swifs controlled substances procedures manual v2.3 (02.26.2009) 157 pages.pdf

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Dallas County Southwestern Institute of Forensic Sciences

CONTROLLED SUBSTANCES

PROCEDURE MANUAL Version 2.3

Authorized by: Elizabeth Todd, Ph.D., Chief Forensic ChemistryMonica Lopez, Supervisor Controlled Substances LaboratoryKaren Young, Quality Manager

Effective date: February 26, 2009

This is a non-controlled copy of a controlled document.



B. Primary technical review is conducted by the primary analyst. C. Technical review is also conducted by a supervisor or any other signer of the case

report. D. Peer/technical review is also conducted by a non-signing analyst for 20% or six

(whichever is least ) cases per analyst per month.

E.

During the early stages of training, a report may be signed by the training analyst, theinstructor, and a supervisor. F. Components of case review are described in the Institute Quality Manual and in the

Guidelines for Reviewing Drug Cases resource document.

IV. Controlled Substances Quality Committee:

A. The Controlled Substances Quality Committee is made up of two or more Chemistsselected by the Controlled Substances Supervisor. Criteria for serving on theCommittee includes but is not limited to a broad understanding of overall laboratoryfunction, organization and communication skills, attention to detail, etc.

B.

Quality Committee responsibilities include1. Review logs and records for completeness and consistency with policy priorto filing.

2. Maintain awareness of processes and procedures used in the Laboratory andidentify departures from written procedures or good laboratory practice.

3. Recommend changes to procedures, policies, and processes to ensure andimprove Laboratory quality.

C. The Quality Committee functions independently within the Laboratory with referenceto quality process review.

1. When quality issues are identified that cannot be addressed through routinepolicies and procedures, the Quality Committee member should immediatelybring this to the attention of the Controlled Substances Supervisor, Lab Chief,and/or the Institute Quality Manager.

a) Disagreement regarding appropriate action will be referred to theExecutive Committee.

D. All Controlled Substances staff is expected1. To actively participate in quality processes as outlined in the Institute Quality

Manual and Laboratory Quality Manual.2. To run and evaluate appropriate QC as noted in analytical procedures.3. To participate actively with the Quality Committee to resolve noted issues and

to further quality processes in the Laboratory.

V. Reliability of Standards, Controls, and Critical Reagents:

A. Refer to the Controlled Substances Procedure Manual for specific informationregarding stability of standards, controls, and reagents.

B. In general, standards, controls, and critical reagents are considered acceptable for useas long as results meet assay acceptance criteria.

Dallas County Institute of Forensic Sciences 2 Quality ManagementControlled Substances Laboratory Version 2.2




VI. Use of Positive and Negative Controls

A. Positive quality control samples are run each day an assay is performed and evaluatedas outlined in each procedure.

1.

Results are summarized on the applicable GC or GC/MS Quality Control Log;the log and instrument output are filed in the applicable GC or GC/MSLogbook.

B. A negative control is run each day a GC or GC/MS is used.1. On a rotating basis, a procedural blank from one procedure is extracted and

analyzed by GC.a) Results are summarized on the applicable GC Quality Control Log; the

log and instrument output are filed in the applicable GC QC Logbook.b) On a weekly basis, rotate between sodium bicarbonate (NaHCO 3)

extract, sodium hydroxide (NaOH) extract, and ethanol (EtOH) withIS; prepare negative controls weekly.

(1) For example:(a) Week 1 – NaHCO 3 extract, name “NEGCTRL-

NaHCO 3”, use method METH.M(b) Week 2 – EtOH with IS, name “NEGCTRL-EtOH”,

use method HEROIN.M(c) Week 3 – NaOH extract, name “NEGCTRL-NaOH”,

use method METH.M2. Solvents used for GC/MS are analyzed as a negative control for GC/MS.

a) Results are summarized on the applicable GC/MS Quality ControlLog; the log and instrument output are filed in the applicable GC/MSQC Logbook.

(1) A fresh sample of solvent is analyzed.(a) Methylene chloride with internal standard, name

“NEGCTRL-MeCl 2”, use method NEGCTRL.M(b) Methanol, name “NEGCTRL-MeOH”, use method

DRUGANA.M3. An acceptable negative control contains no identifiable drug substance;

however, it may contain a solvent front and minor non-drug peaks. The GCchromatogram should not contain peaks with retention times near that of routinely tested drugs.

a) The mass spectrum for all non-solvent peaks on the GC/MS negativecontrol total ionization chromatogram must be evaluated by the analystto determine if a peak is drug related.

(1) If a peak is not drug related it will be lined through and initialedby the analyst.

(2) If a peak is drug related, troubleshooting will be conducted todetermine the source of the drug, and casework will not beperformed on that instrument until this issue is resolved.





b) If the GC chromatogram for the negative control contains non-solventpeaks, the negative control will be run by GC/MS to determinewhether the peak is drug related.

(1) If a peak is not drug related it will be lined through on the totalionization chromatogram, initialed by the analyst, and retained

with the GC negative control. (a) A recurring minor peak in the negative control(based upon retention time) needs to be run byGC/MS only once.

(2) If a peak is drug related, troubleshooting will be conducted todetermine the source of the drug, and casework will not beperformed on the applicable GC until this issue is resolved.

c) Troubleshooting peaks in the Negative Control (1) The analyst will advise a supervisor that peaks are present in a

negative control, whether peaks are drug or non-drug related, andoutline the steps that will be taken to evaluate the situation.

(a) Evaluation may include but is not limited to re-injecting the negative control, analyzing a newnegative control, performing instrument maintenanceand/or repair, etc.

(2) The supervisor and the analyst will - in all cases - evaluate thesample(s) analyzed immediately prior to a negative controlcontaining drug substance to determine whether these samplesshould be reevaluated and/or reanalyzed.

VII. Housekeeping:

A. Good housekeeping is the responsibility of Analysts, Evidence Registrars, and othersworking in the Controlled Substances Laboratory.

B. Areas to be cleaned are designated as Workstations 1- 5 for room 206 andWorkstations 1-4 for room 401 (refer to maps located on the Cleaning Checklistform).

1. These areas are sample prep areas used by the chemists.C. Additional areas that also require cleaning on a routine basis include: hoods, office

and designated clean areas, and around instrumentation and computers.D. Each week cleaning will be documented on the Drug Laboratory Cleaning Checklist.E. Routine Cleaning (not recorded on Cleaning Checklist)

1. After each exhibit or case is completed, the chemist is responsible for wipingdown his or her bench area with clean paper towels or kimwipes to remove anyresidue material from the previous exhibit or case.

2. If the bench paper is soiled, replace it.3. Wipe off balances, spatulas, scalpels after each exhibit or case.

F. Daily Cleaning (not recorded on Cleaning Checklist)1. Put away glassware2. Put away reagents3. Discard extraction tubes and autosampler vials as needed





G. Weekly Cleaning (recorded on Cleaning Checklist)1. Clean workstation thoroughly2. Re-stock supply drawers3. Check reagent levels4. Dust or vacuum around instruments and computers

5.

Clean hoods6. Clean office or designated clean area7. Check the biohazard boxes, they should not exceed 20 lbs. (~3/4 full)8. Check chemical waste bottles, contact Deputy EHS manager for disposal

H. 3. Monthly Cleaning (recorded on Cleaning Checklist)1. Vacuum behind instruments

VIII. Testing Validation:

A. Validation and verification of new testing methods is summarized in the QualityManual.

B.

The Supervisor and/or Section Chief will typically design a specific testing protocolto validate the accuracy of a new method or to verify the accuracy of a methodtransferred from one instrument to another.

1. Transfer of a Method to New Instrumentationa) Proper calibration and operation of new instrumentation are verified

and documented using the applicable instrument calibration process.b) Analytical results are compared between the new and old

instrumentation.(1) Where possible, side by side operation of old and new

instrumentation is compared using the same samples or extracts.c) Standards, internal standards, and quality control samples should meet

their respective criteria described in the analytical procedure.d) Test specimens should also be run and should meet acceptability

criteria established for quality control samples or similar proficiencytest results.

e) Replicate analytical runs should be made on a single day and alsocompared between multiple days; criteria should meet thoseestablished for standards, internal standards, and quality controls; testspecimens should meet acceptability criteria established for qualitycontrol samples or similar proficiency test results.

f) As applicable, analysts are trained in operation of newinstrumentation.

2. Development of a New Analytical Methoda) A new analytical method may be proposed based upon literature, other

established procedures, or knowledge and experience of the materialsto be analyzed.

b) The target sensitivity and linear range is established based uponexpected sample conditions and instrument performance.

c) Standard curves are run to assess the applicability of the proposedanalytical technique in comparison to the targeted analytical needs.






d) A formal procedure is written.e) The method is evaluated for interference from expected matrices or co-

occurring substances.f) The method is evaluated for stability by repeating analysis of single

prepared samples and duplicate preparation of samples both within day

and between day.g) Variability of standards, internal standards, quality control samples,and specimens are evaluated with respect to literature values and/orsimilar established procedures.

h) Criteria for acceptable standard curves, internal standards, and/orquality control samples are established.

i) The method is revised and revalidated as necessary. j) Applicable analysts are trained, and results are reviewed for stability

within analyst.k) Method results may be evaluated against external standards or

specimen results from reference laboratories; criteria for acceptability

will be similar to that established for quality control samples.




ABBREVIATIONS LIST

The following is a list of abbreviations used in the Drug Laboratory section. The abbreviations

can be used in any combination of upper and lower case with or without periods. Common chemical

abbreviations are equally acceptable and are not listed here.

Word or phrase Abbreviation6-monoacetylmorphine mamalprazolam alpzamount amtblank blkclear clrdeionized water DI H2Odilution dildo not report DNRevidence evid

exhibit exforensic laboratory number FL#gross weight gwtInstitute of Forensic Sciences ifsinternal standard I.S.large lgliquid liqlysergic acid diethylamide lsdmarihuana mjmaterial matmethamphetamine methmiscellaneous miscnet weight net wtno controlled substance NCSno reaction NRpetroleum ether pet etherPhysicican's Desk Reference PDRpowder pwdrprecipitate pptquality control qcresidue resretention time rtsealed cardboard box scbsmall smstandard std

syringe syrunknown unkvolume volweight wtwith w/, c (with a line over it)without w/o

Dallas County Institute of Forensic SciencesControlled Substances Laboratory 1

AbbreviationsVerion 2.0

This is a non-controlled copy of a controlled document



Drug and Procedure Cross Reference

Drug Procedureacetaminophen acidic

alprazolam direct dilution

amphetamine alkaline

barbituates acidic

boldenone miscellaneous materials

caffeine acidic

carisoprodol acidic

chlordiazepoxide weak alkaline

clonazepam direct dilution

cocaine weak alkaline

codeine alkalinediazepam direct dilution

diethylpropion alkaline

ethchlorvinyl acidic

ethosuximide acidic

fenfluramine alkaline

flurazepam direct dilution

ghb miscellaneous materials

heroin direct dilution

hydrocodone alkalinehydromorphone weak alkaline

ibuprofen acidic

ketamine weak alkaline

lorazepam direct dilution

lsd lsd

MDA alkaline

MDEA alkaline

MDMA alkaline

meperidine alkaline

meprobamate acidic

methamphetamine alkaline

monoacetylmorphine direct dilution

morphine weak alkaline/direct dilution

mushrooms/cactus buttons miscellaneous materials

Dallas County Institute of Forensic SciencesControlled Substances Manual 1

Drug and Procedure Cross ReferenceVersion 2.0




nandrolone miscellaneous materials

olanzapine direct dilution

oxandrolone miscellaneous materials

oxazepam direct dilution

oxycodone alkalineoxymetholone miscellaneous materials

phencylidine weak alkaline

phendimetrazine alkaline

phentermine alkaline

prazepam direct dilution

propoxyphene alkaline

salicylates acidic

stanolone miscellaneous materials

stanozolol miscellaneous materials

temazepam direct dilution

testosterone miscellaneous materials

thc marihuana

theophylline acidic

tiazolam direct dilution

valproic acid acidic

Dallas County Institute of Forensic SciencesControlled Substances Manual 2

Drug and Procedure Cross ReferenceVersion 2.0




Dallas County Institute of Forensic SciencesControlled Substances Procedure Manual

Summary of Changes from Previous Manual Version

Previous Version: Controlled Substances Procedure Manual, version 1.0Current Version: Controlled Substances Procedure Manual, version 2.x

1. All procedure versions were changed consistent with the move to electronic format andtypographical corrections were made where applicable.

2. No other substantive changes were made to the following sections: Purpose, Drug LIMS,and Testimony.

3. Evidence Management – A section has been added regarding evidence security andprocess was clarified as needed.

4. Analysis and Reporting of Casework – Previous changes by memo were incorporatedinto the procedure, a summary regarding analyst handling of evidence was added, and

process was clarified as applicable.5. Quality Management – This section was expanded to address additional quality issuesincluding establishment of a Quality Committee, critical reagents, housekeeping, andcase review.

6. The Abbreviations and Drug and Procedure Cross Reference administrative sections arenew to this manual.

7. The following procedures have been reorganized to improve utilization with minorupdates as needed: Acetylated Derivatives, Acidic Drug Analysis, Alkaline DrugAnalysis, Cocaine Direct Dilution, Direct Dilution, IR Procedure, LSD, Marihuana, andWeak Alkaline Drug Analysis.

8. Color Testing – A quality control documentation section was added, minor updates andreorganization were performed.

9. Miscellaneous Materials – More specific information regarding testing of GHB andmushrooms is provided, the section on clandestine laboratories has been moved to theAlkaline Drug Analysis procedure, and Morphine Syrup was moved to a standaloneprocedure and upgraded.

10. Offsite Sampling, Pharmaceutical Analysis, and Unknown Sample Screening are newlycreated procedures detailing current process covered in other procedures or practices.

11. Cocaine Free Base procedure was removed; it is covered in the Cocaine Direct Dilutionprocedure.

Dallas County Institute of Forensic Sciences 1 Changes from Previous VersionControlled Substances Laboratory Version 2.0




Controlled Substances Procedure Manual Version 2.xRevisions and Corrections

EffectiveDate

Description Authorizedby

2/28/08 Quality Management: addition of Section VI. Use of Positive andNegative Controls (version 2.1) ELT

4/9/08 Revision of Quality Management, Section VI. Use of Positive andNegative Controls to improve instruction. (version 2.2)

ELT

2/26/09 Color Testing: color test results for BZP and TFMPP were added.(version 2.1)

ELT

2/26/09 Miscellaneous Materials: GHB Section 2.d.iv was revised to clarifyinstructions. (version 2.1)

ELT

2/26/09 Pharmaceutical Analysis, Visual Identification Sections 1.b and 1.dwere revised to describe procedures for single or partial items.(version 2.1)

ELT

2/26/09 Analysis and Reporting of Casework: Section L.2 and L.3 wasrevised to reflect current policy for naming resubmittal and amendedreports. (version 2.1)

ELT

2/26/09 Direct Dilution: A typographical error on the molecular weight of heroin was corrected in the training notes. (version 2.1)

ELT

2/26/09 Morphine Syrup Analysis: A typographical error on the molecularweight of morphine was corrected in the training notes. (version 2.1)

ELT

2/26/09 LSD Analysis: A typographical error on the units (mg/mL) underLSD/LAMPA Standard was corrected. (version 2.1)

ELT

2/26/09 Weak Alkaline Drug Analysis: Processing of PCP on cigarettes wasclarified, and a typographical error in the solvent name was corrected

in the Analysis of Cocaine in Oil procedure. (version 2.1)

ELT

2/26/09 Remove IR Procedure, Version 2.0 and replace with FTIR, Version2.0.

ELT

Dallas County Institute of Forensic Sciences 1 Revisions and CorrectionsControlled Substances Laboratory Version 2.3




Dallas County Institute of Forensic Sciences Statement of PurposeControlled Substances Laboratory Version 2.0

STATEMENT OF PURPOSE

The Dallas County Forensic Laboratory is a division of the Dallas County Southwestern Instituteof Forensic Sciences. It is an independent laboratory established through joint agreement of theDallas County Commissioners Court and UT-Southwestern Medical School. The Laboratory isnot a part of any police agency, the Dallas County District Attorney’s Office, nor the DallasCounty Sheriff’s Office. The Laboratory operates on a fee-for-services basis, and its services areavailable to anyone paying the fees prescribed by the Dallas County Commissioners Courtwithin the policies and procedures established by the Commissioners Court and the Director of the Institute.

The purpose of the Drug Analysis Section of the Dallas County Institute of Forensic Sciences isas follows:

1. To analyze materials controlled by the Texas Drug Laws - including but not limited tothe Texas Controlled Substances Act, Simulated Controlled Substances, DangerousDrugs, Volatile Chemicals, Abused Glues, and Aerosol Paints (Chapters 481 - 485 of the Texas Health and Safety Code) - and the Federal Controlled Substances Act;

2. To testify in court proceedings regarding testing results, methods of analysis, and thegeneral effects of material submitted to the laboratory;

3. To assist submitters in the identification of drug substances, raw materials, andprecursors in the manufacture of these substances and adulterants and dilutants whichmay be present in the final product.

The purpose of this manual is to outline the activities conducted by this Laboratory and toprovide an overview of sample analysis strategy. Because of the unique nature of many of thesamples submitted to this Laboratory, exact analytical procedures cannot be prescribed for everycase. Therefore, analytical techniques described in this manual are given as guidance, and theactual choice of analytical methodologies will be left to the discretion of the Drug Analyst,Supervisor, and/or Section Chief. All variances from these procedures, however, will bedescribed in the case record. It is the goal of this laboratory to perform analyses conforming toaccepted standards of laboratory practice.

OVERVIEW OF LABORATORY ACTIVITIES

Samples are usually received into the laboratory by the Evidence Registrar. A unique laboratorynumber is assigned to each case. Evidence is stored in a sealed condition until it is opened by ananalyst. During analysis evidence is stored in the evidence vault, in the personal possession of the analyst, or in the analyst’s personal locked storage area. The analytical process includesdescription, weighing, analysis, and reporting of evidence. Cases are reviewed by a supervisor,and a report sent to the submitting agency. Evidence is resealed and stored in a secure area untilit is returned to the submitting agency. Testimony regarding work performed and general drugtoxicology is provided as applicable.




Drug Analysis Laboratory

EVIDENCE MANAGEMENT:Evidence Security; Receipt and Release of Drug Evidence; Records Management

I.

Evidence SecurityA. Because of the inherent value of drug evidence and criminal penalties related topossession of controlled substances, all Drug Laboratory staff must at all times bevigilant about protecting drug substances in the custody of the Institute.

B. Staff must remain actively engaged during the processing and handling of drugmaterials and maintain a critical perspective about their own actions, the actions of coworkers, and the actions of others in the Laboratory or at the Institute as it relates toprotecting controlled substances, processing intermediates, and analytical residues.

C. It is the responsibility of all staff to immediately advise a supervisor of suspectedmisuse or loss of suspected or known controlled substances or breaches in security orprocedures that may lead to misuse or loss of suspected or known controlled

substances. D. Staff actions that compromise the security of controlled substances in the possessionof this Laboratory will be investigated internally and externally by law enforcementagencies as appropriate.

E. Staff is subject to disciplinary action up to and including termination1. for failure to maintain care, custody, and control of known or suspected

controlled substances in their possession 2. for misuse or loss of a known or suspected controlled substances3. for failing to advise a supervisor of known or suspected loss or misuse of

known or suspected controlled substances or breaches in security or procedurethat may lead to their loss or misuse

4. for failing to cooperate with investigations F. As provided for by law, staff is also subject to criminal investigation and prosecution

in regard to mis-handling of controlled substances.G. Drug Laboratory Security

1. Drug Vault – Routine access to the drug vault is limited by access cardauthorization to the Drug Evidence Registrars and the Drug LaboratorySupervisor.

2. Drug Laboratory – Routine access to other Drug Lab areas is limited byaccess card to authorized staff only: Drug Evidence Registrars, Drug ChemistsII and III, Drug Lab Supervisor, and Section Chief.

3. Only authorized staff has unescorted access to the Drug Lab areas.a) Other visitors – including cleaning crews, instrument vendors, Institute

staff from other labs, etc. - must be escorted at all times. (1) The person allowing entrance to a visitor is responsible for

visually monitoring the activity of the visitor until the visitor ishanded over to another authorized staff member or escorted outof the secure area.

4. Drug Lab areas are controlled by intrusion alarms, access cards, and keylocks.

Dallas County Institute of Forensic Sciences 1 Evidence RegistrationControlled Substances Laboratory Version 2.0




a) The last person out of a Drug Lab area is responsible for key-lockingthe door at any time of the day.

b) The last person out of a Drug Lab area at the close of business isresponsible for setting the security alarm.

c) All staff are responsible for using the security check list located in

each Drug Lab area to monitor the status of security and evidence inthe area. H. Evidence Security

1. Drug evidence should routinely be in the personal possession of authorizedpersonnel, a locked storage locker, or vault.

a) Large or bulky evidence may be left in the secure laboratory duringanalysis if a locked storage area is not available or practical.

2. Staff should work in a manner to ensure that evidence remains within theircustody while in their possession and is not lost or contaminated.

a) Trash cans should not be placed directly under a work area. 3. Personal storage areas should be kept neat and orderly; evidence should be

returned to Evidence Registration in a timely manner. a) Staff must advise a supervisor if evidence remains in their personalstorage area for more than one month.

I. Evidence Accountability 1. Accountability: Staff is accountable for evidence, processing intermediates,

analytical residues, and standards for the entire time that these items remainthe responsibility of the Institute.

a) Evidence may leave the Institute only by approved processes: (1) Evidence is generally released to the submitter (chain of

custody required) (2) With the permission of the submitter, evidence may be released

to destruction using a method approved by InstituteAdministration (chain of custody required)

(3) Medical Examiner pharmaceuticals are released to destruction(chain of custody required)

(4) Proficiency test materials, old training materials, unusedstandards, and other drug materials of a useable quantity mustbe released to destruction using a method approved by InstituteAdministration (chain of custody required)

(5) De minimus quantities of processing intermediates andanalytical residues may be disposed

(a) in biohazard waste (b) as a residue in glass waste

(6) Evidence may be released upon direction of the submitter or inresponse to court order, subpoena, or other legal direction.

b) Use of drug materials, processing intermediates, or analytical residuesoutside standard operating procedure requires supervisory approvalwith transfer using chain of custody and tracking of use by asupervisor.

2. Use of evidence material for training or testing purposes:





a) With the permission of a submitting agency, drug evidence may beretained for training and testing purposes.

(1) A description of retained items must be placed into the case fileand signed by the analyst and a supervisor.

(2) Items retained must be stored in the Drug Vault and

inventoried by the Drug Lab Supervisor. II. Receipt and Release of Drug EvidenceA. General Information

1. General management of evidence is described in the Evidence Handlingsection of the Quality Management Program.

a) Additional information specific to the Drug Analysis Laboratory isdescribed in this section.

2. Duties described in this section will usually be performed by a DrugLaboratory Evidence Registrar or the Drug Lab Supervisor but may beperformed by other designated Drug Lab staff.

a) The term “Evidence Registrar” will encompass all of the above named

entities and the drug vault for the purposes of this document.3. All Drug Laboratory staff may receive evidence in the event that an EvidenceRegistrar is not available.

a) Staff will follow proper evidence receipt procedures and maintainevidence in a secure location until it can be released to an EvidenceRegistrar.

b) Only designated individuals with routine evidence registrationresponsibilities will have access to the drug vault.

4. Responsibilities of the individual receiving the evidence include completingthe chain of custody form, obtaining proper and legible submitter/billinginformation, assessing the status of evidence seals, and ensuring that theevidence package is properly sealed, as applicable, and stored in a securelocation.

a) Evidence logging may occur at a later date.B. Evidence Seals

1. To the extent feasible, evidence received by the Drug Analysis Laboratoryshould be properly sealed prior to receipt.

a) A container is properly sealed when it is secured in a permanentmanner to prevent undetected access to the contents and when itscontents cannot readily escape.

b) The seal must be marked with an identifying mark such as the initialsof the person sealing the evidence.

c) The Evidence Registrar will assess the status of the seal at the time of evidence receipt.

(1) Where possible, evidence should be sealed by the submittingagency prior to receipt by the Evidence Registrar.

(a) The Evidence Registrar should instruct the submittingagency to repackage and/or reseal prior to submission.

(2) In any case, it is the responsibility of the Evidence Registrar toensure that evidence is properly sealed upon receipt and to





repackage and/or seal evidence as necessary prior to storage inthe vault.

(a) When the Evidence Registrar must reseal submittedevidence, initials and date should be placed on thereinforced seal.

2.

It is unusual that evidence received by the Drug Laboratory is of the size ornature that it cannot be properly sealed. However, under these conditionsalternate methods may be used.

a) Evidence should be transferred as soon as possible to the analyst forprocessing.

b) Evidence may be stored in a hood using a unique lock/key, or if noother option is available, evidence may be placed in the drug evidencevault.

c) Where possible, evidence should be properly sealed followinganalysis.

(1) If this is not feasible, evidence should be returned to the

submitting agency as soon as possible.3. Evidence is not required to be sealed during analysis as long as it ismaintained in a secure area with limited access.

C. Chain of Custody1. All evidence transfers – external and internal - will be documented using the

Evidence Summary form and Drug LIMS.a) Chain of custody records must be executed at the time of evidence

transfer.b) For details of this procedure refer to the chapter, “Drug Laboratory

Information Management System,” in this manual.2. Evidence transfer must include legible documentation of the following:

a) Name, signature, and affiliation of individual(s) receiving andreleasing evidence

(1) For Institute staff, initials or electronic identifier are acceptablein place of the signature, and affiliation is not necessary.

