined areas within the laboratory where morgue clothing will be processed for gunshot residues or trace evidence. This area is only considered a hot zone while morgue clothing is being processed for gunshot residues or trace evidence. The hot zone is no longer considered a hot zone after the analysis of morgue clothing has been completed and the zone has been cleaned per the cleaning methods below. When a hot zone is active, only a single case can be worked within the zone at that time. Main Bench Hot Zone The main bench hot zone is a designated area consisting of a portion of the main work bench and the surrounding perimeter floor as designated on the Trace Evidence Unit Diagram (Appendix 1). The front section of the main workbench which is outside of the hot zone can only be used by the analyst/analysts who are actively using the main bench hot zone (when the hot zone is active). Vent Hood Hot Zone The vent hood hot zone is a designated area consisting of the vent hood and surrounding floor and counter top as designated on the Trace Evidence Unit Diagram (Appendix 1). Tacky Mats Tacky mats will be located on the floor inside the lab at the main lab door area and office door area. Also, tacky mats will be located on the floor outside the boundaries for the main bench hot zone and vent hood hot zone areas.
Dallas County Institute of Forensic Sciences Forensic Laboratory Trace Evidence Housekeeping Procedure Ver. 2.1 Page 3 of 11

Cleaning Protocols The specific cleaning protocols for areas throughout the laboratory and office are detailed in Appendix 2. Weekly Presumptive Testing/Cleaning The areas described in the Weekly Housekeeping Assignments Chart (Appendix 3) will be presumptively tested and/or cleaned and logged weekly. Monthly Presumptive Testing/Cleaning The areas described in the Monthly Housekeeping Assignments Chart (Appendix 4) will be presumptively tested and/or cleaned and logged monthly. Personal Protective Equipment (PPE) Minimum personal protective equipment required for housekeeping is detailed in Appendix 5. Appendix 6 details minimum PPE for analytical activities. Quality Assurance/Quality Control The areas described in the Weekly Housekeeping Assignments Chart (Appendix 3) will be tested weekly for blood contamination using presumptive testing using the leucomalachite green (LMG) or phenolphthalein presumptive blood tests.
The areas described in the Monthly Housekeeping Assignments Chart (Appendix 4) will be tested monthly for blood contamination using presumptive testing using the leucomalachite green (LMG) or phenolphthalein presumptive blood tests. Should blood be detected in an area, the cleaning protocol described in Appendix 2 should be followed. The area will then be tested again after cleaning. If blood is detected in an area after cleaning (with the exception of the interior walls in the vent hood), the area will be re-cleaned until the area tests negative for the presence of blood.
Appendix 1: Trace Evidence Unit Diagram

Appendix 2: Cleaning Protocols Cleaning Protocols
Location Computer Areas/Desk (Office) Computer/Instrument Areas (Laboratory) Floor - Office Hot Zone - bench top Hot Zone - cabinet faces/drawer pulls Hot Zone - floor Hot Zone - hood Hot Zone - microscopes Non Hot Zone - floor (Laboratory) Hood (used for other than morgue clothing) (bench top) - Glass and Ignitable Liquid analyses, Slide prep, other non-biological sample prep Cleaning Procedure Wipe w/ 10% bleach. Wipe w/ 10% bleach. Mop w/ 10% bleach and Swiffer wet mop. Wipe w/ 10% bleach. Wipe w/ 10% bleach. Mop w/ 10% bleach and Swiffer wet mop. Wipe w/ 10% bleach. Cover knobs with foil/plastic/paper wrap pre-analysis. Remove foil/plastic/paper wrap post-analysis. Wipe w/ 10% bleach. Mop w/ 10% bleach and Swiffer wet mop. Frequency Monthly, as needed* Weekly, as needed* Weekly, as needed* Pre- and post-analysis/prep session; weekly, as needed* Post-analysis Post-analysis; weekly, as needed* Pre- and post-analysis; weekly, as needed* Clean post-analysis. Weekly, as needed*
Wipe w/ 10% bleach.
Pre- and post-analysis
Cleaning Protocols
Location Non Hot Zone microscopes AA prep bench top SEM prep bench top Slide prep bench top Sink areas Cleaning Procedure Wipe w/ 10% bleach. Wipe w/ 10% bleach. Wipe w/ 10% bleach. Wipe w/ 10% bleach. Wipe w/ 10% bleach. Frequency Monthly, as needed* Weekly, as needed*/Pre- and post-analysis/prep session Weekly, as needed*/Pre- and post-analysis/prep session Weekly, as needed*/Pre- and post-analysis/prep session Weekly, as needed*
Tacky mats (Adjacent to Remove top layer of tacky mat. As needed Hot Zone) Tacky mats (Lab Remove top layer of tacky mat. As needed entry/office entry) NOTE: Clean Hot Zone bench tops and clean Hot Zone floors will be waxed monthly. NOTE: If no analyses are performed within a week (e.g. analysts not present due to training/meetings), cleaning for that week is not required. NOTE: Any area potentially contaminated with blood during examination must be cleaned with 10% bleach and presumptively tested for blood. Repeat this process until the area tests negative. * Areas designated as weekly or monthly cleaning as needed will be presumptively tested for blood prior to cleaning. If the area is negative, no cleaning is necessary. If the area tests positive, clean the area using the corresponding cleaning procedure above. The area should be presumptively tested again. Continue to clean the area using the corresponding cleaning procedure until the area tests negative for blood. For the office and laboratory floor, when a positive area is found, only that area should be cleaned until negative, not the entire floor.
Appendix 3: Weekly Housekeeping Assignments Weekly Housekeeping a controlled This is an uncontrolled copy ofAssignments document Week of _______________ Note: Final review must be completed by no later than _________ Assigned Areas to be Presumptively Tested and/or Pre-Cleaning Post-Cleaning Individual Cleaned Test Results Test Results Initials Office Floor DWS desk area Sink area Middle desk area Printer area VH area Entry to office Refrigerator area Laboratory Floor AA prep area Side sink area SEM prep area SEM area Entry to lab Main bench hot zone (middle aisle) MSP area PLM area Hair bench area Freezer area Entry to office VH locker area Hood hot zone Computer/Instrument Areas GCMS area Glass microscope area Behind GCMS area PLM area Arson oven area MSP area Main bench Hot Zone Area Front Back Middle Front paper roll Back paper roll Vent Hood Hot Zone Area Desk Benchtop adjacent to hood Hood benchtop Main benchtop AA prep bench area SEM prep bench area/SEM console Benchtop Coater SEM console Slide prep bench area Benchtop Stereoscope Magnifier Sink Areas Main sink Side sink Reviewed by ________________________________ on ____________________________ Signature Date Dallas County Institute of Forensic Sciences Forensic Laboratory Trace Evidence Housekeeping Procedure Ver. 2.1 Page 8 of 11

Appendix 4: Monthly Housekeeping Assignments
Monthly Housekeeping Assignments Month of __________ Note: Final review must be completed by no later than the last day of the month PostAssigned Areas to be Presumptively Tested and/or Pre-Cleaning Cleaning Individual Cleaned Test Results Test Results Initials Office Individual Computer Areas/Desk Individual Computer Areas/Desk Individual Computer Areas/Desk Individual Computer Areas/Desk Individual Computer Areas/Desk Non Hot Zone microscopes Comparison scope Stereoscope PLM MSP Dissection scope (for SEM stub prep) Dissection scope (by arson oven) Hot Zone bench tops waxed Hot Zone floors waxed Reviewed by ________________________________ on _______________________________ Signature Date

Appendix 5: Minimum Personal Protective Equipment for Housekeeping Tasks
Task Cleaning office
Minimum PPE Gloves Plastic apron Eye Protection Cleaning hot zones in lab Gloves Lab coat or plastic apron Shoe covers Eye protection Cleaning of non-hot zones in lab Gloves Lab coat or plastic apron Eye protection Cleaning of analytical equipment and computer Gloves keyboards Lab coat or plastic apron Eye protection Appendix 6: Minimum Protective Equipment for Analytical Activities Task Gunshot residue/distance determination (morgue clothing) Routine PPE Gloves Lab coat Shoe Covers while in active hot zone Autopsy mask Eye protection Hearing and eye protection in firing range Gloves Lab coat Eye protection while processing evidence and chemicals Gloves Lab coat or plastic apron Gloves Lab coat Shoe covers while in active hot zone Autopsy Mask Eye protection
Gunshot residue handwiping analysis (AA) sample preparation
Gunshot residue analysis (SEM/EDS) sample preparation Examination of physical evidence (morgue clothing or significantly bloody evidence) for trace evidence
Examination of physical evidence (non- Gloves bloody or slightly bloody evidence) for Lab coat trace evidence Handling of bulk chemicals Gloves Lab coat or plastic apron Eye protection (safety glasses or face shield)
Dallas County Institute of Forensic Sciences Forensic Laboratory Trace Evidence Housekeeping Procedure Ver. 2.1 Page 10 of 11