(2) Signature only is acceptable for routine submitters whoseprinted name and signature are maintained in an annualsignature log by the Evidence Registrar.

b) Method of shipment if applicable(1) Shipping papers and/or tracking numbers, such as certified

mail number, should be noted in the case file.c) Date and time of evidence transfer (time and date stamp may be used)d) General description of evidence transferred if the entire case is not

transferrede) Status of specimen sealf) Case name and/or Institute case number; agency case number as

applicableD. Evidence Receipt





1. All evidence received into the Laboratory should be accompanied by a legibletransmittal sheet and/or an Institute Evidence Summary form which includesthe following information as applicable:

a) Submitting agency name and contact name(1) Complete address and phone are required if the submitter is not

a regular client.b) Billing agency name, billing address, billing contact, and phone if billing information differs from submitter information

c) Case named) Submitting agency case numbere) Officer badge number as applicablef) Analysis requested as applicableg) General description of evidence submitted

2. In-person transfera) The submitting agent(s) will transfer custody of evidence to the

Evidence Registrar by executing the chain of custody.

b)

The Evidence Registrar will accept evidence by completing the chainof custody.(1) At this time, the Evidence Registrar will compare the

transmittal sheet or evidence submission form with theevidence for correct name, service number, and arrest date andinspect the condition of the evidence seal.

(2) Questions regarding evidence and paperwork will be resolvedat this time.

3. Lockbox transfera) The Evidence Registrar may receive evidence directly from a lockbox.

(1) At this time, the Evidence Registrar will compare thetransmittal sheet or evidence submission form with theevidence for correct name, service number, and arrest date andinspect the condition of the evidence seal.

(2) Questions regarding evidence and paperwork will be resolvedas soon as possible and referred to a supervisor as needed.

4. Evidence remains in the custody of the Evidence Registrar until it is releasedfor analysis.

E. Evidence Tracking1. Location and possession of evidence will be tracked throughout the storage

and analysis process.a) For details of this procedure refer to the chapter “Drug Laboratory

Information Management System” in this manual.F. Case Completion and Release

1. A case is complete when a Supervisor, Section Chief, or other reviewer signsthe case report.

a) Computerized case records should also be updated as appropriate.b) The analyst will return the signed report and the sealed evidence to the

Evidence Registrar using proper chain of custody: Evidence Summaryform and Drug LIMS.





c) Evidence will be stored in the Drug Evidence Vault until release.2. Evidence is available for return to the submitter when the final report has been

completed and signed.a) The Evidence Registrar is responsible for notifying a submitter that

evidence is available for release.

3.

To release evidence, the Evidence Registrar completes the external chain of custody on the Evidence Summary form.a) The name of the individual receiving the evidence, the date, and time

of transfer are noted on the Evidence Summary form.b) If the identity of the individual receiving evidence is unknown to Drug

Laboratory staff, identification must be requested and verified.c) Computerized case records should also be updated as appropriate.

4. Evidence may be released only to the submitting agency or to an entityapproved by the submitting agency or in response to and in compliance with asubpoena, court order, or other legal direction.

a) Evidence is usually released to the submitter; release to another entity

requires supporting documentation in the case file.b) Evidence may be returned by mail or package delivery with propernotation made in the case file.

5. Controlled substances may not be released to submitters who do not haveauthorization to possess controlled substances.

a) Disposition of these items will be arranged with the submitter on acase by case basis and may include storage by IFS, disposal, transfer toa properly designated agent, etc.

6. If the submitting agency has not arranged for disposition of evidence within90 days of case completion, the Evidence Registrar may contact the submitterin writing requesting that the submitter collect evidence within 30 days orprovide IFS approval for evidence destruction.

a) If evidence remains after this 30 day period, it may be returned to thesubmitting agency by mail or package service, and the submitter billedthe applicable shipping fee.

III. Records Management A. Records management and release is described in the “Control and Maintenance of

Case Record Documentation” and “Disclosure of Information” sections of the QualityManagement Program.

1. Specific Drug Laboratory information is provided here.B. Primary Custodians of Records for the Drug Analysis Laboratory include the

Evidence Registrar, Drug Chemist III, Laboratory Supervisor, and Section Chief.C. Drug Chemist II are Custodians of Records for case which they analyzed.D. The Evidence Registrar manages records on a daily basis and provides copies of

reports as appropriate.E. The Evidence Registrar oversees transfer of case files to off-site storage.F. Copies of case reports are provided to the submitting agency and as applicable to

other investigative or prosecuting entities.G. Distribution of case reports will be documented in the case file.





Dallas County Institute of Forensic Sciences 1 ME Pharmaceutical & Drug Evidence Controlled Substances Laboratory Version 2.0

STORAGE, TESTING, AND DESTRUCTION OF MEDICAL EXAMINERPHARMACEUTICALS AND DRUGS

Pharmaceutical and drug evidence collected or received by the Dallas County Office of theMedical Examiner (OME) is submitted to Drug Evidence Registration for storage anddestruction. In some cases, the Controlled Substances Laboratory will perform testing on thisevidence at the request of Medical Examiner staff.

Additional information regarding the submission of drug evidence may be found in the EvidenceRegistration section of the Controlled Substances Procedure Manual.

I. Submission of Medical Examiner Drug Evidence to Drug Evidence Registration

A. Submission Using the Field Agent Lockbox

• Field Agents will deposit properly sealed evidence in the Field Agent DrugLockbox.

• Evidence must be submitted in tamper evident plastic bags or other containerswith the Field Agent’s initials across any non-factory seals.

• A case barcode will be placed on the evidence bag. If more than one bag issubmitted, the Field Agent will write the case number and case name on eachadditional bag.

• A Medical Examiner Drug Submission form must be completed and submittedwith each case submitted.

• Each case submission to the Field Agent Drug Lockbox must be documentedon the Medication Drop Log.

B. Submission Directly to the Drug Lab

• Evidence which requires testing is often submitted directly to Drug EvidenceRegistration by the Office of the Medical Examiner.

• In accepting Medical Examiner evidence for testing, the Drug EvidenceRegistrar accepts evidence on behalf of both the Medical Examiner’s Office(as it relates to this current policy of storage and destruction) and the DrugLaboratory (as it relates to testing).

• A Medical Examiner or Field Agent may contact a Drug Evidence Registrar torequest analysis of evidence previously submitted.

II. Management of Medical Examiner Drug Evidence

A. The Drug Evidence Registrar ensures that all Medical Examiner drug evidencehas a proper evidence submission form and is properly sealed.

B. The Registrar enters evidence into the Medical Examiner drug evidence trackingsystem and store evidence in a secure location.

C. The Registrar may release drug evidence to a Field Agent upon request withcompletion of appropriate chain of custody. Evidence may be returned to theDrug Evidence Registrar in person or dropped into the Field Agent Drug Lockboxby the Field Agent returning the drug evidence. The Registrar will complete the





chain of custody as appropriate. It is expected that the Field Agent will returndrug evidence in a timely fashion; variance should be brought to the attention of aSupervisor.

D. Release of evidence to other than a Field Agent or Medical Examiner requireswritten permission of the Chief/Deputy Chief Field Agent or Chief/Deputy Chief Medical Examiner. Chain of custody will be documented in the appropriate casefile.

III. Retention of Medical Examiner Drug Evidence after Case Completion

A. Medical Examiner Drug Evidence will be held for at least 90 days post collection.B. Evidence will be considered for destruction upon case completion or 90 days post

collection whichever is later.C. Requests to retain drug evidence beyond the period noted above must be

submitted in writing to the Chief of Forensic Chemistry by the individualrequesting evidence retention and conform to the requirements noted in theMedical Examiner Drug Evidence Disposal and Hold Policy (refer to Appendix).

D. On their own behalf, Institute staff may request retention of Medical Examiner

drug evidence beyond the routine retention period by sending a written request tothe Chief of Forensic Chemistry identifying the following:

Case NumberDecedentRequestor NameReason for HoldLength of HoldDate of Hold Request

III. Disposal of Medical Examiner Drug Evidence

A. Medical Examiner Property

1. As needed, Medical Examiner drug evidence which exceeds 90 days fromcollection, is not held for Medical Examiner evidentiary purposes, or heldper the Medical Examiner Drug Evidence Disposal and Hold Policy willbe disposed.

2. The Drug Evidence Registrar will prepare a list of cases for destruction.3. Cases designated for disposal will be placed into a disposal container,

sealed, witnessed by two IFS staff, one of which should be a DrugEvidence Registrar. Cases included in each disposal box will be noted, the

box will be sealed, and the seal initialed by both staff. The box is deemedready for destruction provided the seal remains intact. This process mustbe repeated if the seal is broken for example to add or remove a case.





B. Forensic Laboratory Property

1. Certain drug materials collected by the Institute Forensic Laboratoryincluding but not limited to drug materials remaining from analyticalprocedures, drug standards, and drug materials not retrieved by submittingagencies will be identified for disposal.

2. These materials will be placed into a disposal container and the contentswitnessed by two Institute staff, one of which should be a Drug EvidenceRegistrar. Contents of the box will be noted, the box sealed, and the sealinitialed by both staff. This process must be repeated if the seal is broken.

C. Order for Destruction

An Order for Destruction (refer to Appendix) listing the cases and/or drugmaterials to be disposed will be submitted to the Chief Medical Examiner, whopresides over the Court of Inquest, for signature and authorization to dispose.

D. Disposal Regulations and Policies

1. Possession and disposal of drug substances are regulated by the DrugEnforcement Agency (DEA), the Texas Commission of EnvironmentalQuality (TCEQ), and the Environmental Protection Agency (EPA).Disposal facilities may also have policies and procedures which must befollowed.

2. An appropriate disposal facility will be selected by InstituteAdministration and Purchasing.

3. Specific arrangements must be made with the disposal facility prior toeach destruction.

4. Only finished drug substances (including plant material) may be sent tothe disposal facility. Specific arrangements must be made for disposal of clandestine laboratory chemicals, aerosol cans, or other types of waste.

5. Institute staff or other entity designated by the Chief Medical Examinermust retain custody of drug evidence until actual physical destruction atthe disposal facility; this is called a “witnessed burn.”

6. A certified peace officer or DEA licensee must also accompany Instituteevidence to the disposal facility.

7. Disposal is documented on a manifest and/or other certificate of destruction. The destruction records must be signed by two individuals onbehalf of the Institute.

IV. Retention of Records

The following records will be retained on the same schedule as other Medical Examinerrecords: the original Order of Destruction, inventory of cases/materials disposed, originalmanifest or certificates of destruction, Medical Examiner Drug Submission forms, andother relevant materials related to the destruction.




SOUTHWESTERN

TELEPHONE: 214-920-5990FAX: 214-920-5812INSTITUTE OF FORENSIC SCIENCES

AT DALLAS5230 Medical Center Drive

Dallas, Texas 75235

MEDICAL EXAMINER DRUG EVIDENCE DISPOSAL AND HOLD POLICY

Medical Examiner drug evidence is authorized for disposal upon case completion or 90days post collection whichever is later unless an interested party acts as described below:

Storage of Medical Examiner drug evidence beyond the standard storage period notedabove requires specific action on the part of the agency/individual requesting thatspecimens be held. Medical Examiner drug evidence may be held for one year incrementsprovided all of the following conditions are met prior to 90 days from sample receipt by theInstiute in year one or prior to the anniversary date of evidence receipt by the Institute forevidence held per this policy beyond one year):

A. The Chief of Forensic Chemistry must receive a written request from theagency/individual requesting that drug evidence is retained for one or one additional year.This written notice must include the case name; the Medical Examiner case number; thename, phone number, and complete mailing address of the agency/individual requestingspecimen hold; and a description of the materials to hold, AND

B. The Chief must be in receipt of a check for the amount of the Annual Specimen StorageFee authorized by the Dallas County Commissioners Court. The check must be madepayable to Dallas County and reference the case name and/or case number, AND

C. It is the responsibility of the agency/individual requesting evidence hold to renewthe annual evidence hold prior to the anniversary date of evidence receipt at theInstitute. Otherwise samples will be disposed per Institute policy. The Institute willnot provide annual notice of this requirement to renew the sample hold request andprovide payment, AND

D. Dallas County reserves the right to change this policy at any time. Reasonable effort willbe made to notify the agency/individual requesting the evidence hold; however, noguarantee is made in this regard. It is the responsibility of the agency/individualrequesting evidence hold to keep the Institute advised of address changes, etc.

All correspondence and payment to Dallas County must be sent to the Chief of ForensicChemistry, Dallas County Institute of Forensic Sciences, 5230 Medical Center Drive, Dallas, TX75235. All correspondence and payment must be received prior to the routine destruction date oranniversary date of evidence receipt at the Institute.

This policy pertains to retention of drug evidence only and does not guarantee evidence release. Release of evidence requires approval of the Chief Medical Examiner, submitting agency, and/or proper legal authority. In addition, the entity or individual requesting release






must provide proper authorization to possess drug materials as applicable, for example a DEA number. Additional fees related to evidence release are the responsibility of the requestor.





OVERVIEW OF ANALYSIS AND REPORTING OF CASEWORK

The following provides guidance regarding analysis and reporting of suspected drug evidence.

Analysts should consult with supervisors as needed in the implementation of this guidance.Variance from written procedure must be documented in the case and reviewed and approved by asupervisor.

I. Internal Chain of CustodyA. The internal chain of custody begins when the analyst takes possession of cases from the

Evidence Registrar.B. All internal transfers of evidence are documented on the internal chain of custody section

of the Evidence Summary form which is the official chain of custody record.1. Internal transfers will also be recorded as applicable in Drug LIMS to facilitate

administrative tracking of evidence.

C. When evidence is transferred from one analyst to another, the evidence may be sealed ortransferred in person unsealed.

1. If evidence is transferred in person unsealed, both analysts must verify theinventory at the time of transfer and document this by initialing and dating theinventory log.

II. Sealing of EvidenceA. Evidence remains sealed until it is processed, i.e. inventoried, weighed, sampled, etc.

1. Only one case is processed at a time.2. Evidence is resealed at completion of processing.

B. Immediately prior to sealing the evidence container, the analyst will verify the presenceof all items listed on the inventory which are not otherwise accounted for in the case file,

for example materials used in analysis.1. All exhibits will be placed into the evidence bag with any additional residue

tubes if applicable.2. Any additional items included will be marked “added by lab”, “lab bag”, etc.3. The analyst will document concurrence with the inventory by writing “sealed”,

initials, and date in the upper left portion of the transmittal sheet.C. All evidence will be sealed in a secure, tamper evident manner.

1. The seal must be initialed and dated by the analyst sealing the evidence.2. In the specific case of a heat sealed evidence bag, the analyst will initial and date

the inside of the bag along the cut area and heat seal the bag through the initialand date.

D. The internal chain of custody form will be completed as the sealed evidence is releasedfrom the custody of the analyst to the Evidence Registrar; this transfer will also bedocumented for administrative purposes using the evidence transfer function of DrugLIMS.

E. If evidence is reopened at another time, the inventory will be verified against the originalinventory taking into consideration materials accounted for otherwise in the case file.

1. Concurrence with the inventory will be documented by writing “reopened”,initials, and date in the upper left portion of the transmittal sheet.

Dallas County Institute of Forensic Sciences Analysis and Reporting of CaseworkControlled Substances Laboratory 1 Version 2.1



2. Immediately prior to resealing the evidence container, the analyst will verify thepresence of all items listed on the inventory which are not otherwise accountedfor in the case file. The analyst will document concurrence with the inventory bywriting “sealed”, initials, and date in the upper left portion of the transmittalsheet.

F. Exit Weight of Primary Containers1. The sealed evidence container will be weighed at the time the container is sealedand the weight entered in the case file as exit weight.

2. If evidence is reopened, the process will be repeated with the new entranceweight and exit weight noted in the case file.

3. It is the responsibility of the analyst and case reviewer to include evaluation of entrance and exit weights as a part of routine case review.

III. Inspection and Weighing of Primary Evidence ContainersA. The analyst will inspect the evidence container to determine if it is sealed.

1. If the evidence container is sealed, the analyst will indicate this by writing“sealed” and/or initialing on the evidence container.

2. The analyst will also note that the evidence was sealed by indicating sealed onthe internal chain of custody.B. The analyst will weigh the sealed primary evidence container(s) to determine the

submission weight.1. The weight is entered on the Evidence Summary form.2. The balance identification number is also recorded.3. In the case of multiple primary evidence containers, each container will be

weighed separately.4. Primary container weights will be compared to the agency submission weight.

a) Significant variation will be witnessed by a second chemist andimmediately brought to the attention of the supervisor who will

determine whether to suspend analysis pending notification of thesubmitter.

C. The analyst will open the evidence.1. To open evidence in a heat sealed bag, the analyst will cut the factory seal (if

present), write the case number and initials on the cut strip, and place the stripinto the evidence bag.

2. As possible, evidence will be opened in a manner which leaves the original sealspresent.

D. The analyst will then inventory the evidence.IV. Inventory and Marking of Evidence

A. The analyst is responsible for making an inventory of all submitted evidence.

1. Upon opening the primary evidence container, the analyst will document thecontents of the evidence on the Evidence Summary form.

2. The analyst will compare the submitting agency’s inventory to the contents of theopened evidence.

a) Any variation in the agency’s inventory, such as addition or deletion of suspected drug evidence and item count discrepancies, will beimmediately witnessed and verified by another analyst who will alsoinitial and date the inventory description.




(1) The primary analyst will also immediately notify a supervisorwho will determine if the submitting agency should be notified.

B. Identifying Evidence1. Each case is assigned a unique case number by the Evidence Registrar.2. The analyst will usually determine exhibit numbers.

a) “Like populations” within a case will be grouped into exhibits. Likepopulations are pieces of evidence of similar size, packaging, and/orgeneral appearance.

b) Evidence will be identified on worksheets and on the report by the casenumber and an exhibit number.

c) The exhibit number will be a combination of letters and numbers asfollows:

(1) The primary evidence containers will be identified as Exhibit 1,2, 3, etc. (Ex. 1).

(2) Like populations of evidence inside the outer evidence containerwill be grouped together and identified by a number and letter.

(a) For example, Ex. 1A will include all similar evidencefound inside the outer container.(b) Ex. 1B will include a second type of evidence found

inside the outer container.(c) Loose substance found inside the evidence bag will

generally be considered one exhibit and identified by anumber and letter, for example, Ex. 1C.

d) If there is more than one item in each population described above, theexhibits actually analyzed will be further identified by a number.

(1) For example, Ex. 1A1 and Ex. 1A2 represent two pieces of evidence from evidence group 1A which were analyzed.

e) Where possible, the submitting agency’s item numbers will be used if they fit the above format. If the submitting agency’s item numbers arenot consistent with the above scheme, then the analyst will usuallyidentify evidence using the above scheme and will note the submittingagency’s corresponding evidence numbers in parenthesis on thetransmittal sheet and on the report, for example, Ex. 1A1 (Item 4).

3. Each piece of evidence will be labeled with the unique case number.a) If the evidence cannot be labeled, the proximal container must be marked

with the case number.4. Pieces of evidence which are analyzed should be marked with the case number,

exhibit number, and analyst’s initials.

a) It must be clear from the case record or evidence labeling which evidencereceived what testing.

b) If the evidence cannot be marked, the information must be placed on theproximal container.

5. If the proximal container was added by the laboratory, it should be so markedand noted.

V. Analytical ProtocolsA. Analytical Protocol Forms




1. Drug Identification Protocol and Marijuana Protocol forms are used tosummarize all analytical testing performed for a case.

a) The analyst enters the starting date for the case, the case number, exhibitnumber, and a description of the evidence.

b) A record of the testing is entered on the form as analyses are performed;

transcription of analyst notes from “scratch paper” is not acceptable.c) Calculations are also performed directly on this form.d) In general, each exhibit analyzed should have a Drug Identification

Protocol form.(1) Color testing or tentative identification of additional exhibits not

otherwise analyzed may be summarized on a separate DrugIdentification Protocol form or other summary sheet.

(2) Calculations must be shown in the case file.B. Weighing of Evidence

1. A total weight of the suspected controlled substance, less packaging, must beobtained for each population of evidence analyzed with the exception of a

residue.a) Weights should be entered onto the Drug Identification Protocol orMarihuana Analysis Protocol for each applicable exhibit.

b) The analyst must verify that the balance to be used is properly calibrated.c) The balance identification number used for each weight is recorded on

the protocol form.d) The total weight of the exhibit(s) is usually determined directly by

measuring the weight of the material.(1) In some cases, it may be necessary to determine the exhibit

weight by difference (total weight of packaging and contentsminus the weight of packaging). In this situation, the weight of

packaging is determined by actual weight or by averaging theweight of packaging from several representative items within oneexhibit.

2. For non-residue samples, an aliquot of each exhibit chosen for quantitativeanalysis will be weighed and placed into a screw cap vial or other suitablecontainer for further quantitative analysis.

3. Reporting weights.a) Weights from analytical balances are usually reported in milligrams.b) Weight determined from a top loading balance is usually reported in

grams.4. Suspected marihuana is usually determined in ounces and pounds.

C. Analytical Testing1. Selection of Evidence for Analysis

a) If numerous pieces of evidence are submitted to the Laboratory, theanalyst will select evidence for analysis based on the following criteria:

(1) Item(s) specifically requested by submitting agency(2) Chemical(s) in the highest penalty group(3) Evidence with the greatest weight(4) Other as determined by the analyst and/or supervisor




b) If initial testing is negative, testing will continue until a controlledsubstance is identified or until all exhibits have tested negative.

c) In general, a complete analysis will be performed on at least one piece of evidence in a case when a controlled substance is identified.

(1) A complete analysis usually consists of color test(s) and/or

preliminary identification of marked pharmaceutical preparations,unique qualitative analysis (such as GC/MS or IR), andquantitative analysis (such as GC).

(2) Additional testing may be performed as noted above, asdetermined by the analyst and/or supervisor, or when weight willincrease the penalty group.

(3) Any combination of analytical tests may be performed onadditional pieces of evidence.

d) Evidence may also be composited for testing.(1) If evidence is to be composited, each individual piece of evidence

to be combined will be color tested or otherwise tested to verify

the presence of a controlled substance.(2) To preserve the physical condition of the evidence as submittedand to minimize health hazards related to handling evidence, arepresentative sample from each piece of evidence to becombined will usually be taken, mixed into a homogenoussample, and used for analysis.

(a) In some cases, entire exhibits may be combined.(b) It must be clear from the Protocol form whether a single

exhibit or composited exhibits were analyzed and whethera portion of each item or the entirety of each item wascomposited.

e) If the number of items or exhibits needed to reach the applicableaggregate weight limit is large, analysis of a valid subset of the entirepopulation of samples may be performed using color testing,compositing, and analysis usually by GC/MS or IR. Quantitation mayalso be performed.

f) Documentation of materials analyzed and analyses performed must beclearly documented in the case file.

g) If there are numerous exhibits in a case and a substantial portion of exhibits will be processed for analysis in a manner which changes thephysical characteristics of the evidence, the analyst must photograph theevidence prior to analysis to establish a record of the original appearance

of the evidence as submitted.2. Color Testing and Preliminary Identification of Marked Pharmaceuticals

a) Color test(s) will usually be performed on a sample of each exhibit to beanalyzed using the methods described in the Color Testing procedure.

(1) If a color change occurs, the color of the spot test(s) performedand the preliminary identification should be recorded on the DrugIdentification Protocol and/or Marihuana Analysis Protocolforms.




(2) If there is no change in color, a negative result must be noted.b) Pharmaceuticals may be tentatively identified by markings using the PDR

and other indexes. This process should be documented on the Protocolform or other summary sheet.

3. Qualitative Identification

a) Unique identification of a controlled substance is typically made usingGC/MS or IR. Analytical methods are selected and noted on the DrugIdentification Protocol or Marihuana Analysis Protocol.

(1) The mass spectrum of any substance named in the final reportmust be included in the case file with a spectrum of theappropriate standard.

(a) A copy of the total ion chromatogram should also beincluded, and the identity of peaks reported on the finalreport must be labeled on the total ion chromatogram.

(b) In the case of a residue, a blank using the same analyticalprogram will be run immediately prior to the analysis of

the unknown and included in the case file.(2) The IR spectrum of the specimen analyzed must be included inthe case file along with a spectrum of the appropriate standard.

4. Quantitation a) Quantitation is usually performed by GC; although other techniques such

as UV may be used. The quantitative method used is noted on theProtocol sheet.

b) Written quantitative procedures may be found in the Procedure Manualfor the Drug Analysis Laboratory.

c) For GC analysis, the peaks in the chromatogram that correspond to thecontrolled substance shall be clearly labeled.

(1) In the case of a residue, a blank analysis using the same analyticalprogram will be run immediately prior to the analysis of theunknown substance and included in the case file.

d) The quantitative procedure including a summary of the extractionprocedure for each analytical method must be noted on the DrugIdentification Protocol Sheet.

(1) All calculations related to quantitative analysis are performed onthe protocol sheet including dilutions made.

(2) Calculations are made using all figures reported from theanalytical balance.

e) Instrument output is included as a part of the case file.

5. Identification of Non-controlled Substances and Ancillary Pharmaceuticalsa) If no controlled substance is identified in the analytical process, this will

be stated on the report.b) Marked dangerous drugs, over the counter preparations, and other

preparations may be identified through visual inspection usingmanufacturers markings, size, color, etc.

(1) The reference used to visually identify a substance should benoted in the case file.




(2) When these methods are used, it must be clearly stated on thereport; for example, “The material was visually identified as ___stated by the manufacturer to contain ____.”

6. Use of Non-standard Methods a) Because of the unique nature of many forensic specimens, exact

analytical procedures cannot be prescribed for every case. Therefore,analytical techniques described in this manual are given as guidance, andthe actual choice of analytical methodologies will be left to the discretionof the Drug Analyst, Supervisor, and/or Section Chief.

(1) All deviations from written procedures must be documented inthe case file.

(2) Use of methods not included in this manual requires approval of asupervisor and must be documented fully in the case file.

7. Verification of Case Number and Use of Bar Codes a) Throughout the analytical process, containers must be properly labeled

with a unique case/exhibit number.

b) Analysts must verify appropriate sample number prior to each specimentransfer.

c) Bar codes are used where possible to verify sample identity.(1) If the barcode is not properly read by the reader, the vial number

should be verified and noted by a second chemist.8. Calculating and Reporting Results

a) Results to be included on the final report are entered in a clear manner onthe Drug Identification Protocol; this includes the name of substancesidentified, the amount of any substances quantitated, and a percent of controlled substance in the exhibit tested if applicable.

(1) To calculate concentration of a controlled substance, all figures

recorded from the balance and the GC will be used.(2) Total exhibit weight measured on an analytical balance will be

recorded to 1/10 mg or as consistent with the accuracy of thebalance. If a top loader is used, weight will usually be recorded to1/100 g or as consistent with the accuracy of the balance.

(3) In each exhibit, the calculated amount of controlled substancewill usually be truncated and reported as follows:

Drug Analysis:

Calculated Result Reporting Format

0 - 1 mg 0.x mg1 - 99 mg xx mg100 - 999 mg 0.xx grams1 - 1.49 grams 1.xx grams1.5 – 29.9 grams xx.x grams30 - 999 grams xxx grams1000 grams and up 1.xx kilogramsLSD is usually truncated to a whole number (x micrograms).




1. administrative information: unique forensic laboratory case number, submittercase or reference number, submitter address, case name, arresting officer badgenumber, evidence receipt date, submitting individual information, receivingindividual information, general description of the item received, and the totalweight of the primary container(s)

2. analytical information and conclusions: a listing of each exhibit analyzed,description of exhibit(s) analyzed, identification of any controlled substancesidentified, adulterants or dilutants as applicable, weight of the controlledsubstance, purity of the controlled substance, and the total weight of the exhibit.

3. a list of exhibits suspected of being a controlled substance which were notanalyzed

4. a list of analyses performed5. signature of the analyst and reviewer

F. The analyst will perform a review of the typewritten report and ensure that it accuratelyreflects the results of analytical testing, is free of typographical errors, and is consistentwith laboratory policy.

G. The analyst will sign the report and complete a billing form.H. The case file is then sent to a supervisor for technical/peer review and countersignature.1. In an emergency situation in which a supervisor is not available, the case may be

reviewed by a second analyst who countersigns the case “reviewed by ...”.2. The technical/peer reviewer will initial each page of the examination

documentation.I. A copy of the report will be provided to the submitting agency and to the courts by

request.J. A notation will be made in the case file of the mailing/faxing date and entities receiving

a copy of the completed report.1. By standard practice, the Dallas County District Attorney’s Office has access to

electronic unsigned reports for the Dallas Police Department; this is not noted inthe case file.

K. The case file consists of the typewritten report, handwritten reports or notes, the DrugIdentification Protocol or Marihuana Analysis Protocol, all analytical work done by theanalyst which is reflected in or relied upon for the written report, instrument printouts,Description of Evidence form, the transmittal sheet, record of conversations, photos, peerreview sheets, and/or other relevant information.

L. Corrected, re-submittal, and amended reports1. If it is determined that a revised or corrected report must be generated, the report

will bear the notation “Corrected Report.” Copies of the corrected reports will besent to agencies receiving the previous copy of the report. The corrected report

will be filed along with the original case in the case folder.2. If additional work is requested on a completed case and the evidence has been

resubmitted to the Institute for this additional analysis, the report will typicallyinclude results of both submissions and be marked “Resubmittal.” A copy of thereport will be sent to all agencies receiving the previous report.

3. If additional work is requested on a completed case in which the final report hasbeen released but the evidence is still at the Institute, the report will typicallyinclude results of both submissions and be marked “Amended Report.” A copy of




the report will be sent to all agencies receiving the previous report.VII. Security of Evidence and Reports

A. Evidence is stored sealed as received from the submitting agency in the evidence storagevault until it is opened by the analyst for analysis.

B. During analysis evidence is stored in the vault, in the personal possession of the analyst,

or in the analyst’s personal locked storage area.C. After analysis, evidence is sealed and stored in the evidence storage vault until itsrelease/return to the submitting agency.

D. The completed case file, consisting of all records contributing to the reported results, ismaintained by the Evidence Registrar.

1. Case files may be stored on site or off-site in the Dallas County Records Storagefacility.

2. Retention of files is in accordance with Dallas County policy as implemented bythe Dallas County Records Manager.

VIII. Integrity of Evidence A. The quality of forensic analyses depends on preserving the integrity of the evidence. The

analyst must routinely use critical judgement and good lab practices and techniques at alltimes including but not limited to the following:

1. One case is processed at a time; although samples may be extracted in batches.2. Case numbers or bar code labels used on test tubes and other containers are cross

checked with the case and exhibit number.3. When bar codes are read by analytical equipment, the bar code must match with

the expected barcode number or vial identity verified by a second chemist.4. A fresh weighing paper or weighing boat is used during sample weighing;

balance calibration is verified prior to use.5. New, unused test tubes are used for laboratory analysis.6. Non-disposable equipment such as spatulas are thoroughly cleaned between use.

7. Case numbers and exhibit numbers on instrument records are compared withsample numbers.

8. The case number and handwritten initials of the record generator must appear oneach page of a case file.

9. When corrections are necessary to case records, the part in error will receive asingle strike through which is initialed by the analyst or responsible individual,and the correction will be written nearby. Correction fluid will not be used.

10. During analysis, the evidence must remain under the personal control of theanalyst unless it is formally released to another analyst for further testing. In anemergency, supervisors may access evidence.

11. Gloves should be changed as needed.

IX. Summary of Analyst Evidence Handling Process A. Initial Opening and Closing of Evidence

1. Obtain the submission weight of entire evidence package and enter on EvidenceSummary sheet.

2. Open evidence where possible without destroying other seals. Initial and dateany strip cut from the evidence bag and place into the evidence bag.

3. Perform a complete inventory of all evidence. Initial and date the Evidence




Summary sheet under the inventory.4. Compare Lab inventory to agency submittal inventory. If there is variance in

drug evidence, advise another analyst to immediately verify the inventory andsign and date the Evidence Summary sheet. Advise a supervisor immediately.**

5. Process evidence.

6. Re-inventory evidence* as it is placed into the evidence bag and reseal evidenceusing a proper seal.7. If the reinventory is reconciled, write “sealed” with initials and date in the upper

left of the Evidence Summary sheet. If the inventory does not match, advise asupervisor immediately.**

8. Obtain the exit weight of the entire evidence package and enter on EvidenceSummary sheet.

B. Reopening evidence1. Obtain a new submission weight of the entire evidence package and enter on

Evidence Summary sheet.2. Open evidence where possible without destroying other seals. Initial and date

any strip cut from the evidence bag and place into the evidence bag.3. Reinventory evidence*.4. If the reinventory is reconciled, write “reopened”, date and initials in the upper

left of the Evidence Summary sheet. If the inventory does not match, advise asupervisor immediately.**

5. Perform activities.6. Reinventory evidence* as it is placed into the evidence bag and reseal evidence

using a proper seal.7. If the reinventory is reconciled, write “sealed”, date and initials in the upper left

of the Evidence Summary sheet. If the inventory does not match, advise asupervisor immediately.**

8. Obtain a new exit weight of the entire evidence package and enter on theEvidence Summary sheet.

C. Related Issues1. Evidence remains sealed until it is opened for processing.2. Only one case is opened and processed at a time.3. Evidence is resealed at the conclusion of processing.4. All seals will meet the description of “proper sealed” detailed in the Quality

Manual.5. It is the responsibility of the analyst and the case reviewer to include evaluation

of submission and exit weights as part of routine case review.6. If room is not available on the Evidence Summary sheet, use the back of the

Evidence Summary sheet or add an additional sheet of paper. All entries shouldbe clearly identified as to their purpose.

D. Notes1. *Reinventory evidence - To verify the presence of all items listed on the

inventory which are not otherwise accounted for in the case file, for examplethose used in analysis.

2. **Supervisory responsibility – Document and investigate the situation in a timelymanner. Advise Section Chief. Advise submitter as applicable. Initiate Request





for Review as applicable.



DRUG LABORATORY INFORMATION MANAGEMENT SYSTEM(LIMS)

I. General Information

The Drug LIMS is designed to provide evidence tracking administrative internal and externalchain of custody, result entry and report writing, billing entry and reporting, and storage andtransfer of “non-official” report copies to the Dallas County District Attorney’s office.

II. User Log-In

The “User” is defined as the person who is entering data into the Drug LIMS. Each chemist andevidence custodian has an individual log-in name and password for security purposes and ease of system use.

When “logging in” to the system, double-click the Drug LIMS icon found on the computer

desktop. The user should enter their initials in the “User” box or pick their initials from the dropdown list. The user should then enter their unique password in the “Password” box and hit<Enter> or click on “Log In”. This will allow the user entry into the Drug LIMS and the MainMenu.

III. Menu Structure

Main MenuEvidence Transfer

Case SubmissionAssign Case to ChemistTransfer of CaseRelease EvidencePrint Chain of CustodyExit to Main Menu

ResultsResults EntryCase & Billing ReportsReview CasesExit to Main Menu

QueriesFind CaseExit to Main Menu

UtilitiesChange PasswordClear Case Transfer TableExit to Main Menu

Log Out

Dallas County Institute of Forensic Sciences 1 Laboratory Information SystemControlled Substances Laboratory Version 2.0




IV. Evidence Transfer

A. Case Submission

This function is used for the purpose of entering new cases from submitting agencies into

Drug LIMS and initiating chain of custody. Case and agency information may be inputusing two different strategies: manual entry and download of agency data.

Manual Entry :1. Input all agency information in text fields provided (Agency, Date, Received From)2. Input all case information for each case submitted, as applicable (DefendantName,

DOA, TAG#, SER#, Invc#, Status, Priority)3. Assign FL# by either typing the number in the FL# field, by barcoding the number

into the field, or by using the Assign FL#s button. Utilizing the Assign FL#s assignsthe first case in the field with a User inputted number, and assigns the following casesnumbers by increments of one.

4.

Data is updated and cases are ready for assignment once the Accept Data button hasbeen clicked. (NOTE: The Evidence Registrar may exit from the Case Submissionform without assigning FL numbers. The information is saved in the data table untilsuch time as the FL numbers are assigned and accepted.)

Downloaded Entry from Disc:1. Insert the floppy disk into the disk drive.2. Click the Import Cases from Floppy Disk button.3. Verify imported information.4. Assign FL numbers as described above in steps 3 and 4 (Manual Entry).

Note: A Supervisor must input billing and mailing data for new submitting agenciesbefore evidence can be logged in.

B. Assign Case to Chemist

This function is used for the purpose of transferring cases from the sealed evidencevault/evidence registrar to a chemist for analysis.

1. From the Evidence Transfer menu, select Assign Case to Chemist button.2. The receiving chemist must then log into the Drug LIMS system by entering their

User ID into the “To” field, entering their password into the “To Password” field and

tabbing to the “Cases to transfer” or hitting <Enter>. (Default information for thecurrently logged on user, i.e. the user transferring the evidence, and the date areautomatically filled in.)

3. The evidence registrar will then initiate the Internal Chain of Custody Form in handwritten notation, and electronically by either barcode scanning the transferred case orby manually picking the case out of the generated pick list, clicking the “Transfer”check box next to the case number. (NOTE: Rush cases appear at the top of the pick list, followed by Expedite, and Normal cases.)





V. Results

This menu item is used to enter evidence descriptions, type of evidence submitted, results andweights of examinations, examinations performed, billing information, and any other pertinentinformation found on the case report.

To enter the results of an examination on a particular case, choose the Results button on the MainMenu, which will open a new Results Menu.

A. Results Entry (Drug Cases)

1. The user completing the case must be logged into Drug LIMS.2. From the Results menu, select Results Entry.3. Scan the bar code or manually type in the desired FL#.4. Enter the number, description of the evidence submitted, and weight and units of the

evidence bag(s), box(es), etc. The drop down lists may be used for this operation.

(i.e. One heat sealed evidence bag weighing 28.3 grams). Refer to reporting resultssection in Analysis and Reporting of Casework.5. Enter the exhibit number.6. The Analyst’s initials will appear in the Analyst box. The default is the User

currently logged into Drug LIMS.7. The Requesting Agency is defaulted from the evidence registration process, but

should be verified before proceeding.8. Enter the number of items tested. NOTE: entering “one” will create the item container

in singular form, any other entry will result in a plural format.9. Enter an item description and container. The drop down lists may be used for this

operation.

10. Enter the description of the evidence exhibit and the substance. The drop down listsmay be used for this operation. NOTE: A comma will be placed between the twodescriptives; if only one adjective is needed, use only the first description box. If additional descriptives are needed, free-form typing is used and correct punctuationshould be added.

11. Select the Drug button.12. Enter the Substance to be reported, the Amount, Units, Percentage (Pct), Total

Weight and Total Weight Units.13. Enter any adulterants or dilutants in subsequent “Substance” fields.14. When all information has been entered, select the Update Result button.15. The User can then proofread the rough draft of the report, and add any other

information in the “Result” field.16. If more than one exhibit has been analyzed, repeat the above steps after advancing

the “Record” number. NOTE: If multiple exhibits are found to contain the samecontrolled substance, it may be of value to the user for the report to include the totalor aggregate weight of the multiple exhibits. This can be done by entering all data forthe last exhibit number, entering all relevant exhibit numbers in the AggregateExhibits box, entering the aggregate weight and units, and then clicking the UpdateResult button.





17. Enter all Examinations that were performed for each exhibit. The defaultedexaminations for Drug Cases are “Color Test, Gas Chromatography, and GasChromatography/Mass Spectrometry.” To add or delete examinations, click on theExaminations button, click the Clear Examinations button, click on each testperformed from the list on the left, and then click the Accept button.

18. Enter all Billing information. The defaulted billing charges are one ExploratoryQualitative (302) and one Gas Chromatography/Mass Spectrometry (305).Additional charges are added by using the drop down pick list and entering thecorresponding number of charges for that examination. Billing is entered on a “perexhibit” basis.

19.When all data has been entered, click the Exit button to return to the Results menu, orenter a new FL# to enter data for additional cases.

B. Results Entry (Marihuana Cases)

1. The user completing the case must be logged into Drug LIMS.

2.

From the Results menu, select Results Entry.3. Bar code scan or manually type in the desired FL#.4. Enter the number, description of the evidence submitted, and weight and units of the

evidence bag(s), box(es), etc. The drop down lists may be used for this operation.Refer to the reporting results section in Analysis and Reporting of Casework.

5. Enter the exhibit number.6. The Analyst’s initials will appear in the Analyst box. The default is the User


should be verified before proceeding.8. Enter the number of items tested. NOTE: Entering “one” will create the item

container in singular form, any other entry will result in a plural format.9. Enter exhibit description and container. The drop down lists may be used for thisoperation. A comma will be placed between the two descriptives, if only oneadjective is needed, use only the first description box. If additional descriptives areneeded, free form typing is used and correct punctuation should be added.

10. Select the Marihuana button.11. The Substance to be reported, “marihuana” is the default, the Total Weight and Total

Weight Units are entered.12. When seed germination is requested, Click the “Seeds” box if seeds were present, and

click the “Germinate” box if the seeds were capable of germination. If seeds werecapable of germination, then the Net Weight and Net Units are entered.

13. When all information has been entered, select the Update Result button.14. The User can then proofread the rough draft of the report, and add any other

information in the “Result” field.15. If more than one exhibit has been analyzed, repeat the above steps after advancing the

“Record” number. NOTE: If multiple exhibits are found to contain marihuana, itmay be of value to the user for the report to include the total or aggregate weight of the multiple exhibits. This is done by entering all data for the last exhibit number,entering all relevant exhibit numbers in the Aggregate Exhibits box, entering the





aggregate weight and units, and then clicking the Update Result button.16. Enter all Examinations that were performed for each exhibit. The default

examinations for Marihuana Cases are “Color Test, Microscopic Test, GasChromatography/Mass Spectrometry, and Seed Germination (when seeds arepresent).” To add or delete examinations, click on the Examinations button, click the

Clear Examinations button, click on each test performed from the list on the left, andthen click the Accept button.17. Enter all Billing information. The default billing charges are one

Marihuana/Cannabinoids (308), one Gas Chromatography/Mass Spectrometry(305), and one Marihuana Seed Germination (309), (when conducted). Additionalcharges are added by using the drop down pick list and entering the correspondingnumber of charges for that examination. Billing is entered on a “per exhibit” basis.

18. When all data has been entered, click the Exit button to return to the Results menu, orenter a new FL# to enter data for additional cases.

C. Results Entry (Product Identification)

1. The user completing the case must be logged into Drug LIMS.2. From the Results menu, select Results Entry.3. Bar code scan or manually type in the desired FL#.4. Enter the number, description of the evidence submitted, and weight and units of the

evidence bag(s), box(es), etc. The drop down lists may be used for this operation.Refer to the reporting results section in Analysis and Reporting of Casework.

5. Enter the exhibit number.6. The Analyst’s initials will appear in the Analyst box. The default is the User


should be verified before proceeding.8. The total number of items (tablets/capsules) are entered into the “Number of items”field. NOTE: Entering “one” will create the item container/product form in singularform, any other entry will result in a plural format.

9. Enter an item description and container. This entry is actually a description of theproduct form (capsule/tablet/etc.). The drop down lists may be used for thisoperation.

10. Select the Product ID button.11. Do not make an entry in the “Product Name” field. Press the “Product Search”

button. A new form will appear.12. If the product is known, select it from the “Find Product” drop down list. When the

desired product is found, press the “Send Selection to Report” button.13. If the product is NOT on the list, a new entry can be created by typing the unique

identifier (logo) into the “Unique Identifier” field. Copy (Ctrl-c) and paste (Ctrl-v)this unique identifier into the “Logo” and “Find Product” fields. Enter all knowninformation into blank fields and press the “Send Selection to Report” button.

14. Enter data into remaining fields (Total Weight and Units), and click the “Analyzed”box if a mass spectrum was obtained, and what substance(s) was identified.

15. When all information has been entered, select the Update Result button.





This function may only be used by Authorized Reviewers such as a supervisor. Once areport is reviewed and countersigned, the reviewer will approve the case. A revieweddate is entered and a “non-official” copy of the report is sent to the Dallas County DA’scomputer server for their use. NOTE: Only DPD cases are sent to the DA’s server.

VI.

Queries

This function is used to find cases by a number of different entries. Two views are allowed forthis screen: Form View and Datasheet View. Form View is ideal for looking at a single record.Datasheet View is best suited for multiple records. A disadvantage of the latter is that to view allinformation the User must scroll the screen horizontally to see all fields. Scrolling through therecords is accomplished by using the record selectors at the top or bottom of the screen.

To find specific cases :1. From the Main Switchboard, select Queries button.2. Select the Find Case button.

3.

Select the Filter By Form button.4. Enter the desired information to be searched into any of the fifteen (15) fields. NOTE: Morethan one field may be entered.

5. Select the Apply Filter button.6. When finished select the Exit button.

NOTE: If an item to be searched might have more than one entry, for example, a defendant withthe last name of Smith, then enter the last name and an asterisk in quotation marks ( “Smith,*” )and select the Filter by Form button.

VII. Utilities

This function is used to change the Users password and to clear all transfer tables.

To change password:1. Select the Change Password button2. Enter Old Password3. Enter New Password4. Confirm New Password5. Select OK

Drug LIMS will then restart and the User will be asked to log back into the system.

NOTE: The Clear Transfer Table should only be used by the Evidence Registrar or Supervisor,and only when there is not a transfer of cases being preformed.

VIII. Log Out

This function is used to exit out of the Drug LIMS.





COURT TESTIMONY, DEPOSITIONS, and other LEGAL PROCEEDINGS

1. General

1.1. The Dallas County Institute of Forensic Sciences is an independent laboratory which

provides services on a fee for services basis under direction of the Dallas CountyCommissioners Court and the Director of the Institute.1.2. As such, the Institute is not part of any police agency, the Dallas County Sheriff’s

Office, or the District Attorney’s Office.1.3. Most cases submitted to the Laboratory are forensic in nature and employees may

reasonably be expected to provide testimony in legal proceedings regarding facts andopinions related to submitted evidence.

1.4. As outlined in the mission statement of the Institute, it is the goal of Institute staff toperform forensic laboratory analyses with accuracy, integrity, and reliability and topresent written and oral results of analyses in a complete and impartial manner.

2. Fact Testimony

2.1. All employees of the Forensic Chemistry Section are subject to call for fact testimony byvirtue of their employment with the Institute.

2.2. This type of testimony is used for building a record at trial concerning events occurringprior to trial such as receipt and release of evidence, custody of evidence, typing of reports, etc.

2.3. Employees called as fact witnesses must limit their testimony to personal actions taken(receipt and release of evidence, record generation, lab number assignment, typing, etc.).

2.4. Use of laboratory records by fact witnesses shall be limited to identification of applicable records and actions personally conducted by the employee.

2.5. The fact witness should not respond to questions about legal or scientific aspects of thecase; these should be referred to other witnesses.

3. Introducing a Business Record

3.1. Laboratory staff may be called to introduce a laboratory report as a business record.3.2. This typically occurs when the testifying staff did not perform work on the case under

discussion.3.3. The witness will answer a standard set of questions designed to establish the case report

as a business record.3.4. Then the witness will read the report into the record.

4. Expert Witness Testimony

4.1. Most testimony performed by analysts and supervisors will blend fact testimony withopinion or expert testimony.

4.2. Testifying staff are expected to maintain proficiency in the following areas:4.2.1. A thorough understanding of applicable Texas and federal laws.4.2.2. A broad general knowledge of natural science as applicable.

Dallas County Institute of Forensic Sciences 1 TestimonyControlled Substances Laboratory Version 2.0




4.2.3. An appropriate subject matter expertise in the employee’s discipline.4.2.4. Knowledge of the legal requirements for maintaining chain of custody of evidence

and for ensuring care, custody, and control of evidence and official records of theiranalyses.

4.2.5. Mastery over the scientific and technical aspects of the analytical methods used

and the legal and scientific certainty of the validity of their results.4.2.6. The ability to defend their analytical findings under court examination with clearand concise testimony using acquired forensic skills.

4.3. Until such time as an employee is considered acceptable by the Section Chief to givecourtroom testimony, he shall not provide expert testimony in those cases in which hehas prepared the report but shall refer such cases to the designated analyst or supervisorwho will have co-signed the case report.

4.4. Expert witness testimony will be limited to the analyst’s area of expertise and will befurther limited to testimony in cases in which the analyst actually performed work, work was performed under their supervision, or testimony is provided with approval of asupervisor.

4.5. The analyst is responsible for testimony concerning laboratory policy or interpretation of the law only as it pertains to the analytical conclusion reached in the specific case attrial.

4.6. Because expert knowledge is not subject to subpoena, analysts cannot be required toprovide testimony in any case in which they did not perform analyses.

4.7. Permission to conduct outside employment requires prior permission of the SectionChief forwarded up to the Institute Director; the policy relating to outside employment iscovered in the Dallas County Code.

4.8. An employee providing testimony as part of his County duties, must produce a subpoenaunless testimony is provided for the Dallas County District Attorney’s Office or meetsother standing arrangement.

4.8.1. Pre-arrangement has been made with the Dallas County District Attorney’s Officeto honor telephone or fax requests in order to avoid the expense and inconvenienceof issuing subpoenas for Institute employees.

4.9. Individuals leaving the building to go to Court should check out with the SectionSecretary or Evidence Registrar.

4.10. All requests – including subpoenas – for testimony which is unrelated to the analysis of a specific Institute case must be reviewed prior to trial with a supervisor or InstituteDirector in the absence of a supervisor.

4.11. The individual receiving a subpoena is responsible for advising the requestor of applicable preparation, testimony, and travel fees to be charged by Dallas County relatedto the subpoena; written agreement to pay fees should be received from the requestorprior to the date of the proceeding.

4.11.1. Disagreement about payment of fees should be brought to the attention of asupervisor and the Civil Section, Dallas County District Attorney’s Office, prior tothe proceeding.

4.11.2. The Dallas County Commissioners Court has ordered that payment is required inadvance (two hours minimum) for all services provided to private attorneys and anycosts in excess of the minimum are payable at the time service is rendered.





4.11.3. At the discretion of the Director, payment may be required before any service isrendered.

5. Testimony in the Capacity of Supervisor

5.1. The Eighth District of Texas, Court of Appeals in the case of Antoine Delano Caw v. theState of Texas (No: 08-92-00155-CR) has determined that chemists employed by theDallas County Forensic Laboratory do not meet the definition of law enforcementpersonnel. Therefore, test results sponsored by a supervisor are admissible as a businessrecords exception to the hearsay rules.

5.2. A supervisor usually enters the report as a business record. He then provides testimonyregarding education and training of the analyst and their oversight of the analyst. Afterreview of case file documentation, the supervisor can also testify as an expert witnessbased upon his own evaluation of data in the case file.

6. Dress

6.1. Professional business attire should be worn to all legal proceedings.6.2. This usually includes a tie and/or jacket for men and dress, skirt, or pantsuit for women.6.3. Shorts, jeans, and tee shirts are not appropriate.6.4. Physical appearance should be neat and professional.6.5. Dress code for federal may be more stringent; direction is usually provided with the

subpoena if applicable.

7. Review of Testimony

7.1. Testimony of staff will be reviewed annually as described in the Quality ManagementProgram.

8. General Guidelines for Testimony

8.1. Tell the truth at all times.8.2. If you do not know or are unsure of an answer, clearly state this; you may state that you

are not trained in this area, refer the question to a supervisor, etc.8.3. Remain composed and professional; treat all parties with respect.8.4. Keep on sound scientific ground; stay within your area of expertise.8.5. Be prepared; review case prior to trial.8.6. Understand the difference between possibility and probability.8.7. Do not answer questions you do not understand. Ask for questions to be repeated or

rephrased.8.8. Do not provide answers to unasked questions.8.9. Explain scientific concepts in clear layman’s terms; avoid use of jargon.8.10. Speak to the jury (jury trial) or judge (trial before the court).8.11. When problems or confusion arise, speak to the Judge.8.12. Speak slowly and distinctly. Speak in a tone that can be heard by the jury and court

reporter.