Handling of liquid nitrogen Cryo-gloves Lab coat Face shield None Gloves Lab coat or plastic apron None Gloves Lab coat or plastic apron
Transporting properly sealed evidence Preparation of microscope slides Examination of microscope slides Sample preparation (visual inspection and insertion of d-flex strip into sample container) of fire debris for ignitable liquid analysis Sample extraction and loading sample extracts onto GC/MS for fire debris/ignitable liquid analysis
Gloves Lab coat or plastic apron Eye protection

SOP: FABRIC AND MATERIALS DAMAGE ANALYSIS, Version 1.0 (02.24.2009) I. Principle Textile items and other materials are examined to determine the mechanism for a separation or cause of damage. This method relies on macroscopic and microscopic examination of an exhibit to determine the physical characteristics of a defect, and to determine if the characteristics indicate a mechanism of separation or damage.
II. Sample Requirements Samples suitable for damage analysis shall include textile materials including clothing garments, fabrics, upholstery material and fabric backed tapes. Suitable samples may also include paper, plastics and other pliable materials. III. Safety Standard laboratory precautions Biohazard precautions, if applicable IV. Equipment & Materials Stereomicroscope with illumination Illuminated magnifying lens Scalpel, knife and other cutting instruments as needed Camera Indelible ink pen Rulers (metric and US Customary Units) Tape measures (US Customary Units) Trace evidence collection and preservation tools and materials: refer to the current version of the Trace Evidence Recovery Examinations General Procedures. V. Procedure 1. Examine the item macroscopically to determine the general location, shape and size of all significant damaged areas. a) Document the location of all significant/pertinent defects in the bench notes. b) Document the approximate shape of defects using sketches and/or photographs in the bench notes.
Dallas County Institute of Forensic Sciences Trace Evidence Unit Fabric and Materials Damage Analysis, Version 1.0 Page 1 of 13

c) Using an appropriate measuring device (ruler or tape measure), measure the extents of significant defects. i. Using a metric scale, measure to within ~ 0.5cm ii. Using US customary units, measure to within ~ 0.25. 2. Examine damaged areas with a stereomicroscope or a magnifying lens with appropriate illumination. a) Examine the damaged areas for microscopic features such as melted fibers, apparent lead residues, foreign fibers, glass, paint particles or other debris at the separation edge(s). i. The presence of foreign debris in the damaged area will be documented in the bench notes and photographed in situ if possible. ii. Loose foreign debris in the damaged area that is likely to be lost during analysis or handling will be collected and preserved using an appropriate method. b) Observe the fibers within each thread along the edge of damaged textiles to determine if they are uniform in length or if there is a large variation in length. c) Observe the ends of the threads along the edge of the defect to determine if adjacent threads are uniform in length or if there is a large variation in their length. d) Observe the damaged edges of other non fabric materials such as paper, plastic, leather, etc. to determine if the damaged surface is smooth or jagged in appearance. Determine the presence of tool marks on the damaged edge. The presence of tool marks along a defect edge will be documented in the case notes and if requested by the investigating agency, will be forwarded to the firearms unit for tool mark analysis. 3. The following types of damage may be identified on the basis of macroscopic and microscopic characteristics (see the Interpretation section for a more detailed discussion): i. Cuts (from knives, scissors, sharp implements, etc.) ii. Tears iii. Punctures iv. Burns v. Melts vi. Seam Separations vii. Normal wear viii. Abrasive wear 4. Observations of normal wear are noted in the bench notes but are not typically reported unless pertinent to the case.
Fabric and Materials Damage Analysis, Version 1.0 Page 2 of 13
5. Photograph and document all pertinent damaged areas. a) Examples of possible non-pertinent damage areas may include medical personnel cuts, normal wear defects, and burn holes, etc. b) Non-pertinent damage areas are typically defects which are not related to the criminal event under investigation. c) Non-pertinent damage areas may be noted in the bench notes; however, detailed examination of these areas is not required. d) The report will also reflect that not all defects were examined or that analysis was restricted to certain pertinent damage areas. 6. In some instances, experimental test cuts, tears, burns, or defects may be made to assist in making a determination. a) Test cuts, tears, burns, or other defects may be performed on a similar type of fabric or substrate material. b) The actual questioned item will not be used for tests such as cuts, tears, burns, etc. unless prior approval has been granted by the responsible agency such as the DAs office, court or submitting agency. i. If experimental test cuts, tears, burns, etc. are performed on the evidence item, the analyst shall clearly mark the test area to distinguish it from the damaged area in question. Test defects will be denoted by marking the area with indelible ink and labeling the test with T1, T2, T3, etc. c) A weapon/implement similar to the questioned weapon or implement may be used to make the test cut or tear. 7. If test cuts, tears, burns or other defects were produced, compare the characteristics of the tests to the damaged item. VI. Documentation of test results 1. Photograph the damaged edges of any test cuts, or significant tears, burns or other damage. a) Photographs will include overall and close up images of the damaged areas. b) Overall photographs or sketches will be included in the bench notes to aid in locating the relative position of the damage area to the exhibit being examined. c) Photographs will include a scale whenever practical. d) If annotations are made to a photograph to highlight specific features or other details, there must also be an un-annotated copy of the photograph included in the bench notes.
2. Document in the bench notes any specific features of the damage areas of test specimens such as uniform cut fiber ends, smooth cut surfaces, irregular fiber ends, or jagged or distorted edges. a) All bench note documentation should be made on the appropriate worksheets (See Appendix 1). 3. Document in the bench notes the presence of burnt fibers, melted fibers or melted edges at the defect. 4. Document in the bench notes any similarities and/or differences between the test defects and the questioned defects. VII. Interpretation 1. Cuts. A determination that the damage is characteristic of a cut is made when the individual fibers within each thread are uniform in length and the adjacent threads are uniform in length or that the damaged edge of the material is smooth in appearance. Cuts may also be characterized by tool marks that are lengthwise to the cut edge in appropriate materials. Secondary cuts may be observed in cases where the blade penetrates through a fold in the fabric material creating multiple cut defects from a single cutting event. a) Knife cut: Most often produced by a knife; however, may be produced by other sharp implements. Directionality may be indicated if the back of the blade produces different characteristics to the cutting edge. Variables which may affect the profile of the knife cut include the elasticity of the material, sharpness of the blade and angle of the blade to the material, and whether the material is taut or loose at the time the damage occurred. b) Scissor cut: Indicated by the presence of stoppages or small steps produced in the opening and closing action of the scissors as they are cutting along material. Scissor cuts may also be characterized by tool marks that are perpendicular to the cut edge in appropriate materials. Scissor cuts may also be characterized by V shaped notches that are sometimes observed at the terminal end of a scissor cut.