Dallas County Institute of Forensic Sciences Acetylated DerivativesControlled Substances Laboratory 1 Version 2.0

FORMATION OF ACETYLATED DERIVATIVES

Analysis of N-Hydroxy MDA

Principle of Assay:

In some situations, chemicals with reactive hydrogens do not chromatograph well due toadsorption and/or thermal break down in the inlet of a gas chromatograph (GC). Occasionally,analytes do not separate well enough by GC for their analysis. Under these circumstances,chemical derivatization may solve these chromatographic issues and allow successful analysis of the substances in question. Acetylation is one method of derivatization. Using acetylation,chemicals which contain active hydrogens (for example –OH, -SH, and –NH) are converted intoesters, thioesters, and amides respectively. When acetic anhydride [(CH 3CO) 2O]is used as theacetylating agent, the reactive hydrogen is replaced with an acetyl group (CH 3CO-).

At the high temperatures encountered in GC and GC/MS, N-hydroxy-3,4-

methylenedioxyamphetamine (N-hydroxy MDA) undergoes pyrolytic disproportionation. Onemolecule of N-hydroxy MDA is oxidized to 3,4-methylenedioxyphenyl-2-propanone-2-oxime(oxime) with simultaneous reduction of another molecule of N-hydroxy MDA to 3,4methylenedioxyamphetamine (MDA). As a result at least two chromatographic peaks areproduced. Acetylation of N-hydroxy MDA results primarily in a diacetylated molecule which isstable during GC and GC/MS analysis. Whenever N-hydroxy MDA and the oxime are detectedby standard analytical procedures, acetylation should be performed to accurately identify thesubstances present.

Equipment:

Gas chromatograph-mass spectrometer a methylsiloxane capillary column such as an HP-5MS,30 m x 0.25 mm x 0.25 um film thickness and gas chromatograph-flame ionization detector withsplit/splitless injector containing a methylsiloxane capillary column such as an HP-1, 15m x 0.32mm x 1.0 um film thickness (see GC/MS and GC Methods Notebooks in Drug Laboratory).

Screw top culture tubes, 25 mL, 20 mm x 125 mm, screw cap with Teflon linerScrew top culture tubes, 15 mL, 16 mm x 125 mm, screw cap with Teflon linerVolumetric flasks, 10 mL, 25 mL, 500 mLAutosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsVortex mixerCentrifugeTest tubesAnalytical balancePipettes, variouspH paper

Reagents:

Acetic anhydride, reagent grade or better





in the exhibit. If powder is also present, remove a sample and add to the material scrapedfrom the solid pieces. Pulverize the resulting composite sample and analyze as described.

c) GC/MS Identificationi) Transfer approximately 10 mg of material to 1 mL methanol in a test tube.

(1) The analyst will vary the amount of material and methanol as needed to obtain an

acceptable mass spectrum.ii) Vortex and centrifuge as necessary.iii) Transfer an aliquot to an autosampler vial and inject on the GC/MS using BLANK.M

method. A chromatogram displaying MDA and the oxime indicates the presence of N-OH MDA.

iv) N-hydroxy MDA decomposes on the injection block to MDA and the oxime,therefore acetylation is required to provide definitive identification by GC andGC/MS.

v) Transfer 50.0 mg sample to a 15 mL screw cap culture tube, add 1-2 mL aceticanhydride, cap, let stand 24 hours at room temperature. Evaporate to dryness.

vi) Reconstitute with methanol.

vii) Inject an aliquot on the GC/MS using BLANK.M method.d) GC Quantitation

i) Weigh approximately 10 - 50 mg of the material to be analyzed, and record theweight on the Drug Protocol Worksheet.

ii) Transfer sample to a 15 ml labeled, screw cap culture tube.iii) N-hydroxy MDA decomposes on the injection block to MDA and the oxime,

therefore acetylation is required.iv) Transfer 50.0 mg sample to a 15 mL screw cap culture tube, add 1-2 mL acetic

anhydride, cap, let stand 24 hours at room temperature. Evaporate to dryness.v) Add 5.0 mL of deionized water and approximately 200 mg sodium bicarbonate to the

culture tube.vi) Add 5.0 mL of internal standard solution.vii) Cap the tube and place on rotator for 5 - 10 minutes.viii) Centrifuge for 5 - 10 minutes on medium setting.ix) Transfer an aliquot of the organic layer to an autosampler vial.x) Inject extracted sample into GC using the appropriate instrument method

and calculate the results.

Instrument Parameters:

See GC and GC/MS Methods Notebooks located in the Drug Laboratory.

Reporting Criteria:

1. Report both the quantity and the identity of the drug when the concentration of the drug iswithin +/- 20% of the calibration curve on the GC and the GC/MS is complete. It may benecessary to dilute extracted samples to bring them within the curve range.

2. Report the amount of the drug as insufficient for quantitation when the drugconcentration is below 20% of the calibration curve on the GC and the GC/MS iscomplete.





Calculations:

1. Dilutionsa. In any situation in which a dilution is made, multiply the concentration of drug

(mg/mL) by the dilution factor. A notation relating to how dilutions were made

must be made in the case file.2. Materials Analyzed by Weight:a. concentration of drug (mg/mL) x volume of internal standard solution used for

extraction (mL) x total exhibit weight (mg)/extracted sample weight (mg) = mg of drug in the exhibit as the free base

3. Percent drug in the exhibit:a. mg of drug in the exhibit/total weight of the exhibit x 100 = % of drug in the

exhibit





Training Notes:Acetylation Procedure

1. N-hydroxy MDA often appears as round unmarked white tablets or round green speckledtablets. Weight of tablets is often about 500 mg.

2. Whenever MDA and the oxime are identified in standard GC or GC/MS runs, this

procedure should be performed to determine whether N-hydroxy MDA is present and thesource of the MDA and oxime.3. Acetic anhydride is moisture sensitive. It is also volatile and reactive; it should be used

in the hood.4. Since N-hydroxy MDA has two reactive hydrogens (the amine and hydroxyl), it will

form a diacetyl derivative. Incomplete derivatization will produce both the monoacetyland diacetyl products which will appear as two chromatographic peaks.

5. Liquids should be evaluated for suitability. Water, alcohols, and other liquid vehiclescontaining reactive hydrogens will compete with the sample for acetylation usuallyresulting in poor acetylation of the sample. Liquids may be taken to residue and thenacetylated; however, care should be taken to remove water or other solvent residue prior

to acetylation.




Dallas County Institute of Forensic Sciences Acidic Drug AnalysisControlled Substances Laboratory 2 Version 2.0

Erlenmeyer flasks, variousGraduated cylinders, variousAnalytical balancePipettes, variouspH paper

Reagents:

Phenanthrene, reagent grade or betterChloroform, reagent grade or betterHCl, reagent grade or betterMethanol, reagent grade or betterHCl, reagent grade or betterAnalytical standards

Reagent Volume of Chemical Volume of deionized H 2O

25% HCl 10 mL 30 mLIn the hood, place 30 mL deionized water into a 50 mL graduated cylinder and carefully add 10mL of concentrated HCl using a graduated cylinder. Transfer to a 50 mL Erlenmeyer flask forstorage.

Methanolic HCl (5%)Transfer 95 mL of methanol to a 100 mL Erlenmeyer flask, then add 5 mL concentratedHCl.

Safety Precautions:

The most common type of chemical or biological exposure in this type of laboratory is a splashto the skin or eye. Skin, mucous membranes, or eyes which have been splashed with commonlyused chemicals or biologicals should be thoroughly washed for at least 15 minutes in cool tapwater or eye wash station. Refer to appropriate MSDS’s for additional chemical information.Report the incident immediately to a supervisor. Seek medical attention as necessary.

Chloroform is a chlorinated solvent and is considered a human carcinogen. Use in a hood or in awell ventilated area. Avoid contact with skin, eyes, or mucous membranes.

Hydrochloric acid is corrosive. Avoid contact with skin, eyes, and mucous membranes.

Methanol is a flammable solvent. Avoid contact with skin, eyes, and mucous membranes.





Internal Standard Solution Preparation:

Internal Standard Amount of Chemical Final Volume Solvent

0.5mg/mL phenanthrene 0.25 grams phenanthrene 500 mL chloroform

Transfer 0.25 g phenanthrene to a 500 mL volumetric flask, and bring to volume with solvent.Mix by inverting flask.

Calibration Standards:

All solutions of stocks and standards are kept in the refrigerator. Allow the standards to come toroom temperature before using.

The concentration, amount, and volume of the calibration stock and calibration standards mayvary proportionally depending on the availability of drug, the expected concentration range of the drug, and the needed volume of standard. The following is provided as a guide:

Calibration Stock Amount of Drug (free acid) Final Volume Solvent

5.0 mg/mL Drug 50.0 mg 10 mL deionized water

Transfer 50.0 mg drug calculated as the free base to a 10 mL volumetric flask, and bring tovolume with deionized (DI) water. Mix by inverting flask. Sonicate as needed. Transfer to a 15mL screw cap culture tube for storage.

Calibration Procedure:

1. Choose a minimum of three appropriate calibration standards for the calibration curvebased on the linear range required for the sample or drug to be analyzed.

2. Using a Hamilton syringe, and/or a volumetric pipette, place the appropriate amount of calibration stock into a 15 mL screw cap culture tube. Add deionized water to make atotal volume of 5.0 mL.

Calibration Standards Amount of Calibration Stock Amount of DI H 20 Volume I.S. solution0.10 mg/mL 0.10 mL 4.90 mL 5 mL

1.00 mg/mL 1.0 mL 4.0 mL 5 mL5.00 mg/mL 5.0 mL 0 5 mL

3. Add 5 drops of 25% HCl and 5.0 mL internal standard solution.

4. Cap the tubes and place on rotator for 5 - 10 minutes.5. Centrifuge for 5 - 10 minutes on medium setting.6. Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top; chloroform on the bottom.7. Inject the extracted calibration standards into the GC using the appropriate method.





2. If the QC sample is not within the set limits of +/- 5% of the target concentration, additionalaction must be taken to obtain an acceptable QC result such as re-running QC, re-extractingand re-running QC, making new stock with re-extraction and re-analysis, re-calibrating (runcurve), and/or consulting a supervisor.

Color Testing:

See the section on Color Tests. Spot tests will usually be run on each item of non-pharmaceutical evidence within one exhibit up to the applicable statutory weight limit.

Analytical Procedure:

1) Powdered Samples and Other Solids:a) Obtain the total weight of the material in the exhibit to be analyzed and record on the

Drug Protocol Worksheet.b) Create a representative specimen by taking a sample from many or all of the solid pieces

in the exhibit. If powder is also present, remove a sample and add to the material scrapedfrom the solid pieces. Pulverize the resulting composite sample as necessary and analyzeas described.

c) GC/MS Identificationi) Transfer approximately 10 mg of material to approximately 1 mL methanol in a test

tube.(1) The analyst will vary the amount of material and methanol as needed to obtain an


method.

d) GC Quantitationi) Weigh approximately 10 - 50 mg of the material to be analyzed, and record the

weight on the Drug Protocol Worksheet.ii) Transfer sample to a 15 mL labeled screw cap culture tube.iii) Add 1.0 - 5.0 mL of deionized water using a volumetric pipette and 1 - 5 drops of

25% HCl using a Pasteur pipette to the culture tube.iv) Add 1.0 - 5.0 mL internal standard solution.v) Cap the tube and place on rotator for 5 - 10 minutes.vi) Centrifuge for 5-10 minutes on medium setting.vii) Transfer an aliquot of the organic layer to an autosampler vial.viii) Inject extracted sample into GC using appropriate instrument method and calculate

the results.

2) Tablets, Capsules, and Other Solid Pharmaceutical Preparations:a) Obtain the total weight of the material in the exhibit to be analyzed and record on the

Drug Protocol Worksheet.





b) Create a representative sample for analysis and grind to a powder if necessary.i) Capsules – typically a composite sample is used for analysis.ii) Tablets – typically one tablet is selected for analysis.

c) Logo Identificationi) Refer to Pharmaceutical Analysis Procedure.

d) GC/MS Identificationi) Transfer an amount of sample that is equivalent to approximately 1 mg of drug toapproximately 1 mL methanol in a test tube.(1) The analyst will vary the amount of material and methanol as needed to obtain an

acceptable mass spectrum.ii) Vortex and centrifuge as necessary.iii) Transfer an aliquot to an autosampler vial and inject on the GC/MS using

BLANK.M method.e) GC Quantitation

i) Weigh approximately 10 - 50 mg of the material to be analyzed, and record theweight on the Drug Protocol Worksheet.

ii) Transfer sample to a 15 mL labeled screw cap culture tube.iii) Add 1.0 - 5.0 mL of deionized water using a volumetric pipette and 1 - 5 drops of 25% HCl using a Pasteur pipette to the culture tube.

iv) Add 1.0 - 5.0 mL internal standard solution.v) Cap the tube and place on rotator for 5 - 10 minutes.vi) Centrifuge for 5-10 minutes on medium setting.vii) Transfer an aliquot of the organic layer to an autosampler vial.viii) Inject extracted sample into GC using appropriate instrument method and calculate

the results.

3) Liquid Samples:

a) Liquid samples may be analyzed by weight or by volume. If the sample is to be analyzedby volume, a known volume of the liquid must be weighed to determine density.i) If the volume of liquid is small, it should be treated as a residue; see below.ii) Obtain the total weight of liquid in the exhibit to be analyzed and record on the Drug

Protocol Worksheet.(1) If the liquid is to be analyzed by volume, record the total volume on the Drug

Protocol Worksheet.iii) Mix the liquid well before sampling.iv) GC/MS Identification

(1) Place approximately 1 part sample to 4 parts methanol in a 15 mL screw capculture tube.

(a) The analyst will vary the amount of material and methanol as needed to obtainan acceptable mass spectrum.

(2) Transfer an aliquot to an autosampler vial. Analyze by GC/MS using BLANK.Mmethod.

v) GC Quantitation





a screw cap.(4) Label the tube “added by laboratory”, include FL# and initials, and place this tube

in the evidence bag along with the evidence.


See the GC and GC/MS Methods Notebooks located in the Drug Laboratory.

Reporting Criteria:

1. Report both the quantity and the identity of the drug when the concentration of the drug iswithin +/- 20% of the calibration curve on the GC and the GC/MS is complete. It may benecessary to dilute extracted samples to bring them within the curve range.

2. Report the amount of the drug as insufficient for quantitation when the drug concentration isbelow 20% of the calibration curve on the GC and the GC/MS is complete.

Calculations:

1. Dilutionsa. In any situation in which a dilution is made, multiply the concentration of drug (mg/mL)

by the dilution factor. A notation relating to how dilutions were made must be made inthe case file.

2. Materials Analyzed by Volume:a. concentration of drug (mg/mL) x volume of internal standard solution used for extraction

(mL) x total exhibit volume/extracted sample volume = mg of drug in the exhibit as thefree base

3. Materials Analyzed by Weight:

a. concentration of drug (mg/mL) x volume of internal standard solution used for extraction(mL) x total exhibit weight (mg)/extracted sample weight (mg) = mg of drug in theexhibit as the free base

4. Percent drug in the exhibit:a. mg of drug in the exhibit/total weight of the exhibit x 100 = % of drug in the exhibit





Training Notes: Acidic Procedure

1. If GC/MS results are negative when run on BLANK.M, run on alternative GC/MS methodssuch as LOWDOSE.M, LSD.M, etc. until satisfied that no controlled substance is present.

2. The free acid form of a barbiturate may not be soluble in water; therefore, these standards

may be made in ethanol. For quantitation, the proper amount if ethanolic calibrationstandard is evaporated to dryness before proceeding to extraction.3. Clarke’s Analysis of Drugs and Poisons is a good source for determining the solubility of a

particular drug standard.4. Some drug combinations such as Fiorinal with codeine contain acid and alkaline drugs. One

approach for this combination preparation is to first perform an alkaline extraction foridentification of codeine and caffeine and quantitation of codeine. Then perform an acidextraction on the aqueous phase remaining after the alkaline extraction. To do this, add 25%HCl to the aqueous phase until the pH<3. Continue with the acid extraction by adding 5.0mL internal standard solution. Qualitatively identify salicylate and butalbital in the organicphase by GC/MS.

5. Some pharmaceutical preparations of acid drugs, such as phenobarbital, are in time releaseform. To improve recovery it this case, allow the sample to sit overnight in 5.0 mL water and5 drops of 25% HCL. In the morning, continue the assay by adding 5.0 mL internal standardsolution and following the acid drug procedure.

6. A sonicator may be used to bring materials into solution. Care should be used regarding thelength of time materials are left in the sonicator since heat may decompose some drugs.Typically, a sonication time of 5 minutes or less is used.

7. Valproic acid and ethchlorvynol are volatile. Solutions containing valproic acid orethchlorvynol should be evaporated carefully and removed from the evaporation station as thetube reaches dryness. Due to their volatility, valproic acid and ethchlorvynol should berun using the volatiles GC/MS method.




analysis using this procedure.

Equipment:

Gas chromatograph-mass spectrometer containing a methylsiloxane capillary column such as an HP-

5MS, 30 m x 0.25 mm x 0.25 um film thickness and/or gas chromatograph-flame ionization detectorwith split/splitless injector containing a methylsiloxane capillary column such as an HP-1, 15 m x0.32 mm x 1.0 um film thickness (see GC/MS and/or GC Methods Notebooks in Drug Laboratory).

Screw top culture tubes, 25 mL, 20 mm x 125 mm, screw cap with Teflon linerScrew top culture tubes, 15 mL, 16 mm x 125 mm, screw cap with Teflon linerVolumetric flasks, 10 mL, 25 mL, 2 literAutosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsVortex mixerRotatorCentrifuge

SonicatorGraduated cylinders, variousTest tubesAnalytical balanceHamilton syringes, 100 uL, 250 uL, 500 uLPipettes, variouspH paperAdjustable 10 mL Dispensette Reagent BottleErlenmeyer flask, 50 mL, 100 mLMortar and Pestle

Reagents:

n-Butyl chloride, reagent grade or betterChloroform, reagent grade or betterNaphthalene, reagent grade or betterPhenanthrene, reagent grade or betterMethanol, reagent grade or betterHCl, reagent grade or betterSodium hydroxide, reagent grade or betterAnalytical standards

Reagent Amount of Chemical Volume of deionized H 2O40% NaOH (w/v) 40 g NaOH 100 mLTransfer to a 250 mL Erlenmeyer flask. In a hood, immerse the flask in a cold tap water bath. USECAUTION, this mixture will get extremely hot. Cautiously swirl the flask to dissolve. Cool and mixwell.

Reagent Volume of Chemical Volume of deionized H 2O

Dallas County Institute of Forensic Sciences Alkaline Drug AnalysisControlled Substances Laboratory 2 Version 2.0




25% HCl 10 mL 30 mLIn the hood, place 30 mL deionized water into a 50 mL graduated cylinder and carefully add 10 mLof concentrated HCl using a graduated cylinder. Transfer to a 50 mL Erlenmeyer flask for storage.

Methanolic HCl (5%)

Transfer 95 mL of methanol to a 100 mL Erlenmeyer flask, then add 5 mL concentrated HCl.

Safety Precautions:

The most common chemical exposure in this type of laboratory is a chemical splash to the skin oreye. Skin, mucous membranes, or eyes which have been splashed with commonly used chemicalsor biologicals should be thoroughly washed for at least 15 minutes in cool tap water or eye washstation. Refer to MSDS’s for additional chemical information. Report the incident immediately to asupervisor. Seek medical attention as necessary.

n-Butyl chloride is flammable. Use in a vent hood or in a well ventilated area. Avoid contact withskin.

Sodium hydroxide and hydrochloric acid are corrosive. Avoid contact with skin, eyes, and mucousmembranes.

Methanol is a flammable solvent. Use in a hood or in a well ventilated area.

Chloroform is a chlorinated solvent and is considered a human carcinogen. Use in a hood or in awell ventilated area. Avoid contact with skin.

Internal Standard (I.S.) Solution Preparation:

Internal Standard Amount of Chemical Final Volume Solvent0.5 mg/mL phenanthreneor naphthalene

1.00 g phenanthrene ornaphthalene

2.0 L n-butyl chloride

Transfer 1.00 g phenanthrene or naphthalene to a 2.0 L volumetric flask, and bring to volume withsolvent. Mix by inverting flask.


All solutions of stocks and standards are kept in the refrigerator. Allow the solutions to come to

room temperature before using them.

The concentration, amount, and volume of the calibration stock and calibration standards may varyproportionally depending on the availability of drug and the expected concentration of the drug. Thefollowing is provided as a guide:

Calibration Stock Amount of Drug (as base) Final Volume Solvent5.0 mg/mL Drug 50.0 mg 10 mL deionized water





Transfer 50.0 mg drug calculated as the free base to a 10 mL volumetric flask, and bring to volumewith deionized (DI) water. Mix by inverting flask. Sonicate as needed. Transfer to a 15 mL screwcap culture tube for storage.



2. Using a Hamilton syringe and/or volumetric pipette, place the appropriate amount of calibration stock into a 15 mL screw cap culture tube. Add deionized (DI) water to makea total volume of 5.0 mL.

Calibration Standards Amount of Calibration Stock Amount of DI H 2O Volume I.S. solution0.10 mg/mL 0.10 mL 4.90 mL 5.0 mL1.0 mg/mL 1.0 mL 4.0 mL 5.0 mL5.0 mg/mL 5.0 mL 0 mL 5.0 mL

3. Add 5 drops of 40% sodium hydroxide and 5.0 mL internal standard solution.4. Cap the tubes and place on a rotator for 5 - 10 minutes.5. Centrifuge for 5 - 10 minutes on medium setting.6. Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top; chloroform on the bottom.7. Inject the extracted calibration standards into the GC using the appropriate instrument

method.8. Determine if the data are acceptable using the instructions found in the Calibration

Curve/Response Factor Log. An acceptable calibration curve has a correlationcoefficient, r 2 > 0.995. If the curve is acceptable, file it in the CalibrationCurve/Response Factor Log located in the Drug Laboratory. If not, seek supervisoryassistance as needed.

Quality Control Standard:

Ideally the quality control standard is made from a different lot number or manufacturer than thecalibration stock standard. At a minimum, it should be made from a different stock solution.

A quality control standard must be successfully run on each day this procedure is used.

The concentration, amount, and volume may vary proportionally depending on the availability of drug. The following is provided as a guide:

QC Stock Amount of Drug (as base) Final Volume Solvent2.0 mg/mL Drug 50 mg 25 mL deionized waterTransfer 50.0 mg drug calculated as the free base to a 25 mL volumetric flask, and bring to volumewith deionized water. Mix by inverting flask. Sonicate as needed. Transfer to a 25 mL screw capculture tube for storage.





Quality Control Procedure:

1. Using a volumetric pipette, place 2.5 mL of quality control stock and 2.5 mL DI waterinto a 15 mL labeled, screw cap culture tube. Add 5 drops of 40% sodium hydroxide and

5.0 mL internal standard solution.

QC Standard Amount of QC Stock Amount of DI H 2O Volume of I.S. solution1.0 mg/mL Drug 2.5 mL 2.5 mL 5.0 mL

2. Cap the tube and place on rotator for 5 - 10 minutes.3. Centrifuge for 5 - 10 minutes on medium setting.4. Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top and chloroform on the bottom of the respective water layers.5. Inject the extracted quality control sample into the GC using the appropriate instrument

method.

Evaluation Criteria:

1. If the QC sample is within the set limits of +/- 5% of the target concentration, proceedwith analysis.

2. If the QC sample is not within the set limits of +/- 5% of the target concentration,additional action must be taken to obtain an acceptable QC result such as re-running QC,re-extracting and re-running QC, making new stock with re-extraction and re-analysis, re-calibrating (run curve), and/or consulting a supervisor.

Color Testing:

See the section on Color Testing. Spot tests will usually be run on each item of non-pharmaceuticalevidence within one case up to the applicable statutory weight limit. Color testing may beperformed on pharmaceutical evidence as applicable.

Analytical Procedure :

1) Powdered Samples, Hard Chunky Powders, and Other Solids:a) Obtain the total weight of the material in the exhibit to be analyzed and record on the Drug

Protocol Worksheet.b) Create a representative specimen by taking a sample from many or all of the solid pieces in

the exhibit. If powder is also present, remove a sample and add to the material scraped fromthe solid pieces. Pulverize the resulting composite sample as necessary and analyze asdescribed.

c) GC/MS Identificationi) Transfer approximately 10 mg of material to approximately 1 mL methanol in a test tube.

(1) The analyst will vary the amount of material and methanol as needed to obtain anacceptable mass spectrum.

ii) Vortex and centrifuge as necessary.





(b) Cap the tube and place on rotator for 5 - 10 minutes.(c) Centrifuge for 5 -10 minutes on medium setting.(d) Transfer an aliquot of the organic layer to an autosampler vial. Note: n-

butylchloride will be on the top and chloroform on the bottom.(e) Inject the extracted sample into GC using appropriate instrument method and

calculate the results.

5) Residue Samples: a) Carefully rinse the residue into a container using methanol.b) GC/MS Identification

i) Run a methanol blank before each residue sample using DRUGANA.M or BLANK.Mmethods and place in case file.

ii) Place an aliquot of the methanol washing into an autosampler vial. Analyze by GC/MSusing BLANK.M method.

c) GC Quantitationi) Transfer the sample/methanol mixture to a 15 mL glass screw cap culture tube, add 1-3

drops of methanolic HCl, and evaporate to dryness.ii) Based on the estimated drug concentration of the material, determine the extractionvolume. Add the same amount of water and extraction solvent:(1) Add 1.0 – 5.0 mL of deionized water to residue, 1-5 drops of 40% NaOH, and 1.0-

5.0 mL internal standard solution.iii) Cap the tube and place on a rotator for 5 - 10 minutes.iv) Centrifuge for 5 - 10 minutes on medium setting.v) Run a methanol blank before each residue sample using the same method used for the

sample and place in case file.vi) Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl

chloride will be on the top and chloroform on the bottom.

vii) Inject the extracted sample into GC using the appropriate instrument method andcalculate the results.(1) If it is necessary to dilute the residue, return to the original washing and dilute.

viii) When analysis is complete return any extracted sample remaining in the autosamplervial to the original culture tube used for the extraction.(1) Remove and discard the aqueous layer from the culture tube.(2) Add 1-3 drops of methanolic HCl to the extracted sample to convert the drug to its

more stable hydrochloride salt form.(3) Take the extracted sample to residue, in a laboratory fume hood. Close with

a screw cap.(4) Label the tube “added by laboratory”, include FL# and initials, and place this tube in

the evidence bag along with the evidence.

6) Clandestine Methamphetamine Laboratory Samples: a) Determine whether the liquid sample is aqueous or organic.

i) If the sample is a solid, discuss analysis with supervisor.b) Determine and record pH on Drug Protocol Worksheet.

i) A pH of 1 indicates the presence of concentrated acid. In this case, no further analysis isdone.





See GC and GC/MS Methods Notebooks in Drug Laboratory.

Reporting Criteria:

1. Report both the quantity and the identity of the drug when the concentration of the drug is within+/- 20% of the calibration curve on the GC and the GC/MS is complete. It may be necessary todilute extracted samples to bring them within the curve range.

2. Report the amount of the drug as insufficient for quantitation when the drug concentration isbelow 20% of the calibration curve on the GC and the GC/MS is complete.

Calculations:

1. Dilutionsa. In any situation in which a dilution is made, multiply the concentration of drug (mg/mL) by

the dilution factor. A notation relating to how dilutions were made must be made in the

case file.2. Materials Analyzed by Volume:

a. concentration of drug (mg/mL) x volume of internal standard solution used for extraction(mL) x total exhibit volume/extracted sample volume = mg of drug in the exhibit as thefree base

3. Materials Analyzed by Weight:a. concentration of drug (mg/mL) x volume of internal standard solution used for extraction

(mL) x total exhibit weight (mg)/extracted sample weight (mg) = mg of drug in the exhibit as the free base

4. Percent drug in the exhibit:a. mg of drug in the exhibit/total weight of the exhibit x 100 = % of drug in the exhibit

5. Amount drug in mg/100 mL (typically for codeine cough syrup):a. mg / 100 mL = mg (drug) X 100

Total Volumeof exhibit





Training Notes: Alkaline Procedure

1. If GC/MS results are negative when run on BLANK.M, run on alternative GC/MS methodssuch as LOWDOSE.M, LSD.M, etc. until satisfied that no controlled substance is present.

2. If a substance is dissolved in methanol and is determined to contain acetaminophen by

GC/MS, the material should be extracted using this alkaline procedure and analyzed by GCand GC/MS to determine if codeine or hydrocodone is present.3. GC quantitation of hydrocodone must be performed using chloroform - not n-butyl chloride -

as extracting solvent.4. A sonicator may be used to bring materials into solution. Care should be used regarding the

length of time materials are left in the sonicator since heat may decompose some drugs.Typically, a sonication time of 5 minutes or less is used.

5. Once a quantitation procedure is begun, the extraction procedure should be followed throughto completion and not stopped mid-extraction. Prolonged exposure of drugs to a basicsolution may cause decomposition.

6. The choice of internal standard - phenanthrene or naphthalene - is made to avoid coelution of

the internal standard with the drug.7. The toxicity of n-butyl chloride is less than that of chloroform; therefore, where possible, n-butyl chloride is the extraction solvent of choice. However, extraction efficiency of somedrugs is low or variable in this solvent, and in this case, chloroform is used.

8. Dihydrocodeinone is an alternate name for hydrocodone. It is used to identify hydrocodonepreparations listed in Penalty Group 3. Report as hydrocodone (dihydrocodeinone).

9. If the Marquis color test turns green, the extracted sample must be analyzed by GC/MS inorder to determine if 4-bromo 2, 5-dimethoxyphenethylamine (Polo) is present.

10. Diphenhydramine and ketamine co-elute when run by GCMS using BLANK.M. UseSLOWRAMP.M method if there is evidence of the mixture.

11. TFMPP and MDMA may co-elute when run by GC/MS using BLANK.M. It may be

necessary to use SLOWRAMP.M to resolve these peaks.12. Depending on the solubility of the drug standard in water (salt/base form), the calibration

stock may require a different solvent such as ethanol. Refer to the Merck Index or Clarke’sAnalysis of Drugs and Poisons for solubility information. For non-aqueous solutions take toresidue before proceeding to extraction.

13. Calculation of drug weight as the free base: Option 1To calculate the amount of drug as a salt required to produce a target amount of free base,use the following equation:

MW drug (salt) / MW drug (free base) X target amount of free base

Example: Amphetamine sulfate (C 9H13N)2 H2SO 4 MW = 368.5Amphetamine (base) MW = 135.2

368.5 / 2 X 50 mg = 68.1 mg amphetamine sulfate135.2

Note: Occasionally two molecules of drug are included in the salt form. Check the chemicalformula prior to making standard. In this case, the molecular weight of the salt should bedivided by 2 prior to using the formula above.






14. Calculation of drug weight as the free base: Option 2To calculate the percentage of free base in the salt molecule to produce a target amount, usethe following equation:

Example: Amphetamine sulfate (C 9H13N)2 H2SO 4 MW = 368.5Amphetamine (base) MW = 135.2

135.2 X 2 = 0.734% base in salt = 368.5

Amount of salt needed = 50 mg = 68.1 mg amphetamine sulfate0.734




COCAINE DIRECT DILUTIONCOMBINED QUANTITATIVE AND QUALITATIVE ANALYSIS

Principle of Assay:

This method describes a direct dilution procedure for the identification and quantitation of cocaine in suspected drug samples. Cocaine is simultaneously identified and quantitated usinggas chromatography/mass spectrometry (GC/MS).

In this method, a known amount of suspected drug substance is quantitatively diluted indichloromethane containing phenanthrene as the internal standard and analyzed by GC/MS.

Sample Requirements:

Powders and solids are suitable for analysis. Residues and other specimens suspected of containing cocaine should be analyzed using the Weak Alkaline Drug Analysis.

Equipment:

Gas chromatograph-mass spectrometer with split/splitless injector and mass selective detectorcontaining a methylsiloxane capillary column such as an HP-5MS, 30 m x 0.25 mm x 0.25 umfilm thickness (GC/MS Methods Notebook in Drug Laboratory).

Screw top culture tubes, 25 mL, 20 mm x 125 mm, screw cap with Teflon linerScrew top culture tubes, 15 mL, 16 mm x 125 mm, screw cap with Teflon linerVolumetric flask, 2 mL, 10 mL, 6.0 LHamilton syringes, 100 uL, 250 uL, 500 uL

Autosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsVortex mixerCentrifugeSonicatorRotatorAnalytical balanceAdjustable 10 mL Dispensette Reagent BottlePipettes, variousMortar and Pestle

Reagents:

Phenanthrene, reagent grade or betterDichloromethane (methylene chloride), reagent grade or betterAnalytical standards

Safety Precautions:

Dallas County Institute of Forensic Sciences Cocaine Direct Dilution AnalysisControlled Substances Laboratory 1 Version 2.0




Color Testing:

See the section on Color Tests. Spot tests will typically be run on each item of non-pharmaceutical evidence within one exhibit up to the applicable statutory limit. The color test

must be positive to proceed with this procedure.


1. Obtain the total weight of material in the exhibit and record on the Drug ProtocolWorksheet.

2. Create a representative specimen by taking a sample from many or all of the solid piecesin the exhibit. Pulverize the resulting composite sample and analyze as described.

3. Weigh approximately 10-25 mg of material to be analyzed; record the weight on theDrug Protocol Worksheet.

4. Transfer the sample to a clean 15 mL labeled screw top culture tube.

5. Using a Dispensette Reagent Bottle, add 10 mL of internal standard solution and cap.6. Rotate 5 - 10 minutes, vortex or sonicate as needed, and centrifuge for 5 - 10 minutes on

medium setting.7. Transfer an aliquot to a labeled autosampler vial and cap.8. Inject the sample into the GC/MS using the COCQUANT.M method for

quantitative/qualitative analysis, and calculate the results.


See GC/MS Methods Notebook located in Drug Laboratory.

Reporting Criteria:

1. The reporting range of the assay is +/ -20% of the calibration curve.2. When the concentration of the drug is within the reporting range of the assay, the

retention time of the sample is within 0.03 minutes of the quality control sample, and theGC/MS is complete, report both the quantity and the identity of the drug.

3. When the concentration of the drug is below the reporting range of the assay, theretention time of the drug is not within range, or the GC/MS is incomplete, reanalyzeusing the Weak Alkaline Drug Analysis.

4. If GC/MS is complete but below quantitation limit, reanalyze using the Weak AlkalineDrug Analysis.

5. If no indication of cocaine is present, the material is considered negative for cocaine;however, a sample of the material should be diluted with methanol and injected onto theGC/MS as an unknown using the BLANK.M method.

Calculations:






(mg/mL) by the dilution factor. A notation relating to how dilutions were mademust be made in the case file.

2. Materials Analyzed by Weighta. concentration of drug (mg/mL) x volume of internal standard solution used for

extraction (mL) x total exhibit weight (mg)/extracted sample weight (mg) = mg of

drug in the exhibit as the free base3. Percent drug in the exhibit:a. mg of drug in the exhibit/total weight of the exhibit x 100 = % of the drug in the

exhibit





i) Color changes are as follows:

Drug Color changeAmphetamines orange to brownOpiates violet

Diphenhydramine yellowAmitriptyline red to brownMDA, MDMA, MDEA, N-OH MDA purple to black Aspirin pink to cherry red upon standing

4) Mecke Reagent a) Reagent Preparation:

i) Dissolve 250 mg selenious acid in 25 mL concentrated sulfuric acid.ii) Results:

(1) Color changes are as follows:

Drug Color ChangeOpiates greenDiphenhydramine yellowMDA, MDMA, MDEA, N-hydroxy MDA deep aqua blue to black

5) Sodium Nitroprusside/Acetaldehydea) Reagent Preparation:

i) Solution A:(1) Make a 1% solution of sodium nitroprusside (sodium nitroferricyanide) in water.(2) Add 10% by volume of acetaldehyde.(3) Example: Place 0.9 gram of sodium nitroprusside in 90 mL H 2O. Mix

thoroughly. In a hood, add 10 mL acetaldehyde; watch for bumping. Mix.(4) The stock is refrigerated when not in use.

ii) Solution B:(1) Make a 2% sodium carbonate solution in water.(2) Example: Place 2 grams sodium carbonate in 100 mL H 2O. Mix.

b) Procedure:i) Place a small amount of powder in a spot plate.ii) Add one drop of Solution A followed by two drops of Solution B.iii) An immediate blue color indicates presence of a secondary amine such as

methamphetamine. Amphetamine and other primary amines yield a slow pink tocherry red color.

c) Results:i) Color changes are as follows:

Drug Color ChangeMethamphetamine blueAmphetamine slow pink to cherry redMDEA, MDMA blueMDA negative

Dallas County Institute of Forensic Sciences Color Testing ProcedureControlled Substances Laboratory 3 Version 2.1




6) Ferrous Sulfate for Nitroglycerinea) Reagent Preparation:

i) To one volume of a 10% solution of ferrous sulfate (FeSO 4.7H 2O), add 5 volumes of sulfuric acid with cooling.

ii) For example, mix 0.1 g FeSO 4.7H 2O and 1 mL distilled water; add 5 mL H 2SO 4.

b) Results:i) A red or pink color indicates the presence of nitroglycerine.

7) Silver Nitrate Test for the Presence of Chloride Iona) Reagent Preparation:

i) 5% silver nitrate(1) Dissove 5g silver nitrate in 100 mL deionized water.(2) Mix well.

b) Procedure:i) Place powder in test tube and dissolve in distilled water.ii) Add a few drops of 5% silver nitrate and shake.

iii) A precipitate will form if chloride ions are present.iv) Add a few drops of concentrated nitric acid and shake.

c) Results:i) If precipitate persists, the test is positive for the presence of chloride ions.

8) Van Urk Reagent for Hallucinogensa) Reagent Preparation:

i) Dissolve 2 grams of para-dimethylaminobenzaldehyde in 50 mL of ethanolii) Add 50 mL of concentrated hydrochloric acid.

b) Results:i) Slow development of lavender color indicates presence of LSD, LAMPA, psilocybin,

psilocin, etc.

9) Ferric Chloride Test for GHB a) Reagent Preparation:

i) Dissolve 5 grams ferric chloride in 100 ml deionized water.b) Results:

i) An orange color is consistent with the presence of gamma-hydroxybutyrate (GHB).ii) Gamma-butyrolactone (GBL) and 1,4 butanediol do not produce a color change.``

10) Duquenois-Levine for Marihuana Reagent Preparation:a) Reagent Preparation:

i) Mix 1 gram vanillin, 50 mL ethanol, and ½ mL acetaldehyde.b) Procedure and Results:

i) Refer to the Marihuana Procedure.

Color Test Procedure:

To a clean spot test well, add 1 – 2 drops reagent; then add a small amount of material to betested.





Reporting Criteria:

1) Describe color changes or lack of change on the Protocol Sheet.

Quality Control Procedure

Stock solutions of color test reagents will be made up as needed. They may be prepared in bulk volume and distributed among analysts. After they are made, they will be checked by the personpreparing the solution as well as checked by each analyst before put into use. The color reagentswill be checked with the Color Reagent Test Kit. The test kit contains a variety of drugsnecessary to test the color test reagents including cocaine, MDMA, methamphetamine, PCP,GHB, ephedrine, and marihuana. Materials in the test kit have been removed from cases or havebeen purchased and have been verified by GC/MS and or IR.

Common Reagents and Appropriate Check Compounds

Reagent Check CompoundDuquenois-Levine MarihuanaMarquis Heroin, MDMA, MethamphetamineMecke Heroin, MDMACoSCN Cocaine, PCPVan Urk LSDFeCl 3 GHBNitroprusside Methamphetamine, MDMANegative Control Ephedrine

Procedure:1. At the beginning of each month all routine color testing reagents (Duquenois, Marquis,

Mecke, CoSCN, Nitroprusside) will be checked with a positive and a negative control usingthe Color Reagent Test Kit.

2. The results of the color change will be documented on the Monthly Color Reagent Test Logby the analyst(s) conducting the test(s).

3. If there is no change in color document “NR’ or no reaction.4. If a reagent does not produce the appropriate and expected color change, a second known

standard will be evaluated with the same solution. If this second test also produces anegative response, all reagent bottles with this solution will be collected, discarded, and freshsolution prepared.

5. Non routine color reagents (Van Urk, FeCl 3,) will be checked for validity before use.





SELECTED COLOR TEST OBSERVATIONS

A blank entry indicates no color change

Individual Drugs

DrugCobaltThiocyanide Marquis Mecke

SodiumNitroprusside

AcetaminophenAsprin pink to deep

red4-Bromo-2,5-dimethoxyphenethylamine(Polo)

bright green

BZP blueDextromethorphan blue specks slow black yellow-red deep pink Doxepin blue maroonEphedrine SO 4, EphedrineHCl deep pink Fluoxetine (Prozac) slow blue,

diffuseorange-red slow blue

Guaifenesin purple pink MBDB deep purple deep aqua bright blueMDA deep purple deep aquaMDA, isopropenyl few blue

speckspurple, sparse blue purple

MDA, N-hydroxy few bluespecks purple deep aqua

MDEA deep purple deep aqua bright blueMDMA deep purple deep aqua bright blueMethylphenidate blueN-MethylcathinonePhenethylamine orange deep green,

slowPhentermine orangePropylhexedrine blue orange-brown blueTFMPP blueTramadol blue orange






SELECTED COLOR TEST OBSERVATIONS

Drugs in Combination

Drug

Cobalt

Thiocyanide Marquis Mecke

Sodium

NitroprussideAspirin, Cocaine, andGuaifenesin blue purple maroonEphedrine,Caffeine, andPhenylpropylamine(tablets withgreen specks)

pink

Ephedrine, Cocaine,Guaifenesin

blue purple green-purple

Ephedrine and

Dextromethorphan(speckledround tablet )

blue greenspecks

purpleto black

pink-yellow deep pink

Ephedrine andGuaifenesin

blue specks deep purple deep aqua

Methamphetamine,Guaifenesin, andEphedrine

deep purple-violet

green-violet blue

PhenylpropanolamineandDextromethorphan

blue-greenspecks

purple-black pink-yellow deep pink




DIRECT DILUTION ANALYSIS

Principle of Assay:

This method describes a direct dilution procedure for a number of controlled substances

including many opiates and benzodiazepines. Drugs are identified using analytical techniqueswhich provide conclusive identification of the drug. These techniques include gaschromatography/mass spectrometry (GC/MS), and infrared spectroscopy (IR).

Drugs are usually quantitated by gas chromatography (GC). A known amount of suspected drugsubstance is quantitatively diluted in ethanol containing phenanthrene as the internal standard.

Specific details of quantitation for each drug and its linear range of quantitation may be found inthe Calibration Curve/Response Factor Log for each GC. Examples of drugs analyzed using thedirect dilution procedure follow:

Alprazolam Heroin Oxazepam

Clonazepam Lorazepam PrazepamDiazepam Monoacetylmorphine TemazepamFlunitrazepam Morphine TriazolamFlurazepam Olanzapine

Marked pharmaceuticals will usually be identified by logo match and GC/MS withoutquantitation. However when the penalty group or schedule of a marked pharmaceuticalpreparation is determined by dosage or preparation, sufficient testing should be performed forplacement of the substance in a proper penalty group or schedule.


Powders, solids, tablets, capsules, residues, and plant extracts (for example, raw opium andmorphine base) are suitable for analysis. Liquids are not usually suitable for analysis by thisprocedure.

Equipment:

Gas chromatograph-mass spectrometer containing a methylsiloxane capillary column such as anHP-5MS, 30 m x 0.25 mm x 0.25 um film thickness and gas chromatograph-flame ionizationdetector with split/splitless injector containing a methylsiloxane capillary column such as an HP-1, 15 m x 0.32 mm x 1.0 um film thickness (see GC/MS and/or GC Methods Notebooks in Drug

Laboratory).

Screw top culture tubes, 25 mL, 20 mm x 125 mm, screw cap with Teflon linerScrew top culture tubes, 15 mL, 16 mm x 125 mm, screw cap with Teflon linerVolumetric flask, 5 mL, 10 mL, 25 mL, 500 mLAutosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsHamilton syringe, 250 uLVortex mixer

Dallas County Institute of Forensic Sciences Direct Dilution AnalysisControlled Substances Laboratory 1 Version 2.1




CentrifugeSonicatorTest tubesAnalytical balancePipettes, various

Graduated cylinders, variousAdjustable 2 mL Dispensette Reagent BottleMortar and PestleErlenmeyer flask, 100 mL

Reagents:

Phenanthrene, reagent grade or betterMethanol, reagent grade or betterEthyl Alcohol, USP grade, 200 proof - AbsoluteChloroform, reagent grade or better

HCl, reagent grade or betterSodium bicarbonate, reagent grade or betterAnalytical standardsMethanolic HCl (5%)

Transfer 5 mL concentrated HCl and 95 mL of methanol to a 100 mL Erlenmeyer flask.

Safety Precautions:

The most common type of chemical or biological exposure in this type of laboratory is a splashto the skin or eye. Skin, mucous membranes, or eyes which have been splashed with commonlyused chemicals or biologicals should be thoroughly washed for at least 15 minutes in cool tap

water or eye wash station. Refer to appropriate MSDS’s for additional chemical information.Report the incident immediately to a supervisor. Seek medical attention as necessary.

Methanol and ethanol are flammable solvents. Avoid contact with skin, eyes, and mucousmembranes.

Chloroform is a chlorinated solvent and is considered a human carcinogen. Use in a hood or in awell ventilated area. Avoid contact with skin, eyes, and mucous membranes.

Hydrochloric Acid is corrosive. Avoid contact with skin, eyes, an mucous membranes.



0.5 mg/mLphenanthrene

0.25 g phenanthrene 500 mL ethanol

Weigh 0.25 g phenanthrene, transfer to a 500 mL volumetric flask, and bring to volume withsolvent. Mix by inverting the flask.






All solutions of stocks and standards are kept in the refrigerator. Allow the standards to come toroom temperature before using.

The concentration, amount, and volume of the calibration stock and calibration standards mayvary proportionally depending on the availability of drug and the expected concentration rangeof the drug. The following is provided as a guide.

Calibration Stock Amount of Drug (as base) Volume of I.S solution

2.0 mg/mL Drug 20 mg 10 mL

Transfer 20.0 mg drug calculated as the free base to a 10 mL volumetric flask and bring tovolume with I.S. solution. Mix by inverting the flask. Sonicate as needed. Transfer solution to a15 mL culture tube for storage.



2. Using a Hamilton syringe or a volumetric pipette, place the appropriate amount of calibration stock into a 5 mL volumetric flask. Add I.S. solution to make a total volumeof 5.0 mL. Mix by inverting the flask. Sonicate as needed.

Calibration Standards Amount of Calibration Stock Volume I.S. solution0.10 mg/mL 250 uL Dilute to 5 mL

1.0 mg/mL 2.5 mL Dilute to 5 mL2.0 mg/mL 5.0 mL 0 mL

3. Transfer an aliquot to an autosampler vial. Inject into the GC using the appropriateinstrument method.

4. Determine if the data are acceptable using the instructions found in the CalibrationCurve/Response Factor Log. An acceptable calibration curve has a correlationcoefficient, r 2 > 0.995. If the curve is acceptable, file it in the CalibrationCurve/Response Factor Log located in the Drug Laboratory. If not, seek supervisoryassistance as needed.


Ideally the quality control standard is made from a different lot number or manufacturer than thecalibration stock. At a minimum, it should be made from a different stock solution.


The concentration, amount, and volume may vary proportionally depending on the availability of





drug. The following is provided as a guide:

QC Stock Amount of Drug (as base) Volume of I.S. solution1.0 mg/mL Drug 10 mg 10 mLTransfer 10.0 mg drug calculated as the free base to a 10 mL volumetric flask and bring tovolume with internal standard (I.S.) solution. Mix by inverting the flask. Sonicate as needed.Transfer solution to a 15 mL culture tube for storage.


1. Transfer an aliquot of QC Stock to an autosampler vial, inject into GC using theappropriate instrument method.

QC Standard Amount of Drug (as base) Volume of I.S solution1.0 mg/mL Drug Use QC Stock -----------



2. If the QC sample is not within the set limits of +/- 5% of the target concentration,additional action must be taken to obtain an acceptable QC result such re-running QC, re-prepping and re-running the QC, making new stock solution and reanalyzing,recalibrating (run curve), and/or consulting a supervisor.

Color Testing:

See the section on Color Tests. Spot tests will typically be run on each item of non-pharmaceutical evidence within one exhibit up to the applicable statutory limit. Color testingmay be performed on pharmaceutical evidence as applicable.


1. Powder Samples and Other Solids: a. Obtain the total weight of the suspected drug material to be analyzed and record

on the Drug Protocol Worksheet.b. Create a representative specimen by taking a sample from many or all of the solid

pieces in the exhibit. If powder is also present, remove a sample and add to thematerial scraped from the solid pieces. Pulverize the resulting composite sampleand analyze as described.

c. GC/MS Identificationi. Transfer approximately 10 mg of material to be analyzed to approximately

1 mL methanol in a test tube.1. The analyst will vary the amount of material and methanol as

needed to obtain an acceptable mass spectrum.





ii. Vortex and centrifuge as necessary.iii. Transfer an aliquot to an autosampler vial and inject on the GC/MS using

BLANK.M method.d. GC Quantitation

i. Weigh approximately 10 - 50 mg of the material to be analyzed, and

record the weight on the Drug Protocol Worksheet.ii. Transfer sample to a 15 mL labeled screw cap culture tube.iii. Add 1.0 - 5.0 mL of internal standard solution depending upon the

expected concentration of the drug; document the volume used on theDrug Protocol Worksheet.

iv. Rotate for 5 - 10 minutes. Vortex or sonicate as needed.v. Centrifuge for 5-10 minutes on medium setting.

vi. Transfer an aliquot to an autosampler vial, inject the sample into GC usingthe appropriate instrument method, and calculate the results.

2. Tablets, Capsules, and Other Pharmaceutical Preparations:

a. Obtain the total weight of the suspected drug material to be analyzed and recordon the Drug Protocol Worksheet.b. Create a representative sample for analysis:

i. Capsules – typically a composite sample is used for analysis.ii. Tablets – typically one tablet is selected for analysis.

c. Logo Identificationi. Refer to Pharmaceutical Analysis Procedure.

d. GC/MS Identificationi. Transfer an amount of sample that is equivalent to approximately 1 mg of

drug to approximately 1 mL methanol in a test tube.1. The analyst will vary the amount of material and methanol as

needed to obtain an acceptable mass spectrum.ii. Vortex and centrifuge as necessary.

iii. Transfer an aliquot to an autosampler vial and inject on the GC/MS usingBLANK.M method.

e. GC Quantitationi. Weigh approximately 10 - 50 mg of material to be analyzed and record on

the Drug Protocol Worksheet.ii. Transfer sample to a 15 mL labeled screw cap culture tube.

iii. Add 1.0 - 5.0 mL of internal standard solution depending upon theexpected concentration of the drug and record the volume on the DrugProtocol Worksheet.

iv. Rotate for 5 - 10 minutes. Vortex and sonicate as needed.v. Centrifuge for 5-10 minutes on medium setting.

vi. Transfer an aliquot to an autosampler vial, inject the sample into the GCusing the appropriate instrumental method, and calculate the results.