2. Tears. A determination that the damage is characteristic of a tear is made when the individual fibers within each thread display a large variation in their length and when the lengths of the adjacent threads display a large variation in their length or that the damaged edge of the material is jagged, stretched, distorted, or curled in appearance. 3. Mixed Cuts/Tears. Mixed cuts/tears are defects that show characteristics of both a cut and a tear along the length of the damage. 4. Normal Wear. Normal wear may be determined by the presence of irregular worn/frayed edges of holes and other defects. 5. Abrasive Wear. Abrasive wear may be determined due to the presence of worn/abraded fibers or surfaces in the presence of significant debris such as dirt, asphalt, cement particles and other debris. Sometimes, abrasive wear will result in a hole in the substrate material or may just be an abraded surface of the substrate material. Abrasive wear is often associated with hit-and-run type cases. 6. Punctures. Punctures may be characterized by jagged irregular edges in addition to the edges of the defect pointing in the direction of travel of the original puncture. a) Under some circumstances the edges of the defect may show smooth edges and may also have edges that point in the direction opposite of the initial puncture direction as a result of the implement being removed from the puncture. 7. Burns. Burn defects may be determined due to the presence of burnt fibers or material at the edge of the damaged defect. 8. Melts. Melt defects may be determined due to the presence of melted fibers or material at the edge of the damaged defect. 9. Seam Separations. Seam separations may be determined by broken or missing stitching threads at fabric seams. 10. Indeterminate. Damage with few clear characteristics may be difficult to interpret and may therefore be inconclusive.

VIII. Reporting Guidelines 1. If damage was identified, reports may generally be worded as follows: a) b) c) d) e) f) g) h) i) j) k) The damage was consistent with a cut (cut, knife-cut, scissor-cut) The damage was consistent with a tear The damage was consistent with a combination cut and tear The damage was consistent with normal wear The damage was consistent with abrasive wear The damage was consistent with a puncture The damage was consistent with a burn The damage was consistent with a melt The damage was consistent with a melt/burn The damage was consistent with a seam separation The damage lacked sufficient microscopic characteristics to determine the mechanism of damage
2. If damage was not identified, Reports may generally be worded as follows: No pertinent damage was identified in the ______________. 3. The presence of toolmarks on cut edges with potential probative value will be reported. 4. The presence of apparent significant foreign debris at a damaged area will be reported.
IX. Abbreviations 1. SC Scissor cut 2. KC Knife cut 3. C/T - Cut/Tear 4. NW - Normal Wear 5. AW - Abrassive Wear 6. Punct Puncture 7. SS Seam Separation 8. NSD No Significant Damage Identified 9. KN Knit 10. MP Medical Personnel damage 11. Pill Pilling 12. PA Planar Array 13. Snip Snippets