3. Residue Samples:a. Carefully rinse the residue into a small container using methanol. Make a

notation that the specimen is a residue on the Drug Protocol Worksheet.





b. GC/MS Identificationi. Run a methanol blank before each residue sample using DRUGANA.M

or BLANK.M methods and place in case file.ii. Place an aliquot of the methanol washing in an autosampler vial.

iii. Vortex and centrifuge as necessary.

iv. Inject on the GC/MS using BLANK.M method.c. GC Quantitationi. Place the sample/methanol mixture in a 15 mL labeled screw top culture

tube, add 1-3 drops of methanolic HCl and evaporate to dryness.ii. Based on the estimated drug concentration of the material, determine the

dilution volume. Add 1.0 - 5.0 mL of internal standard solution.iii. Sonicate for 5 - 10 minutes.iv. Centrifuge for 5-10 minutes on medium setting.v. Transfer an aliquot to an autosampler vial.

vi. Run a methanol blank before each residue sample using the same methodused for the sample and place in case file.

vii. Inject the sample into the GC using the appropriate instrument method,and calculate the results.d. When analysis is complete return any sample remaining in the autosampler vial to

original culture tube.e. Under a laboratory fume hood, add 1-3 drops of methanolic HCl to the sample

and evaporate to dryness.f. Label the tube “added by the laboratory”, include FL#, initials, and place this tube

in the evidence bag along with the evidence.

4. Low Dose Heroin Identification:a. When low dose heroin is “cut” with acetaminophen, GC/MS identification of

heroin may be obscured by the acetaminophen. The following procedureseparates acetaminophen from heroin and improves the GC/MS. Quantitation of heroin is performed using Procedure 1 above. Make a notation on the DrugProtocol Worksheet when this procedure is used.

b. GC/MS Identificationi. Dissolve 20-30 mg sample in approximately 1 mL of water in a test tube.

1. The analyst will vary the amount of material as needed to obtain anacceptable mass spectrum.

ii. Add NaHCO 3, and approximately 1mL of chloroform.iii. Centrifuge as necessary.iv. Transfer an aliquot of the chloroform layer (bottom) to an autosampler

vial and inject the sample into the GC/MS using BLANK.M method.


See GC and GC/MS Methods located in Drug Laboratory.

Reporting Criteria:





1. Report both the quantity and the identity of the drug when the concentration of the drugis within +/- 20% of the calibration curve on the GC and the GC/MS is complete. It maybe necessary to dilute extracted samples to bring them within the curve range.

2. Report the amount of the drug as insufficient for quantitation when the drugconcentration is below 20% of the calibration curve on the GC and the GC/MS is

complete.

Calculations:



2. Materials Analyzed by Weighta. concentration of drug (mg/mL) x volume of internal standard solution used for

extraction (mL) x total exhibit weight (mg)/extracted sample weight (mg) = mg of

drug in the exhibit as the free base3. Percent drug in the exhibit:

a. mg of drug in the exhibit/total weight of the exhibit x 100 = % of the drug inthe exhibit





Training Notes: Direct Dilution Analysis

1. If GC/MS results are negative when run on BLANK.M, run on alternative GC/MSmethods such as LOWDOSE.M, LSD.M, etc. until satisfied that no controlled substanceis present.

2. When analyzing a morphine sulfate tablet add approximately 100 mg of NaHCO 3 to theinternal standard solution before sonication.3. A sonicator may be used to bring materials into solution. Care should be used regarding

the length of time materials are left in the sonicator since heat may decompose somedrugs. Typically, a sonication time of 5 minutes or less is used.

4. Liquid morphine exhibits are typically quantitated using the Morphine Syrup Analysisprocedure.

5. The heroin monohydrate standard is most often purchased in dilutable form. It isacceptable to prepare and store the solution in the dilutable vial.

6. Identify material as opium when morphine plus four of the following alkaloids (codeine,noscapine, thebaine, papaverine, meconin) are present. Quantitation is not necessary.

Report total weight of material.7. Black tar heroin is frequently encountered as a sticky solid material. It may be necessaryto freeze the sample for 5-10 minutes before proceeding with analysis.

8. Calculation of drug as free base: Option 1To calculate the amount of drug as a salt required to produce a target amount of free base,use the following equation:


Note: Occasionally two molecules of drug are included in the salt form, forexample morphine sulfate. Check the chemical formula prior to making the

standard. In the case of morphine sulfate, the molecular weight of the salt shouldbe divided by 2 prior to using the formula above.

Example : Diacetylmorphine HCl Monohydrate (heroin) C 21H23NO 5 HCl, H 2OMW = 423.9

Diacetylmorphine (base) MW = 369.4

423.9 X 10 mg heroin base = 11.5 mg diacetylmorphine HCl monohydrate (heroin)369.4

9. Calculation of drug as free base: Option 2

Alternatively, to calculate the percentage of free base in the salt molecule to produce atarget amount, use the following equation:

Example : Diacetylmorphine HCl Monohydrate (heroin) C 21H23NO 5 HCl, H 2OMW = 423.9

Diacetylmorphine (base) MW = 369.4






369.4 = 0.871% base in salt = 423.9

Amount of salt needed = 10.0 mg = 11.5 mg heroin0.871




4) Refer to the Appendix for acceptable criteria.E. Running a Polystyrene Scan (Monthly)

1) Click on the Instrument icon.i. Under the Sample tab, name the scan.

ii. Under the Scan tab the range start is 4000 cm -1, end is 515 cm -1, the scan

type should be sample, the units should be %T, the scan should not beminimized, and the duration should be set to 32 scans.iii. Under the Instrument tab the resolution should be 4 cm -1.iv. Under the Beam tab, click on the red disk with holes. Select polystyrene

and hit OK.2) Click Apply. This button will then change to Scan. Click to begin polystyrene

scan.3) Print the polystyrene spectra. Make sure the absorption bands have been

integrated by clicking on the ‘Peaks’ icon in the toolbar, evaluate and initial, andplace the spectra in the FTIR QC Logbook.

4) Refer to the Appendix for acceptable polystyrene criteria.


A positive control (procaine hydrochloride), and a negative control (blank) must be successfullyrun on each day this procedure is used. Review and initial the spectra. Place the spectra in theFTIR QC Logbook. Refer to appendix for acceptable criteria.

Negative ControlA. A negative control must be performed before the positive control.B. Follow the procedure below for running a positive control; however, omit step two.

Positive Control: Procaine HCLA. Click on the Instrument icon.B. Add a small amount of procaine HCl to the crystal.C. Move the pressure arm directly over your sample. Monitor the force gauge as you

tighten the pressure arm (should be ~ 75 for each sample). Click Stop.D. Under the Sample tab, type in the necessary information about your sample.E. Under the Scan tab make sure the range start is 4000 cm -1, end is 515 cm -1, the scan type

should be sample, the units should be %T, the scan should not be minimized, and theduration should be 32 scans.

F. Under the Instrument tab the resolution should be 4 cm -1.G. Under the Beam tab, click on the red disk with holes. Select none and click OK.

H. Click Apply. This button will then change to Scan. Click to begin sample scan.I. Integrate and print the procaine spectra. Review and initial and place in the FTIR QC

Logbook.J. Refer to the ‘Operation of the Spectrum One FTIR’ procedure for printing reports.K. Refer to the Appendix for acceptable procaine hydrochloride spectrum.


Negative Control

Dallas County Institute of Forensic Sciences FTIRControlled Substances Laboratory 3 Version 2.0




A. A negative control must be performed before each sample (include in case file).B. Follow the procedure below for running a sample; however, omit step two and three.

Running a SampleA. Click on the Instrument icon.B. Sampling procedure:

a. Solid samples:i. Cover the crystal with sample. Move the pressure arm directly over yoursample. Monitor the force gauge as you tighten the pressure arm (shouldbe ~ 75 for each sample).

b. Liquid samplesi. Place a drop or two of liquid directly on the ATR crystal. Use enough

sample to cover the crystal completely. Place the pressure arm directlyover the sampling area to prevent evaporation during analysis. Do nottighten the arm.

C. Click Stop.D. Under the Sample tab, type in the necessary information about your sample.

E. Under the Scan tab make sure the range start is 4000 cm-1

, end is 515 cm-1

, the scan typeshould be sample, the units should be %T, the scan should not be minimized, and theduration should be 32 scans.

F. Under the Instrument tab, the resolution should be 4 cm -1.G. Click Apply. This button will then change to Scan. Click to begin sample scan.

Corrective Action:

If the polystyrene standard spectrum, system suitability check, instrument validation,background check, or the negative and positive controls do not meet the acceptance criteria inthe Appendix, the analyst should tag the instrument as “out of service” and advise a supervisor

immediately. Maintenance and repair is recorded in the FTIR Maintenance Logbook.





Appendix

Criteria for an Acceptable Instrument Validation Check are as follows:1) The observed value must fall within specification (upper/lower limit) resulting in

a result of ‘pass’, otherwise the analyst should tag the instrument as “out of service”

and advise a supervisor immediately. Maintenance and repair is recorded in the FTIR QC Logbook.

Abscissa TestTarget (cm -1) Upper Limit (cm -1) Lower Limit (cm -1)3060.00 3062.00 3058.001601.00 1603.00 1598.001028.00 1030.00 1025.00Ordinate Test

Upper Limit (cm -1) Lower Limit (cm -1)3990.00 cm -1 (%T) 80.00 60.00

1030.00 cm-1

(%T) 40.00 20.002000.00 cm -1 (%T) 5.00 -5.00Noise Test Range: 1200 to 1000 cm -1

LimitRMS (%T) 0.0500Peak to Peak (%T) 0.5000Trend (%T) 0.0500

Criteria for Acceptable System Suitability Check are as follows:1) The observed value must fall within specification (upper/lower limit) resulting in

a result of ‘pass’, otherwise the analyst should tag the instrument as “out of service”

and advise a supervisor immediately. Maintenance and repair is recorded in the FT-IR QC Logbook.

Abscissa TestTarget Upper Limit (cm -1) Lower Limit (cm -1)3060.00 3062.00 3058.001601.00 1603.00 1598.001028.00 1030.00 1025.00Noise Test Range: 1200 to 1000 cm -1

LimitRMS (%T) 0.0620

Peak to Peak (%T) 0.3256Trend (%T) 0.0218Throughput TestPeak (cm -1) Lower Limit4000.00 80.002600.00 80.001000.00 80.00Contamination Test





Peak range (cm -1) Upper Limit3100 - 2800 0.1001800 - 1600 0.1001400 - 1100 0.100

Criteria for an acceptable background check are as follows:

1) Compare the background check with the one illustrated below.2) The background spectrum should have the same general shape and appearance as

illustrated below.

Criteria for an acceptable polystyrene standard are as follows:

1) Compare the test spectra with the one illustrated above.





2 1604 +/- 23 1268 +/- 24 1170 +/- 25 1114 +/- 26 770 +/- 2

Criteria for an Acceptable Spectrum are as follows:1) The baseline of the spectrum should be relatively flat2) The signal to noise ratio (SNR) should be high (low noise on the spectrum)3) The sample spectrum should compare favorably with a spectrum of a known standard

in both its overall appearance and in the presence and location of the major peaks.

Training Notes: FTIR Procedure






1. The purpose of a background spectrum is to eliminate the instrument response and featuresintroduced into sample spectra by atmospheric absorption or a cell sampling accessory.When a sample spectrum is collected it is ratioed against the current background spectrumthus removing all instrumental characteristics. All spectral features present are strictly due tosample.

2. Absorption bands shown on a background scan are that of a proprietary polymer coating onthe detector of the instrument. The coating protects the window on the detector from watervapor attack.

3. Care must be exercised with KRS-5 crystals as they may become scratched over time withuse. It is advised that energy throughput is recorded and the spectrum of the ATR accessoryand crystal obtained when the crystal is new. The data should be stored for future referenceto compare the performance of the crystal and accessory at a later date.

4. Clean the crystal and pressure arm before and after analysis with acetone or methanol soakedKimWipes.




LYSERGIC ACID DIETHYLAMIDE (LSD) ANALYSIS

Principle of Assay:

This analysis is designed to identify and quantitate lysergic acid diethylamide (LSD). LSD is

identified by gas chromatography/mass spectrometry (GC/MS) and quantitated by gaschromatography (GC). The GC method separates LSD from its isomer lysergic acidmethypropylamide (LAMPA).


This method is suitable for analysis of LSD in a wide variety of matrices including blotter papersquares, candy, tablets, liquid solutions, and other types of evidence. It is imperative tounderstand the definition of “abuse unit” as described in the Texas Controlled Substances Actprior to analysis.

Equipment:

Gas chromatograph-mass spectrometer containing a methylsiloxane capillary column such as anHP-5MS, 30 m x 0.25 mm x 0.25 um film thickness and/or gas chromatograph-flame ionizationdetector with split/splitless injector containing a methylsiloxane capillary column such as an HP-1, 15 m x 0.32 mm x 1.0 um film thickness (see GC/MS and/or GC Methods Notebook in DrugLaboratory).

Screw top culture tubes, 25 mL, 20 mm x 125 mm, screw cap with Teflon linerScrew top culture tubes, 15 mL, 16mm x 125 mm, screw cap with Teflon linerScrew top conical tubes, 5 mL, screw cap with Teflon liner

Autosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsPipettes, variousHamilton syringes, variousBeaker, 50 mLVolumetric flasks, 5 mL, 25 mLVortex mixerSonicatorScissorsCentrifugeLong range UV light source

Reagents:

Methanol, reagent grade or betterEthyl Alcohol, USP grade, 200 proof-absoluteAnalytical Standards

Dallas County Institute of Forensic Sciences LSD AnalysisControlled Substance Laboratory 1 Version 2.1




Safety Precautions:

The most common type of chemical or biological exposure in this type of laboratory is a splashto the skin or eye. Skin, mucous membranes, or eyes which have been splashed with commonly

used chemicals or biologicals should be thoroughly washed for at least 15 minutes in cool tapwater or eye wash station. Refer to appropriate MSDS’s for additional chemical information.Report the incident immediately to a supervisor. Seek medical attention as necessary.

Methanol and ethanol are flammable solvents. Avoid contact with skin, eyes, and mucousmembranes.

LSD is a hallucinogenic substance, which is active in small dosages. Wear gloves and use otherprecautionary procedures while handling the standard to limit accidental exposure during use.Avoid contact with skin, eyes, and mucous membranes.


Internal Standard Amount of Drug (as HCl) Final Volume Solvent0.5 mg/mL trazodone HCl 12.5 mg 25 mL ethanolTransfer 12.5 mg trazodone hydrochloride to a 25 ml volumetric flask and dilute to volume withethanol. Mix by inverting. Sonicate as needed. Transfer to a 25 mL culture tube for storage.


All solutions of stocks and standards are kept in the refrigerator. Allow the solutions to come toroom temperature before using them.

The concentration, amount, and volume of the calibration stock and calibration standards mayvary proportionally depending on the availability of drug, and the expected concentration rangeof the drug. The following is provided as a guide.

Calibration Stock Amount of Drug (as base) Final Volume Solvent1.00 mg/mL LSD 10.0 mg 10 mL I.S. solutionTransfer 10 mL of I.S. solution using a volumetric pipette to the dilutable bottle containing thedrug. Mix by inverting bottle.


1. Choose a minimum of four appropriate calibration standards for the calibration curvebased on the linear range required for the sample or drug to be analyzed.

2. Using a Hamilton syringe, place the appropriate amount of calibration stock and I.Ssolution into a 5 mL conical screw cap tube. Vortex.





Calibration Standards Amount of Calibration Stock Volume I.S. Solution0.10 mg/mL LSD 10 uL 90 uL0.25 mg/mL LSD 25 uL 75 uL0.75 mg/mL LSD 75 uL 25 uL1.00 mg/mL LSD 100 uL 0

3. Transfer from the conical tube to an autosampler vial with a glass insert.4. Inject into the GC using LSD.M method.5. Determine if the data are acceptable using the instructions found in the Calibration

Curve/Response Factor Log.a. An acceptable calibration curve has a correlation coefficient, r 2 > 0.995.b. If the curve is acceptable, file it in the Calibration Curve/Response Factor Log

located in the Drug Laboratory. If not, seek supervisory assistance as needed.




QC Stock Amount of Drug (as base) Final Volume Solvent1.00 mg/mL LSD 10.0 mg 10 mL I.S. solutionTransfer 10 mL of I.S. solution using a volumetric pipette to the dilutable bottle containing thedrug. Mix by inverting bottle.


1. Using a Hamilton syringe, place the appropriate amount of QC stock and I.S solution intoa 5 mL conical screw cap tube. Mix well.

QC Standard Amount of QC Stock Volume of I.S. solution0.25 mg/mL LSD 0.50 mL 1.50 mL

2. Transfer from the conical tube to an autosampler vial with a glass insert.3. Inject into the GC using LSD.M method.


1. If the QC sample is within the set limits of +/- 10%, proceed with analysis.2. If the QC sample is not within the set limits of +/-10% of the target concentration,

additional action must be taken to obtain an acceptable QC result such as re-running QC,re-prepping and re-runnning the QC, making new stock solution and re-analyzing,recalibrating (run curve), and/or consulting a supervisor.





LAMPA Standard:

LAMPA Standard Amount of Drug (as base) Final Volume Solvent1.0 mg/mL LAMPA 10 mg 10 mL I.S. solutionTransfer 10 mL of I.S. solution using a volumetric pipette to the dilutable bottle containing the

drug. Mix by inverting bottle.

LSD/LAMPA Standard:

LSD (0.5 mg/mL)LAMPA (0.5 mg/mL) Combined Standard

Amount of LSD QC Stock

0.5 mLAmount of LAMPA Standard0.5 mL

Transfer 0.5 mL LSD QC stock and 0.5 mL LAMPA standard to an autosampler vial. Mix welland inject using LAMPA.M method.


1. If the LSD/LAMPA peaks are resolved and identified on the chromatogram, include incase file. This LSD retention time is used for identification of sample.

2. Seek supervisory assistance if peaks are not resolved.

Color Testing:

1. If sufficient sample is available, color test using the Van Urk reagent; for example, select4 squares at random for testing.

2. In addition, long range UV light may indicate presence of drug on items such as candyand sugar cubes, etc.


Note: The final report should contain the weight of LSD quantitated in the exhibit(s) analyzed(when possible) and the number of abuse units as defined by the Texas Controlled SubstancesAct.

“Abuse unit” is defined as follows:(A) except as provided by Paragraph (B):

(i) a single unit on or in any adulterant, dilutant, or similar carrier medium,including, marked or perforated blotter paper, a tablet, gelatin wafer, sugar cube,or stamp, or other medium that contains any amount of a controlled substancelisted in Penalty Group 1-A, if the unit is commonly used in abuse of thatsubstance; or

(ii) each quarter-inch square section of paper, if the adulterant, dilutant, or carriermedium is paper not marked or perforated into individual abuse units; or

(B) if the controlled substance is in liquid form, 40 micrograms of the controlled substance





including any adulterant or dilutant.

1. Paper Squares, Sheets, Sugar Cubes, and Tablets :a. Use the information above to determine the number of abuse units in the exhibit to be

analyzed. For paper sheets, the total area of exhibit must be determined. Record on the

Drug Protocol Worksheet.b. Add 1-2 sugar cubes or tablets, 2 to 4 cut paper squares or quarter-inch square sectionsof paper into a 15mL screw cap culture tube.

i. Record on the Drug Protocol Worksheet.c. Add 1-2 ml methanol, cap and sonicate for 20 minutes.d. Centrifuge for 5 minutes.e. Transfer methanol to a 5 mL conical test tube.f. Rinse culture tube with a few drops of methanol and add to the extract in conical test

tube.g. Place conical test tube in warm water bath and evaporate to residue with air.h. Add at least 100-200 uL of trazodone internal standard solution and vortex to dissolve.

i. Record the volume on the Drug Protocol Worksheet.i. Transfer to autosampler vial with glass insert.

j. Inject the same vial on both GC and GC/MS using LSD.M method.k. Run LSD/LAMPA standard on the GC using LAMPA.M method; include

chromatogram in case file.

2. Liquid Solutions: a. Record the total weight and volume on the Drug Protocol Worksheet.b. Determine the number of abuse units.

i. Record on the Drug Protocol Worksheet.c. Place 40-50 uL into a 5 mL conical test tube. Record the volume on Drug Protocol

Worksheet.d. Add 100-200 uL of trazodone internal standard solution and vortex to dissolve.

i. Record the volume on Drug Protocol Worksheet.e. Transfer to autosampler vial with glass insert.f. Inject the same vial on both GC and GC/MS using LSD.M method.g. Run LSD/LAMPA standard on the GC using LAMPA.M method; include


3. Sweetarts: a. Note: This procedure allows LSD identification but not quantitation.b. Determine the number of abuse units based on number of items (20 Sweetarts = 20

abuse units).i. Record on the Drug Protocol Worksheet.

c. If long range UV light shows fluorescent spots, scrape fluorescent area from 2-3 itemsand place into 15 mL screw cap culture tube.

d. If no fluorescent spots are visible, use 1-2 candies for extraction.e. Record materials tested on Drug Protocol Worksheet.f. Wash with three 5 ml portions of nBuCl:

i. Add 5 mL solvent along with approximately 200 mg NaHCO 3 to culture tube,





rotate 5 minutes, centrifuge and collect supernatant in 50 mL beaker.ii. Repeat process two more times.

g. Take solvent to residue.h. Reconstitute with approximately 0.5 mL trazodone internal standard solution.i. Mix well by vortexing.

j. Transfer to autosampler vial insert.k. Inject same vial on both the GC and GC/MS using LSD.M method.l. Run LSD/LAMPA standard on the GC using LAMPA.M method; include



See GC and GC/MS Methods Notebooks located in Drug Laboratory.

Reporting Criteria:

1. The reporting range of this assay is +/ -20% of the calibration curve.2. If the concentration of LSD is below this range and an acceptable GC/MS spectra is

obtained, reanalyze using more sample or report as present but insufficient for quantitation.3. The final report should contain the weight of LSD quantitated in the exhibit(s) analyzed (if

possible) and the number of abuse units as defined by the Texas Controlled Substances Act.

Calculations:

1. Materials Analyzed by Weight or Volume (with exception of liquids)a. concentration of drug (mg/mL) x volume of internal standard solution

used for extraction x 1000 ug/mg = ug LSD in the dosage unit(s) tested

2. Liquid Materials (only)a. concentration of drug (mg/mL) x volume of internal standard solution

used for extraction x total weight of exhibit (mg) / total weight of sample analyzed(mg) x 1000 ug/mg = ug LSD


(mg/mL) by the dilution factor. A notation relating to how dilutions were made mustbe made in the case file.






Training Notes: LSD Analysis

1. A sonicator is necessary to bring materials into solution. Care should be used regarding thelength of time materials are left in the sonicator since heat may decompose some drugs.Typically, a sonication time of 20 minutes has been found to be effective with regard to good

recovery and minimal decomposition.2. LAMPA and LSD are structural isomers. LAMPA is not scheduled. These substances areresolved by gas chromatography.

3. LSD is light sensitive and degrades with exposure to light. Protect standards from light byusing amber bottles, covering bottles with aluminum foil, etc.

4. LSD may also be detected using long wave UV light.




Dallas County Institute of Forensic Sciences Marihuana AnalysisControlled Substances Laboratory 1 Version 2.0

MARIHUANA AND TETRAHYDROCANNABINOL ANALYSIS

Principle of Assay:

Marihuana is defined by the Texas Controlled Substances Act:

“Marihuana” means the plant Cannabis sativa L., whether growing or not, the seeds of that plant, and every compound, manufacture, salt, derivative, mixture, or preparation of that plant or its seeds. The term does not include:

(A) the resin extracted from a part of the plant or a compound, manufacture,salt derivative, mixture, or preparation of the resin;

(B) the mature stalks of the plant or fiber produced from the stalks;(C) oil or cake made from the seeds of the plant;(D) a compound, manufacture, salt, derivative, mixture, or preparation of the

mature stalks, fiber, oil, or cake; or

(E) the sterilized seeds of the plant that are incapable of beginninggermination.

Non-marihuana material, such as hashish, which contains tetrahydrocannabinol is alsoscheduled.

Marihuana contains more than 400 chemicals. Approximately 60 cannabinoids are present in theplant. (-) Delta 9- trans-tetrahydrocannabinol (levo isomer) is the principal psychoactiveingredient of the marijuana.

This method describes a qualitative procedure for identification of marihuana from plant material

and tetrahydrocannabinol from non-marihuana substances. Identification of marihuana is madeusing color test (Duquenois-Levine), macroscopic and microscopic examination, and GC/MSanalysis for the presence of tetrahydrocannabinol (THC). Non-marihuana substances – such ashashish - are identified using GC/MS to identify THC and positive Duquenois-Levine color test;microscopic analysis must exclude the material as marihuana.

Equipment:

Gas chromatograph-mass spectrometer (GC/MS) containing a methylsiloxane capillary columnsuch as an HP-5MS, 30 m x 0.25 mm x 0.25 um film thickness with split/splitless injector (seeGC/MS Notebook in Drug Laboratory).

StereomicroscopeAnalytical and top-loading balanceDisposable culture test tubes, 12 mm x 100 mmAutosampler vials, 32 mm x 11 mm, Teflon lined sealsVortex mixerDisposable test tubes, 16 x 100 mmBeaker, Parafilm, and paper towels for seed germination





Reagents:

Methanol, reagent grade or betterEthanol, reagent grade or betterDuquenois-Levine reagent (see Color Testing Procedure)

Hydrochloric acid, reagent grade or betterChloroform, reagent grade or better

Safety Precautions:


Methanol is a flammable solvent. Avoid contact with skin, eyes, and mucous membranes.

Concentrated hydrochloric acid is a corrosive. Avoid contact with skin, eyes, and mucousmembranes. Vapors are also corrosive and will corrode metal. Use concentrated acid in a hood.

Chloroform is a chlorinated solvent and is considered a human carcinogen. Use in a hood orwell ventilated area. Avoid contact with the skin, eyes, and mucous membranes.

Overgrowth of mold and presence of mold spores may occasionally be observed in marihuanacases. If these cases must be analyzed, processing must be done in a hood. Seek supervisoryassistance as needed.


Plant materials, oils, solids, residues, and other types of drug evidence are suitable for analysisusing this procedure. Plant material should be dried prior to storage to prevent decomposition.

Sample Preparation:

Obtain the total weight of the suspected drug material minus the packaging. Remove stems orstalks greater than ¼ inch in diameter and note on the Marihuana Identification Protocol sheet.

Color Testing:

See section on Color Testing for preparation of Duquenois-Levine reagent.


This is a qualitative procedure. Results of testing are compared to known characteristics of marihuana or tetrahydrocannabinol verified in this Laboratory using known marihuana or





plant material, hashish, other marihuana preparations, and tetrahydrocannabinol.b) Add approximately 25 mg of suspected material to a disposable test tube.c) Add approximately 2 mL Duquenois-Levine reagent.d) Mix and let settle.e) Add an approximately equal amount of concentrated hydrochloric acid.

f) Mix.i) A deep blue-purple color will develop with marihuana or tetrahydrocannabinol.g) Add enough chloroform to form a visible second layer of liquid.h) Mix and allow to stand until the organic and aqueous layers separate.i) A positive test results when the purple color extracts into the bottom (organic) layer.

i) Note: This test may also be performed on the dried petroleum ether extract of plantmaterial.

4) GC/MS Analysis:a) Place approximately 0.1 g plant material, 1 drop of oil, or aliquot of specimen into a

disposable test tube.

i) The analyst will vary the amount of material as needed to obtain an acceptable massspectrum.b) Add enough methanol to cover sample or dilute to an appropriate concentration for

analysis.c) Mix and allow to separate.d) Place an aliquot of the methanol into an autosampler vial and inject onto the GC/MS for

the identification of tetrahydrocannabinol.

5) Seed Germinationa) Seed germination is performed upon request or when the analyst judges it to be

appropriate.

i) If a submitted exhibit is primarily seeds and not plant material, the analyst shoulddiscuss the case with a supervisor.

b) Label a beaker with the case and exhibit number.c) Take approximately 5-10 seeds randomly from the marihuana exhibit and place between

two sheets of moist paper towel. Fold the paper towel into a packet with the seeds insideand place into a beaker. Cover the beaker with Parafilm.

d) Place the beaker in a dark evidence locker at room temperature for about 3-7 days.e) Inspect the seeds to determine if germination has occurred.f) If germination occurs

i) Photograph the seeds and place the photo in the case file.(1) Label the photo with the case number, exhibit number, date, and your initials;

include a ruler in the photo if applicable.(2) Include the weight of seeds in the weight of marihuana reported.

g) If no germination occursi) Take approximately one ounce of marihuana from the exhibit.ii) Weigh the sample.iii) Separate the seeds.iv) Weigh the seeds.v) Calculate the fraction of seeds in the marihuana sample.





vi) Multiply the gross weight of marihuana by this percent to obtain the total amount of non-germinable seeds.

vii) Subtract this from the gross weight of marihuana to obtain the net weight of marihuana without germinable seeds.

viii) Calculations follow:

(1) (weight of seeds from plant material sample)/(weight of plant material sample) =fraction of seeds in plant material(2) fraction of seeds in plant material x gross weight of marihuana = gross weight of

non-germinable seeds(3) gross weight of marihuana – gross weight of non-germinable seeds = net weight

of marihuana without non-germinable seeds

6) Non-Marihuana Substances Containing THC a) Examples of non-marihuana substances containing THC areb) Hashish/hash - a THC rich resinous material isolated from marihuana. It varies in color

from light tan, green, brown, or black and in texture from soft to very hard.

Microscopically, hashish contains free or unattached cystolithic hairs, simple hairs, andglandular hairs; it may also contain small fragments of torn leaf tissue.

c) Hash oil - a viscous liquid made by solvent extraction of marihuana to concentrate THCand other cannabinoids. It is usually a viscous liquid which may range from amber todark brown in color. Hash oil is typically free of plant fragments.

d) Microscopic Analysis - These materials will not show typical microscopic morphologyfor marihuana. Although, hashish will usually contain characteristic hairs frommarihuana, there will be very little intact leaf material present.i) The analyst must use microscopy to distinguish between powdered marihuana and

hashish. Powdered marihuana will usually contain intact leaf fragments containingcystolithic and simple hairs consistent with characteristic marihuana morphology.

Powdered marihuana is reported as marihuana; hashish is reported as containingtetrahydrocannabinol. It is recommended that these cases be reviewed with asupervisor.

e) Duquenois-Levine and GC/MS – The Duquenois-Levine will be positive and GC/MSwill be positive for THC and typically either cannabinol or cannabidiol.

f) Reporting - Non-marihuana substances which contain THC are reported as containingtetrahydrocannabinol.

7) Pipe Residue a) Rinse the pipe residue with methanol.b) Place methanol in a GC/MS vial and analyze for THC.

c) Return the contents of the GC/MS vial to the residue tube and dry down.d) Perform the Duquenois-Levine test on the residue.e) If the Duquenois-Levine is positive and THC is present, the case is reported: the charred

residue in the pipe contained tetrahydrocannabinol.

Instrument Parameters :

See GC/MS Methods Notebook located in the Drug Laboratory.





Reporting Criteria:

1. Marihuana is identified if both the microscopic and Duquenois-Levine tests are positivefor marihuana. Tetrahydrocannabinol in marihuana is identified by GC/MS; at least one

GC/MS will be run on each marihuana case.a. If the material appears grossly like plant material, the microscopic analysis isinconclusive, THC is present by GC/MS, and the Duquenois-Levine is positivefor marihuana, perform the microscopic analysis on another aliquot of material.If it is still inconclusive, review the case with a supervisor.

2. Tetrahydrocannabinol is identified if marihuana plant material is not present, theDuquenois-Levine is positive, and tetrahydrocannabinol is identified by GC/MS.

3. Exhibits consisting primarily of seeds – not plant material – should be reviewed with asupervisor prior to analysis.





Training Notes: Marihuana Analysis

1. Fresh marihuana plants that have been stored in non-permeable containers decompose. Apositive test for marihuana may not be possible under these conditions. Photograph casewhere possible.

2. Penalty for possession or delivery of marihuana in Texas is covered by marihuana-specific sections of the Texas Controlled Substances Act. Tetrahydrocannabinol isincluded in Penalty Group 2.

3. Dronabinol (trade name Marinol) is a commercial pharmaceutical containing THC insesame oil in a round, soft gelatin capsule. Refer to the steroid method for analysis.Review case with a supervisor. Dronabinol is included in Penalty Group 2.

4. Hashish, hash oil, and other non-marihuana materials containing THC are not specificallycovered by name in the Texas Controlled Substances Act. They are controlled by virtueof the fact that they contain THC.

5. Overgrowth of mold and presence of mold spores may occasionally be observed inmarihuana cases. If these cases must be analyzed, processing must be done in a hood.

Seek supervisory assistance as needed. Photograph case as applicable.6. Plant material is weighed in the condition it is received; it is typically not dried before

processing. If the material is fresh or likely to decompose further in the analyst’s judgment, it is recommended that a photo be taken and included in the case file.

7. When a case contains numerous exhibits, the analyst may choose to run more than oneGC/MS, for example one GC/MS for each 10 items.

8. In some cases (immature and old plant material), it may be necessary to extract the plantmaterial with petroleum ether, evaporate to dryness with heat, and color test the residue.




MISCELLANEOUS MATERIALS

Principle :

In general, positive identification of materials is done by gas chromatography/mass spectrometry

(GC/MS) or infrared spectroscopy (IR). This section concerns procedures identifying controlledsubstances in miscellaneous materials such as GHB, mushrooms, steroids, and volatiles.

Equipment :


IR Spectrophotometer with accessoriesScrew top culture tubes, 15 ml, 16 mm x 125 mm, screw cap with Teflon linerTest tubesVortex mixerSonicatorCentrifugePipettes, variousEvaporating dishes (watch glass)Spot test platespH paperHot plate

Reagents :

Methanol, reagent grade or betterHexane, reagent grade or betterAcetonitrile, reagent grade or better

Safety Precautions :

The most common chemical exposure in this type of laboratory is a chemical splash to the skinor eye. Skin, mucous membranes, or eyes which have been splashed with commonly used

chemicals or biologicals should be thoroughly washed for at least 15 minutes in cool tap water oreye wash station. Refer to MSDS’s for additional chemical information. Report the incidentimmediately to a supervisor. Seek medical attention as necessary.

Methanol and hexane are flammable solvents. Use in a hood or in a well ventilated area.

Acetonitrile is a suspected teratogen as well as a flammable solvent. Use in a hood or in a wellventilated area. Avoid contact with skin.

Dallas County Institute of Foresic Sciences Miscellaneous MaterialsControlled Substances Laboratory 1 Version 2.1




Color Testing :

See the section on Color Testing. Spot tests will usually be run on each item of non-pharmaceutical evidence within one case up to the applicable statutory weight limit and will be

performed on pharmaceutical evidence as applicable.

GHB Analytical Procedure:

1) Liquid Samples: a) Obtain the total weight and the total volume of the material in the exhibit to be analyzed

and record on the Drug Protocol Worksheet.b) Color test with ferric chloride.

i) An orange color is an indication that GHB is present.c) GC/MS Identification

i) Transfer approximately 10-20 drops of liquid to be analyzed to approximately 1.0 mL

methanol in a test tube.ii) Transfer an aliquot to an autosampler vial and inject on the GC/MS using BLANK.M

method.iii) GHB breaks down to GBL at high temperatures on the GC.

(1) The presence of GBL is consistent with the presence of GHB; however,confirmation by IR is required to conclusively determine whether GHB or GBL ispresent.

d) IR Identificationi) Obtain and record tare weight of a watch glass on Drug Protocol Worksheet.ii) Add several drops of sample to a watch glass so that the spot is approximately the

diameter of a quarter, obtain weight of watch glass plus sample and record on the

Drug Protocol Worksheet.iii) Place watch glass on hot plate using low heat. Evaporate sample to dryness.iv) Allow watch glass to cool for several minutes.v) Obtain weight of watch glass plus dry sample and record on the Drug Protocol

Worksheet.vi) Analyze dry sample by IR; refer to IR procedure.vii) Calculate the total weight of GHB.

2) Liquid Samples Containing Sugars:a) Obtain the total weight and the total volume of the material in the exhibit to be analyzed

and record on the Drug Protocol Worksheet.b) Color test with ferric chloride.

i) An orange color is an indication that GHB is present.c) GC/MS Identification

i) Transfer approximately 10-20 drops of liquid to be analyzed to 1.0 mL methanol in atest tube.

ii) Transfer an aliquot to an autosampler vial and inject on the GC/MS using BLANK.Mmethod.





(1) The presence of GBL is consistent with the presence of GHB; however,confirmation by IR is required to conclusively determine whether GHB or GBL ispresent.

d) IR Identificationi) Obtain and record tare weight of a watch glass on Drug Protocol Worksheet.

ii) Add several drops of sample to a watch glass so that the spot is approximately thediameter of a quarter, obtain weight of watch glass plus sample and record on theDrug Protocol Worksheet.

iii) Place watch glass on hot plate using low heat. Evaporate sample to dryness.iv) If the sample does not evaporate, resample.

(1) Place 3-5 mL of sample in a test tube.(2) Evaporate to approximately 1 mL in a hot water bath with air stream.(3) Dissolve in methanol; add methanol until all material dissolves.(4) Filter to remove any insoluble components.(5) Place sample in a test tube and evaporate methanol to approximately 1 mL.(6) Add 5 to 10 mL acetone to precipitate the GHB and decant the solvent.

(7) Wash the precipitate with 1 mL acetone.(8) Evaporate the acetone.(9) Proceed with IR.

e) Reportingi) GHB liquids containing sugar can not be quantitated. Report presence of GHB and

total weight of liquid in exhibit.

High and Low pH Liquids :

Clear aqueous liquids which are extremely acidic or basic to pH paper do not usually containcontrolled substances and typically are not analyzed.

Volatile Liquids :

Volatile liquids are commonly called inhalants; these materials are generally organic solventsand nitrites. They can be identified by gas chromatography/mass spectrometry (GC/MS) and/orinfrared spectroscopy (IR). Identification is made by comparison to standard materials.

Organic nitrites decompose on the injection block of the GC/MS to the corresponding alcohol.The GC/MS can be used to determine the alcohol part of unknown alkylnitrites. Specificidentification of the identity of organic nitrites is made by IR; however, identification may not bepossible for a mixture of organic nitrites.

Since volatile compounds evaporate rapidly, a smear test can be used as a presumptive test.Place a drop of liquid on a hard surface in a hood and smear with gloved finger. If materialevaporates quickly, a volatile may be present.

To identify the volatile content of spray paints and other aerosols, spray a small amount into ascrew cap vial containing 3 mL of methanol. Shake well and allow settling. Place an aliquot of the clear supernatant in an autosampler vial and inject on the GC/MS using VCHEM.M method.





Inhalant paraphernalia such as empty soda cans, empty bottles, rags, and plastic bags can oftenbe successfully analyzed by rinsing with methanol and injecting an aliquot on GC/MS usingVCHEM.M method.

Steroids Analytical Procedure :

Steroids are almost always encountered in dosage forms and in general can be classified astablets/capsules, aqueous injectable solutions, and vegetable oil injectable solutions.

1) Steroids in Oil:a) Obtain the total weight of the material in the exhibit to be analyzed and record on the

Drug Protocol Worksheet. b) Place approximately 6 drops of the oil into a 1:1 mixture of hexane:acetonitrile.c) Mix well by vortexing.d) Transfer the acetonitrile layer (bottom) to an autosampler vial and inject on the GC/MS

using STEROID.M method.2) Tablets, Capsules and Other Pharmaceutical Preparations:

a) Obtain the total weight of the material in the exhibit to be analyzed and record on theDrug Protocol Worksheet.

b) Select one tablet or capsule from a population as a representative sample for analysis.Grind to a powder if necessary.

c) GC/MS Identificationi) Transfer approximately 10 mg of the sample to 1.0 mL methanol in a test tube.ii) Vortex and centrifuge as necessary.iii) Transfer an aliquot to an autosampler vial and inject on the GC/MS using

STEROID.M method.

2) Liquids: a) Obtain the total weight of the liquid in the exhibit to be analyzed and record on the Drug

Protocol Worksheet.b) GC/MS Identification

i) Place approximately 1 part sample to 4 parts methanol in a 15 mL culture tube tube.Mix well before sampling.

ii) Transfer an aliquot to an autosampler vial. Analyze by GC/MS using STEROID.Mmethod.

Mushrooms/Cactus Bulbs Analytical Procedure :

Mushrooms and cactus buttons are the most common plant materials other than marihuanasubmitted for identification. These can be identified by gas chromatography/mass spectrometry(GC/MS) and are not quantitated.

1) Mushrooms:a) Obtain the total weight of the material in the exhibit to be analyzed and record on the

Drug Protocol Worksheet.





b) Locate the part of the mushroom that has a purple/blue tint (usually on the stem) andproceed with color testing using the Van Urk reagent. Record results on Drug ProtocolWorksheet.

c) Chop up approximately 500 mg of material (purple/blue portion).d) Place in a screw cap culture tube.

e) Add enough methanol to cover the material.f) Sonicate for 20 minutes.g) Centrifuge as necessary.h) Decant the methanol into another tube.i) Concentrate the methanol down to approximately 1 mL.

j) Transfer the methanol extract to an autosampler vial and inject on the GC/MS usingLSD.M method.

2) Cactus bulbs (buttons):a) Obtain the total weight of the material in the exhibit to be analyzed and record on the

Drug Protocol Worksheet.b) Chop or grind up approximately 500 mg of material.

c) Place in a screw cap culture tube.d) Add enough methanol to cover the material.e) Sonicate for 20 minutes.f) Centrifuge as necessary.g) Decant the methanol into another tube.h) Concentrate the methanol down to approximately 1 mL.i) Transfer the methanol extract to an autosampler vial and inject on the GC/MS using

LSD.M method.



Reporting Criteria:

1) Report the identity of the drug when an acceptable GC/MS and/or IR is obtained .2) Psilocin and psilocybin cannot be distinguished by GC/MS, therefore report presence of both,

i.e. psilocin/psilocybin.






Training Notes: Miscellaneous Materials

1. A sonicator may be used to bring materials into solution. Care should be usedregarding the length of time materials are left in the sonicator since heat maydecompose some drugs. Typically, a sonication time of 5 minutes or less is used.

2. Seek supervisory assistance and/or refer to the Microgram Bulletin (July-December2003) for mushroom/chocolate concoctions.3. Mushrooms should be analyzed immediately.4. For aqueous steroid injectables, take to residue with heat if necessary, and extract the

solid residue with methanol and analyze by GC/MS.5. The Van Urk produces subtle color changes and is often inconclusive.6. GHB converts to GBL on the injection block of GC/MS.




Dallas County Institute of Forensic Sciences Morphine Syrup AnalysisControlled Substances Laboratory 1 Version 2.1

MORPHINE SYRUP ANALYSIS

Principle of Assay:

This method describes the analysis of morphine in syrup formulations. This drug is amphoteric

and has both acidic and basic functional groups. Extraction of this substance from an aqueousmatrix into an organic phase requires that the pH must be above the pKa for the acidic –OHgroup and below the pKa for the amine function. The weakly basic drug is dissolved in waterand the pH of the solution is made weakly basic (approximately pH 8.5) using sodiumbicarbonate/sodium carbonate mix. In the weakly basic aqueous solution, the weakly basic drugis converted from its ionic salt form to its nonionic free base form. In this form, the drug isquantitatively extracted into ethyl acetate/isobutanol (9:1) containing an internal standard.Quantitative analysis is performed on the extracted drug using gas chromatography (GC).Morphine is identified using gas chromatography/mass spectrometry (GC/MS).


Liquids are suitable for analysis using this procedure.

Equipment:

Gas chromatograph-mass spectrometer containing a methylsiloxane capillary column such asHP-5MS, 30 m x 0.25 mm x 0.25 um film thickness and/or gas chromatograph-flame ionizationdetector with split/splitless injector containing a methylsiloxane capillary column such as HP-1,15 m x 0.32 mm x 1.0 um film thickness (see GC/MS and/or GC Methods Notebooks in DrugLaboratory).

Screw top culture tubes, 25 mL, 20 mm x 125 mm, screw cap with Teflon linerScrew top culture tubes, 15 mL, 16 mm x 125 mm, screw cap with Teflon linerVolumetric flasks, 10 mL, 25 mL, 100 mL, 2 literPipettes, variousGraduated cylinders, variousAutosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsVortex mixerRotatorCentrifugeAnalytical balancepH paper

Reagents:

Sodium bicarbonate, reagent grade or betterSodium carbonate, reagent grade or better





Ethyl acetate, reagent grade or betterIsobutanol, reagent grade or betterEthyl Alcohol, USP grade, 200 proof - AbsoluteAnalytical standardsCarbonate mix

Reagent Amount of ChemicalCarbonate Mix (8:3) 80 g sodium bicarbonate + 30 g sodium carbonate

Pulverize with a mortar and pestle. Store at room temperature.

Ethyl acetate/isobutanol (9:1)Reagent Volume of Solvent Total Volume

Ethyl acetate/ isobutanol (9:1) 90 mL ethyl acetate + 10 mL isobutanol 100 mL

Pour 90 mL of ethyl acetate and 10 mL isobutanol into a 100 mL flask. Mix by inverting theflask.

Safety Precautions:


Ethyl acetate and isobutanol are volatile solvents. Avoid contact with skin; do not breathevapors.


Internal Standard Amount of Drug (as base) Final Volume Solvent

0.5 mg/mL codeine 50 mg 100 mL (9:1) ethyl acetate:isobutanol

Transfer 50 mg codeine calculated as the free base to a 100 mL volumetric flask, and bring tovolume with solvent.


All solutions of stocks and standards are kept in the refrigerator. Allow the solutions to come to

room temperature before using them.

The concentration, amount, and volume of the calibration stock and calibration standards mayvary proportionally depending on the availability of drug and the expected concentration rangeof the drug. The following is provided as a guide:





Transfer 10.0 mg drug calculated as the free base to a 10 mL volumetric flask and bring tovolume with solvent. Mix by inverting the flask. Sonicate as needed. Transfer to a 15 mLculture tube for storage.


1. Place the appropriate amount of QC stock into a 15 mL labeled, screw cap culture tubeusing a volumetric pipette. Add deionized (DI) water to make a total volume of 5.0 mL.

Add approximately 200 mg carbonate mix and 5.0 mL I.S. solution.

QC Standard Amount of QC Stock Amount DI water Volume I.S. solution0.5 mg/mL morphine 2.5 mL 2.5 mL 5 mL

2. Cap the tubes and place on a rotator for 5 - 10 minutes.3. Centrifuge for 5 - 10 minutes on medium setting.4. Transfer an aliquot of the organic layer to an autosampler vial.

5. Inject the extracted QC standard into the GC using SYRMORPH.M method.

Evaluation Criteria :


2. If the QC sample is not within the set limits of +/- 5% of the target concentration,additional action must be taken to obtain an acceptable QC result such as re-running QC,re-extracting and re-running QC, making new stock solution and new QC with re-extraction and reanalysis, recalibrating (run curve), and/or consulting a supervisor.

Color Testing:

See the section on Color Testing. Spot tests will usually be run on each item of non-pharmaceutical evidence within one case up to the applicable statutory weight limit.


Liquid samples may be analyzed by weight or by volume. If the sample is to be analyzed byvolume, a known volume of the liquid must be weighed to determine density. This information isrecorded on the Drug Protocol Worksheet

1. Obtain the total volume and weight of liquid in the exhibit and record on the DrugProtocol Worksheet.

2. GC/MS Identificationa. Place approximately 1 part sample to 4 parts methanol, in a 15 mL screw cap

culture tube.





i. The analyst will vary the amount of material and methanol as needed toobtain an acceptable mass spectrum.

b. Transfer an aliquot to an autosampler vial.c. Analyze by GC/MS using BLANK.M method.

3. GC Quantitation

a. Transfer a known volume and weight of the sample to a 15 mL labeled screw topculture tube and record on the Drug Protocol Worksheet.b. Add deionized water to make a total volume of 5.0 mL.c. Add approximately 200 mg carbonate mix and 5.0 mL internal standard solution

to the culture tube.d. Cap the tube and place on rotator for 5 - 10 minutes.e. Centrifuge for 5 -10 minutes on medium setting.f. Transfer an aliquot of the organic layer to an autosampler vial.g. Inject the extracted sample into GC using SYRMORPH.M method and calculate

the results.


See GC and GC/MS Methods Notebooks in Drug Laboratory.

Reporting Criteria:

1. Report both the quantity and the identity of the drug when the concentration of the drugis within +/- 20% of the calibration curve on the GC and the GC/MS is complete. It maybe necessary to dilute extracted samples to bring them within curve range.

2. Report the amount of the drug as insufficient for quantitation when the drugconcentration is below 20% of the calibration curve on the GC and the GC/MS is

complete.3. Since penalty group is determined by the concentration of this drug, report the amount of

drug in mg/100 mL.

Calculations:



2. Materials Analyzed by Volume

a. concentration of drug (mg/mL) x volume of internal standard solution used forextraction (mL) x total exhibit volume (mL)/extracted sample volume (mL) = mgof drug in the exhibit as the free base

3. Materials Analyzed by weight:a. concentration of drug (mg/mL) x volume of internal standard solution used for





extraction (mL) x total exhibit weight (mg)/extracted sample weight (mg) = mg of drug in the exhibit as the free base

4. Amount drug (mg/100 mL):a. mg / 100 mL = mg (drug) X 100

Total Volume

of exhibit





Training Notes: Morphine Syrup Analysis


2. Results should be reported in mg/100 mL. Penalty group is based on number of mg/100mL.3. Refer to Direct Dilution method for residues and morphine in other matrices.4. The color tests may be inconclusive based on the concentration of the sample or the color

of the liquid.5. Calculation of drug as free base: Option 1

To calculate the amount of drug as a salt required to produce a target amount of free base,use the following equation:


Note: Occasionally two molecules of drug are included in the salt form, forexample morphine sulfate. Check the chemical formula prior to making thestandard. In the case of morphine sulfate, the molecular weight of the salt shouldbe divided by 2 prior to using the formula above.

Example : Morphine sulfate (C 17H19NO 3)2 H2SO 4 . 5H 2O MW = 758.8Morphine (base) MW = 285.3

758.8 / 2 X 10 mg morphine base = 13.3 mg morphine sulfate285.3

6. Calculation of drug as free base: Option 2Alternatively, to calculate the percentage of free base in the salt molecule to produce atarget amount, use the following equation:

Example : Morphine sulfate (C 17H19NO 3)2 H2SO 4 . 5H 2O MW = 758.8Morphine (base) MW = 285.3

285.3 X 2 = 0.752% base in salt = 758.8

Amount of salt needed = 10.0 mg = 13.3 mg morphine sulfate

0.752




OFF-SITE SAMPLING OF EVIDENCE

General Information:

This procedure outlines the process of off-site sampling of suspected controlled substance cases

which is usually performed at a submitting agency property room and submission of coresamples to the Controlled Substances Laboratory for examination. This process is employedwhen it is not feasible to submit evidence directly to the Laboratory for analysis. The mostcommon type of controlled substance sampled off-site is a large marihuana seizure; therefore,this procedure primarily focuses on marihuana cases, but it may be used for other suspectedcontrolled substance cases.