14. ST Steps or Stoppages
X. References 1. Stowell, L.I., Card, K.A., Use of Scanning Electron Microscopy (SEM) to Identify Cuts and Tears in a Nylon Fabric, Journal of Forensic Sciences, Vol. 35, No. 4. July 1990, pp. 947-950. 2. Monahan, D.L. and Harding, H.W.., Damage to Clothing Cuts and Tears, Journal of Forensic Sciences, Vol. 35, No. 4. July 1990, pp. 901-912. 3. Pelton, W.R., Distinguishing the Cause of Textile Fiber Damage Using the Scanning Electron Microscope (SEM), Journal of Forensic Sciences, Vol. 40, No. 5. September 1995, pp. 874-882. 4. Taupin, J.M., Damage to a Wire Security Screen: Adapting the Principles of Clothing Damage Analysis, Journal of Forensic Sciences, Vol. 43, No. 4. 1998, pp. 897-900. 5. Taupin, J.M., Clothing Damage Analysis and the Phenomenon of the False Sexual Assault, Journal of Forensic Sciences, Vol. 45, No. 3, 2000, pp. 568-572. 6. Taupin, J.M., Testing Conflicting Scenarios A Role for Simulation Experiments in Damage Analysis of Clothing, Journal of Forensic Sciences, Vol. 43, No. 4, 1998, pp. 891-896. 7. Robertson, J. and Grieve, M., ed., Forensic Examination of Fibers, 2nd ed., Examination of Damage to Textiles, Taylor and Francis, 1999, pp. 65-87.
XI. Terminology Related to Separation Abrasive wear Cut Bias Burn Hesitation cuts Indeterminate Knit Medical personnel damage Melt Mixed cuts/tears Nick Normal wear Pilling Planar array Puncture Scissor-cut Seam separation Selvedge Snippets Steps Wear caused by abrasive action such as by the friction between a material and a rough surface such as concrete or asphalt. A defect created by a sharp edge implement cutting the threads and fibers of a fabric or some other material. At an angle to. A defect created by the application of heat; characterized by burnt fibers or material. Defects caused by the action of the opening and closing action of scissors as they are cutting along a material. Not precisely determined, determinable, or established. Formed by interlocking loops of continuous thread. Created by medical personnel in order to examine patient most often by scissors and/or tearing. A defect created by the application of heat; characterized by a fused mass. Often, fibers will fuse together at the point of melting. A defect characterized by elements of a cut and a tear. Small cut or notch, sometimes at an end of a cut. Damage caused to garments in the course of everyday wear, such as matting of yarn ends and pilling. Small balls of fibers formed by friction Ends of fibers or yarns line up in the same direction Hole produced by an implement in thrusting action A cut created by the shearing action of an implement. Seam separations are characterized by the absence of stitching or damage to the stitching of a seam in a garment. The outer finished edge of a fabric Short segments of yarn created if a knit fabric is cut at an angle to the thread direction. A defect caused by the action of the opening and closing action of scissors as they are cutting along a material.

Stoppages Tears Tongues Tufts Weave Created by scissors in the opening and closing action. To pull apart or into pieces by force. Tears or scissor-cuts may give rise to tongue-like protuberances. Collection of snippets or loops of yarn from a knit. Formed by the interlacing of two sets of yarns at right angles.

XII. Appendix 1: Forms
Southwestern Institute of Forensic Sciences Dallas, Texas

FL # ___________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ Examiner: __________________ Date:___________________
Southwestern Institute of Forensic Sciences Dallas, Texas

FL # __________________
Examiner: _________________ Date: _________________

Fabric Separation Worksheet Trace Evidence Unit Southwestern Institute of Forensic Sciences FL# ________________ Item # ______________ Defect #:
Cut Knife-cut Scissor-cut Cut/Tear Tear Puncture Yes Yes Yes Yes Yes Yes No No No No No No Burn Melt Seam Separation Normal Wear Abrasive Wear Indeterminate Yes Yes Yes Yes Yes Yes No No No No No No
Notes:
Photos: Conclusion: Defect #:

Notes:
Photos: Conclusion: Analyst ____________________ Date ____________________

Fabric Separation Worksheet Trace Evidence Unit Southwestern Institute of Forensic Sciences FL# ________________ Item # ______________ Defect #:
Notes: ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ ______________________________________________________________________________ Photos: Conclusion: Analyst ____________________ Date ____________________

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