Notification:

To initiate a request for off-site sampling, a submitting agency submits a Notice of MarihuanaCore Sample sheet to the Drug Analysis Laboratory Evidence Registrar typically by fax or in

person.The Evidence Registrar notifies an IFS chemist of the request, issues a unique forensiclaboratory case number to the case, prints IFS evidence labels, and transfers the “Notice of Marihuana Core Sample” sheet to the assigned chemist.

The IFS Chemist contacts the submitting agency to make an appointment for off-site sampling.

Fresh plant material should be sampled as soon as possible, ideally on the next business day.

Transportation:

Employees of the Southwestern Institute of Forensic Sciences do not transport suspected drugevidence. Core samples are left at the property or with law enforcement officers for submissionat a later time.

Mileage reimbursement for business travel to and from the off-site location is handled perstandard County procedures.

Equipment and Supplies:

The chemist transports the following equipment and supplies to the off-site location in or withthe core sample carrying case:

1. Notice of Marihuana Core Sample sheet (obtained from Supervisor or EvidenceRegistrar)

2. IFS evidence labels containing a unique forensic laboratory number to be assigned to thecase (obtained from the Evidence Registrar)

3. Evidence Summary sheet for additional items4. Certified weights of appropriate mass, typically one 1 kg and one 5 lb weight5. Digital camera, charged with space on disc

Dallas County Institute of Forensic Sciences 1 Off-Site SamplingControlled Substances Laboratory Version 2.0




6. Ziplock bags for sampling7. Evidence bags8. Evidence container labels to identify evidence bags and document chain of custody9. Packaging tape10. Evidence tape

11. Duct tape12. Manila envelopes

13. Marihuana protocol sheets14. Box cutters or knives15. Pens and sharpies16. Calculator17. Various office supplies such as scissors18. Kimwipes19. Gloves20. Screwdriver21. Roll of shrink wrap

22. Goggles, plastic aprons, and plastic sleeves

Verification of Balance Operation:

The Chemist must first verify proper operation of the balance at the off-site location using an IFScertified weight and the Laboratory’s standard balance verification procedure. The Analystmakes note of the certified weight used, the actual weight measured by the balance, and thedifference found between actual and expected on the “Notice of Marihuana Core Sample” sheet.

If the difference between the actual and expected weight is outside the accepted range of +/- 3units, the Chemist will inform property room staff of the problem, cease sampling, and requestnotification when the balance has been properly calibrated.

Sampling:

IFS staff will follow Laboratory standard operating procedures when weighing and processingthe suspected controlled substance.

Sampling Procedure:

1. Establish Chain of Custody for primary containers with the submitting agency using theNotice of Marihuana Core Sample sheet.

2. Describe and count the number of primary containers and record them on the Notice of Marihuana Core Sample sheet.

3. Place the unique forensic laboratory number on each primary container.4. Verify that each container is in good condition and properly sealed.

a. If containers are not properly sealed or are in poor condition, report it to theproperty room staff and document this on the Notice of Marihuana Core Samplesheet.

i. Determine whether sampling can continue.

Dallas County Institute of Forensic Sciences 2 Off-Site SamplingControlled Substances Laboratory Version 2.0




Dallas County Institute of Forensic Sciences Pharmaceutical AnalysisControlled Substances Laboratory 1 Version 2.1

PHARMACEUTICAL ANALYSIS

General Information:

1. Pharmaceutical preparations such as tablets, capsules, patches, and lollipops typically are not

quantitated.2. Identification is performed by Logo Identification and/or GC/MS.

Logo Reference Sources:

Acceptable logo reference sources include a PDR, Ident-A-drug, Drug ID Bible, a manufacturer’swebsite, or other primary reference. Questions about the suitability of a logo reference sourceshould be directed to a supervisor.


Pharmaceutical identification falls into two categories: identification by GC/MS and/or visualidentification.

1. Visual Identificationa. Determine the total weight and number of items to be examined and record on the Drug

Protocol Worksheet.b. Assess whether the materials appear to be legitimate pharmaceuticals.

i. Materials suspected of being clandestine, tampered with, or with incomplete logoare not suitable for Visual Identification.

1. Analyze these items by another technique such as GC/MS; seek supervisory assistance as needed.

2. In cases containing only a single item or a single, partial item, photographthe item prior to analysis.

c. Capsules are not typically analyzed solely by Visual Identification.d. Determine the identity of the item(s) to be examined using an acceptable logo reference

source:i. Visually examine each item(s) for logo and appearance.

ii. Document visual appearance and markings on the Drug Protocol Worksheet.1. For cases consisting of a single item, photograph the item prior to

analysis.iii. Document the number of item(s) to be examined per logo on the Drug Protocol

Worksheet.iv. Obtain a printed copy of the logo identification from an acceptable reference and

include in the case file.v. In cases containing a mixture of tablets with complete logos and partial tablets

that are identical to the tablets with complete logos, it is acceptable to include theweight of the partial tablets in the exhibit weight.

e. Results Reportingi. When this procedure is solely used to identify a pharmaceutical, the report must

clearly state that the tablet or capsule was “visually identified as …”




Dallas County Institute of Forensic Sciences Pharmaceutical AnalysisControlled Substances Laboratory 2 Version 2.1

2. GC/MS a. Determine the total weight and number of items to be examined and record on the Drug

Protocol Worksheet.b. Visual Identification

i. Perform a Visual Identification as described above if possible.

c.

GC/MSi. For Visually Identified pharmaceuticals, transfer an amount of sample that isequivalent to approximately 1 mg of drug to a 15 mL screw cap culture tube.

1. For unknown materials, transfer approximately 100-200 mg of sample toa 15 mL screw cap culture tube.

ii. Add 1 mL of methanol.iii. Vortex and/or centrifuge as necessary.iv. Transfer an aliquot to an autosampler vial and inject on the GC/MS using

BLANK.M method.v. It may be necessary to concentrate and or run on a splitless method such as

LOWDOSE, LSD, etc.

d.

Results Reportingi. When this procedure is used it must be clearly stated on the report that thepharmaceutical was “used for analysis.”

ii. If a visual identification was performed, the report should also state that thepharmaceutical “is manufactured to contain …”

3. Quantitationa. If quantitation is required, refer to an appropriate method or seek supervisory assistance.





SCREENING UNKNOWN SAMPLES

Principle

In most cases, the analyst is able to select appropriate analytical procedures based upon color testresults, markings on pharmaceuticals, visual inspection, and/or professional judgment andexperience. When traditional methods fail to indicate a testing approach, the following methodis used to screen unknown samples and provide guidance for additional testing.


Powders, solids, liquids, tablets, capsules, residues, and other types of drug evidence are suitablefor analysis using this procedure.

Equipment:


Screw top culture tubes, 15 mL, 16 mm x 125 mm, screw cap with Teflon linerAutosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsVortex mixerTest tubesPipettes, various

Reagents:

Methanol, reagent grade or better

Safety Precautions:

The most common chemical exposure in this type of laboratory is a chemical splash to the skinor eye. Skin, mucous membranes, or eyes which have been splashed with commonly usedchemicals or biologicals should be thoroughly washed for at least 15 minutes in cool tap water oreye wash station. Refer to MSDS’s for additional chemical information. Report the incidentimmediately to a supervisor. Seek medical attention as necessary.

Methanol is a flammable solvent. Use in a hood or in a well ventilated area.

Color Testing:

Dallas County Institute of Forensic Sciences 1 Screening UnknownsControlled Substances Laboratory Version 2.0




See the section on Color Testing. Spot tests will usually be run on each item of non-pharmaceutical evidence within one case up to the applicable statutory weight limit. Colortesting may be performed on pharmaceutical evidence as applicable.

Analytical Approach

Determine net weight of sample

Perform color test(s)

Dissolve arbitrary amount of sample in methanol.

Run solution by GC/MS usingBLANK.M

If no controlled substance isdetected or a weak spectra is

found run sample onLOWDOSE.M, VIAGRA.M or

LSD.M.

Determine net weight andvolume of sample

Perform color test(s) and testpH and solubility as needed.

Dissolve 1 part sample to 4parts methanol.

Run solution by GC/MS usingBLANK.M



LSD.M.

Wash sample container withmethanol and reserve washing

in sample tube.

Run methanol blank by GC/MSusing BLANK.M. Run

methanol wash of evidence byGC/MS using BLANK.M.



LSD.M

Empty autosampler vial back into sample tube and rinse vial

with methanolic HCl.

Evaporate to dryness.

ResidueSolid Liquid

Once unknown is identified refer to appropriatemethod to complete analysis.







See GC Methods and GC/MS Methods Notebooks.

Reporting Criteria:

1. The identity of controlled substances determined by GC/MS is reported.a. Other procedures as applicable may be used to quantitate the controlled substance.

2. If no controlled substance is identified it will be so noted on the report.3. Other types of testing such as IR may also be used in an attempt to identify an unknown

substance.4. Seek supervisory assistance as needed.




Dallas County Institute of Forensic Sciences Weak Alkaline Drug AnalysisControlled Substances Laboratory 1 Version 2.1

WEAK ALKALINE DRUG ANALYSIS

Principle of Assay:

This method describes the analysis of drugs which are weakly alkaline (weak bases) and/or

which are not stable in the presence of strong base. Examples of drugs identified and quantitatedby this method are cocaine including cocaine in oil, injectable forms of morphine andhydromorphone, phencyclidine, and chlordiazepoxide. Powders and solids suspected of containing cocaine are typically analyzed using the Cocaine Direct Dilution procedure.

Drugs are identified using analytical techniques which provide conclusive identification of thedrug. These techniques include gas chromatography/mass spectrometry (GC/MS) and infraredspectroscopy (IR).

The weakly basic drug is dissolved in water and the pH of the solution is made weakly basic(approximately pH 8.5) using sodium bicarbonate. In the weakly basic aqueous solution, the

weakly basic drug is converted from its ionic salt form to its nonionic free base form. In thisform, the drug is quantitatively extracted into n-butyl chloride or chloroform containingphenanthrene as the internal standard. Quantitative analysis is performed on the extracted drugusing gas chromatography (GC).

Marked pharmaceuticals will usually be identified by logo match and GC/MS withoutquantitation. However when the penalty group or schedule of a marked pharmaceuticalpreparation is determined by dosage or preparation, sufficient testing should be performed forplacement of the substance in a proper penalty group or schedule.


Powders, solids, liquids, tablets, capsules, residues, and other types of drug evidence are suitablefor analysis using this procedure.

Equipment:

Gas chromatograph-mass spectrometer containing a methylsiloxane capillary column such asHP-5MS, 30 m x 0.25 mm x 0.25 um film thickness and/or gas chromatograph-flame ionizationdetector with split/splitless injector containing a methylsiloxane capillary column such as HP-1,15 m x 0.32 mm x 1.0 um film thickness (see GC/MS and/or GC Methods Notebooks in DrugLaboratory).

Screw top culture tubes, 25 mL, 20 mm x 125 mm, screw cap with Teflon linerScrew top culture tubes, 15 mL, 16 mm x 125 mm, screw cap with Teflon linerVolumetric flasks, 10 mL, 25 mL, 2 literAutosampler vials, 32 mm x 11 mm, Teflon lined seals and glass insertsVortex mixerRotator





CentrifugeTest tubespH paperPipettes, variousHamilton syringes, various

Analytical balanceAdjustable 10 mL Dispensette Reagent BottleMortar and PestleErlenmeyer flask, 50 mLGraduated cylinders, various

Reagents:

n-Butyl chloride, reagent grade or betterChloroform, reagent grade or betterPhenanthrene, reagent grade or better

HCl, reagent grade or betterSodium bicarbonate, reagent grade or betterMethanol, reagent grade or betterAnalytical standardsMethanolic HCl (5%)

Transfer 95 mL of methanol to a 100 mL Erlenmeyer flask then add 5 mL concentrated HCl.Acetonitrile, reagent grade or betterHexane, reagent grade or better

Reagent Volume of DI water Volume of HCl

25% HCl 30 mL 10 mL

In the hood, place 30 mL deionized water into a 50 mL graduated cylinder and carefully add 10mL of concentrated HCl using a graduated cylinder. Transfer to a 50 mL Erlenmeyer flask forstorage.

Safety Precautions:

The most common chemical exposure in this type of laboratory is a chemical splash to the skinor eye. Skin, mucous membranes, or eyes which have been splashed with commonly usedchemicals or biologicals should be thoroughly washed for at least 15 minutes in cool tap water oreye wash station. Refer to MSDS’s for additional chemical information. Report the incident

immediately to a supervisor. Seek medical attention as necessary.n-Butyl chloride is flammable. Use in a hood or in a well ventilated area. Do not make contactwith skin.

Hydrochloric acid is corrosive. Avoid contact with skin, eyes, and mucous membranes.

Hexane and methanol are flammable solvents. Use in a hood or in a well ventilated area.





Chloroform is a chlorinated solvent and is considered a human carcinogen. Use in a hood or in awell ventilated area. Avoid contact with skin.

Acetonitrile is a suspected teratogen. Use in a hood or in a well ventilated area. Avoid contact

with skin.



0.5 mg/mL phenanthrene 1.00 grams 2.0 L n-butyl chloride

Transfer 1.00 grams phenanthrene to a 2.0 L volumetric flask and bring to volume with solvent.Mix by inverting the flask.


All solutions of stocks and standards are kept in the refrigerator. Allow the solutions to come toroom temperature before using them.

The concentration, amount, and volume of the calibration stock and calibration standards mayvary proportionally depending on the availability of drug, and the expected concentration rangeof the drug. The following is provided as a guide:

Calibration Stock Amount of Drug (as base) Final Volume Solvent

5.0 mg/mL Drug 50.0 mg 10 mL deionized (DI) water

Transfer 50.0 mg drug calculated as the free base to a 10 mL volumetric flask and bring tovolume with DI water. Mix by inverting the flask. Sonicate as needed. Transfer solution to a 15mL culture tube for storage.



2. Using a Hamilton syringe or volumetric pipette, place the appropriate amount of calibration stock into a 15 mL labeled, screw cap culture tube. Add deionized (DI) waterto make a total volume of 5.0 mL. Add approximately 200 mg sodium bicarbonate and5.0 mL internal standard solution.

Calibration Standards Amount of Calibration Stock Amount of DI H 2O Volume I.S. solution0.10 mg/mL 0.1 mL 4.90 mL 5 mL1.00 mg/mL 1.0 mL 4.00 mL 5 mL5.00 mg/mL 5.0 mL 0 mL 5 mL

3. Cap the tubes and place on a rotator for 5 - 10 minutes.





4. Centrifuge for 5 - 10 minutes on medium setting.5. Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top; chloroform on the bottom.6. Inject the extracted calibration standards into the GC using the appropriate instrument

method.

7. Determine if the data are acceptable using the instructions found in the CalibrationCurve/Response Factor Log. An acceptable calibration curve has a correlationcoefficient, r 2 > 0.995. If the curve is acceptable, file it in the CalibrationCurve/Response Factor Log located in the Drug Laboratory. If not, seek supervisoryassistance as needed.


Ideally the quality control standard will be made from a different lot number or manufacturerthan the calibration stock. At a minimum, it should be made from a different stock solution.



QC Stock Amount of Drug (as base) Final Volume Solvent

2.0 mg/mL Drug 50.0 mg 25 mL deionized (DI) water

Transfer 50.0 mg drug calculated as the free base to a 25 mL volumetric flask and bring tovolume with deionized water. Mix by inverting the flask. Sonicate as needed. Transfersolution to 25 mL culture tube for storage.


1. Using a volumetric pipette, place 2.5 mL of quality control stock and 2.5 mL deionizedwater into a 15 mL labeled, screw cap culture tube. Add approximately 200 mg sodiumbicarbonate and 5.0 mL internal standard solution.

QC Standard Amount of QC Stock Amount of DI water Volume of I.S. solution

1.0 mg/mL Drug 2.5 mL 2.5 mL 5.0 mL

2. Cap the tube and place on rotator for 5 - 10 minutes.3. Centrifuge for 5 - 10 minutes on medium setting.4. Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top and chloroform on the bottom of the respective water layers.5. Inject the extracted quality control sample into the GC using the appropriate instrument

method.

Evaluation Criteria :





Worksheet.b) Create a representative sample for analysis; grind to a powder if necessary.

i) Capsules – typically a composite sample is used for analysis.ii) Tablets – typically one tablet is selected for analysis.

c) Logo Identification

i) Refer to Pharmaceutical Analysis Procedure.d) GC/MS Identificationi) Transfer an amount of sample that is equivalent to approximately 1 mg of drug to

approximately 1 mL methanol in a test tube.(1) The analyst will vary the amount of material and methanol as needed to obtain an


method.e) GC Quantitation

i) Weigh approximately 10 – 50 mg of the material to be analyzed and record the

weight on the Drug Protocol Worksheet.ii) Transfer sample to a 15 mL labeled screw cap culture tube.iii) Add 1.0 - 5.0 mL of deionized water, approximately 200 mg sodium bicarbonate, and

1.0-5.0 mL of internal standard solution.iv) Cap the tube and place on rotator for 5 - 10 minutes.v) Centrifuge for 5 - 10 minutes on medium setting.vi) Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top and chloroform on the bottom.vii) Inject the extracted sample into the GC using the appropriate instrument method and


3) Liquid Samples: a) Liquid samples may be analyzed by weight or by volume. If the sample is to be analyzed

by volume, a known volume of the liquid must be weighed to determine density.b) If the volume of liquid is small, it should be treated as a residue; see below.c) Obtain the total weight of liquid in the exhibit and record on the Drug Protocol

Worksheet. If the liquid is to be analyzed by volume, record the total volume on DrugProtocol Worksheet.

d) GC/MS Identificationi) Place approximately 1 part sample to 4 parts methanol in a 15 mL screw cap culture

tube. Mix well before sampling.(1) The analyst will vary the amount of material and methanol as needed to obtain an

acceptable mass spectrum.ii) Transfer an aliquot to an autosampler vial. Analyze by GC/MS using BLANK.M

method.e) GC Quantitation

i) Transfer a known volume or weight of the sample to a 15 mL labeled screw capculture tube.

ii) If the liquid is aqueous, proceed to step iii. If the composition of the liquid is





unknown or organic, add three drops of methanolic HCl and evaporate the sample todryness or to constant volume.

iii) Based on the estimated drug concentration of the material, determine the extractionvolume. The volumes of water and extraction solvent should be equal: add 1.0 – 5.0mL of deionized water, add approximately 200 mg sodium bicarbonate, and 1.0 - 5.0

mL internal standard solution.iv) Cap the tube and place on rotator for 5 - 10 minutes.v) Centrifuge for 5 -10 minutes on medium setting.vi) Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top and chloroform on the bottom.vii) Inject the extracted sample into GC using appropriate instrument method and


4) Residue Samples: a) Carefully rinse the residue into a container using methanol.b) GC/MS Identification

i) Run a methanol blank before each residue sample using DRUGANA.M orBLANK.M methods; place in case file.ii) Place an aliquot of the methanol washing into an autosampler vial. Analyze by

GC/MS using BLANK.M method.c) GC Quantitation

i) Place the sample/methanol mixture in a 15 mL screw cap culture tube, add 1-3 dropsof methanolic HCl, and evaporate to dryness.

ii) Based on the estimated drug concentration of the material, determine the extractionvolume. Add the same amount of water and extraction solvent: add 1.0 – 5.0 mL of deionized water to residue, approximately 200 mg sodium bicarbonate, and 1.0 - 5.0mL internal standard solution.

iii) Cap the tube and place on a rotator for 5 - 10 minutes.iv) Centrifuge for 5 - 10 minutes on medium setting.v) Run a methanol blank before each residue sample using the same instrument method

used for the sample; place in case file.vi) Transfer an aliquot of the organic layer to an autosampler vial. Note: n-butyl chloride

will be on the top and chloroform on the bottom.vii) Inject the extracted sample into GC using appropriate instrument method and

calculate the results. If it is necessary to dilute the residue, return to the originalwashing for dilution.

d) When analysis is complete return any extracted sample remaining in the autosampler vialto the original culture tube used for the extraction.

i) Remove and discard the aqueous layer from the culture tube. Add 1-3 drops of methanolic HCl to the extracted sample to convert the drug to its more stablehydrochloride salt form.

ii) Take the extracted sample to residue in a laboratory fume hood. Close with a screwcap.

iii) Label the tube “added by laboratory”, include FL#, initials, and place this tube in theevidence bag along with the evidence.





5) Phencyclidine (PCP) Analysis a) Cigarette Samples

i) Obtain the total weight of the cigarette(s) in the exhibit and record on the DrugProtocol Worksheet.

ii) GC Quantitation(1) Soak the cigarette in methanol.(2) Analyze the methanol using the “Residue Samples” method.(3) Inject extracted sample into GC using PCP.M method and calculate the results.

iii) GC/MS Identification(1) Analyze by GC/MS using BLANK.M method using the “Residue Samples”

method.b) PCP in Solvent

i) Obtain the total weight of liquid in the exhibit to be analyzed and record on the DrugProtocol Worksheet.

ii) GC Quantitation

(1) Pipet approximately 50 - 200 uL of sample into a 15 mL labeled screw cap culturetube.(2) Determine weight of the material to be analyzed and record on Drug Protocol

Worksheet.(3) Add a 1.0 – 5.0 mL of water and approximately 200 mg sodium bicarbonate to the

culture tube.(4) Add 1.0 - 5.0 mL of internal standard.(5) Cap the tube and place on rotator for 5 - 10 minutes.(6) Centrifuge for 5 - 10 minutes on medium setting.(7) Transfer an aliquot of the organic layer to an autosampler vial.(8) Inject extracted sample into GC using PCP.M method and calculate the results.

iii) GC/MS Identification(1) Analyze a separate sample by GC/MS using a second sample aliquot.

6) Analysis of Cocaine In Oila) Obtain the total volume and weight of liquid in the exhibit and record on the Drug

Protocol Worksheet.b) GC/MS Identification

i) Place approximately 1 mL of material to be analyzed in a 15 mL screw cap culturetube, add approximately 1 mL of hexane, mix well by vortexing.(1) The analyst will vary the amount of material and hexane/acetonitrile as needed to

obtain an acceptable mass spectrum.

ii) Add approximately 2 mL acetonitrile.iii) Cap the tube and place on rotator for 5 – 10 minutes.iv) Centrifuge 5 – 10 minutes.v) Transfer an aliquot of the acetonitrile layer (bottom) to an autosampler vial. Analyze

by GC/MS using BLANK.M method.c) GC Quantitation

i) Place approximately 1 - 2 mL of material to be analyzed into a 15 mL labeled screw





cap culture tube.ii) Determine weight of material to be analyzed and record on Drug Protocol Worksheet.iii) Add an equal volume of water followed by 1-3 drops of 25% HCl.iv) Rotate 5 – 10 minutes.v) Centrifuge for 5 - 10 minutes on medium setting.

vi) Transfer aqueous layer to a clean 15 mL culture tube.vii) Add approximately 200 mg sodium bicarbonate. Test with pH paper to make suresolution is neutral before proceeding.

viii) Add an equal volume of n-butyl chloride with internal standard and record on DrugProtocol Worksheet.

ix) Rotate 5 – 10 minutes. Centrifuge for 5 - 10 minutes on medium setting.x) Transfer an aliquot of the organic layer to an autosampler vial.xi) Inject extracted sample into GC using COC.M method and calculate the results.



Reporting Criteria:

1. Report both the quantity and the identity of the drug when the concentration of the drugis within +/- 20% of the calibration curve on the GC and the GC/MS is complete. It maybe necessary to dilute extracted samples to bring them within the curve range.

2. Report the amount of the drug as insufficient for quantitation when the drugconcentration is below 20% of the calibration curve on the GC and the GC/MS iscomplete.

3. For PCP cigarette exhibits, report the amount of PCP in the item analyzed, and the total

weight of the item analyzed.

Calculations:



2. Materials Analyzed by Volume:a. concentration of drug (mg/mL) x volume of internal standard solution used for

extraction (mL) x total exhibit volume/extracted sample volume = mg of drug in

the exhibit as the free base3. Materials Analyzed by Weight:

a. concentration of drug (mg/mL) x volume of internal standard solution used forextraction (mL) x total exhibit weight (mg)/extracted sample weight (mg) = mg of drug in the exhibit as the free base

4. Percent drug in the exhibit:a. mg of drug in the exhibit/total weight of the exhibit x 100 = % of drug in the





exhibit 5. Amount drug in mg/100 mL:

a. mg / 100 mL = mg (drug) X 100Total Volume

of exhibit




Training Notes: Weak Alkaline Procedure


2. A sonicator may be used to bring materials into solution. Care should be used regardingthe length of time materials are left in the sonicator since heat may decompose somedrugs. Typically, a sonication time of 5 minutes or less is used.

3. The toxicity of n-butyl chloride is less than that of chloroform; therefore, where possible,n-butyl chloride is the extraction solvent of choice. However, extraction efficiency of some drugs is low or variable in this solvent, and in this case, chloroform is used.

4. To determine whether cocaine is present in the free base or hydrochloride form, refer tothe Color Testing procedure for presumptive salt/base determination and to the InfraredSpectroscopy procedure for conclusive identification of salt/base form.

5. Diphenhydramine and ketamine co-elute when run by GCMS using BLANK.M. UseSLOWRAMP.M method if there is evidence of the mixture.

6. Calculation of drug as free base: Option 1To calculate the amount of drug as a salt required to produce a target amount of free base,use the following equation:


Note: Occasionally two molecules of drug are included in the salt form, forexample morphine sulfate. Check the chemical formula prior to making the


swifs controlled substances procedures manual v2.3 (02.26.2009) 157 pages.pdf

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