1、Designation: E2125 11Standard Guide forMicrocrystal Testing in Forensic Analysis of Phencyclidineand Its Analogues1This standard is issued under the fixed designation E2125; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONMicrocrystal tests are primarily chemical-precipitation tests in which a light microscope is used toobserve and dis
3、tinguish the different types of crystals formed. These tests require skill and expertiseon the part of the analyst that can be adequately gained only through appropriate training andexperience in their use. These tests should not be attempted by those who are unfamiliar with themfor use in the analy
4、sis of phencyclidine and its analogues.1. Scope1.1 This guide describes some standard procedures appli-cable to the analysis of phencyclidine and its analogues usingmicrocrystal tests (1-8).21.2 These procedures are applicable to phencyclidme and itsanalogues which are present in solid dosage form o
5、r in a liquidform. They are not typically applicable to the analysis ofphencyclidine and its analogues in biological samples.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard cannot replace knowledge, skill,
6、or abilityacquired through appropriate education, training, and experi-ence and should be used in conjunction with sound profes-sional judgment.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standa
7、rd to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3E1459 Guide for Physical Evidence Labeling and RelatedDocumentationE1492 Practice for Receiving, Documenting, Storing, andRetrie
8、ving Evidence in a Forensic Science LaboratoryE1732 Terminology Relating to Forensic ScienceE2329 Practice for Identification of Seized DrugsE2548 Guide for Sampling Seized Drugs for Qualitativeand Quantitative Analysis3. Terminology3.1 For definitions of terms used in this standard, refer toTermino
9、logy E1732.3.2 Definitions:3.2.1 aggregationthe collecting of units or parts into amass or whole.3.2.2 birefringenceproperty of some crystals having morethan one refractive index; this will result in interference colorswhich are viewed through a polarized light microscope.3.2.3 grainsthick tablets h
10、aving nearly equal width,breadth, and thickness.3.2.4 habitthe external morphology of the crystal.3.2.5 microdropa small drop of liquid that would fit onthe end of a standard size, flattened toothpick; the approximatevolume of this drop would be 10 to 25 L.3.2.6 nailsa skeleton of some kinds of tria
11、ngles, elon-gated, usually pointed with a short head usually thicker orbroader.3.2.7 needles (acicular)long, thin crystals with pointedends.3.2.8 nuggetsirregularly formed grains without sharpfaces or edges.3.2.9 plierscrystals resembling pliers, generallyX-shaped.3.2.10 razor bladesthin oblong crys
12、tals with length abouttwice the width, resembling a safety razor blade.3.2.11 sheaveselongated crystals form two opposite fansfrom the same joining point.1This guide is under the jurisdiction of ASTM Committee E30 on ForensicSciences and is the direct responsibility of Subcommittee E30.01 on Crimina
13、listics.Current edition approved March 1, 2011. Published April 2011. Originallyapproved in 2001. Last previous edition approved in 2007 as E2125 07. DOI:10.1520/E2125-11.2The boldface numbers in parentheses refer to a list of references at the end ofthis standard.3For referenced ASTM standards, vis
14、it the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2
15、959, United States.3.2.12 skeletal crystala crystal in which all of the spacesin the crystal lattice are not occupied.3.2.13 spindlesshorter than course needles, but moresubstantial cross-section.4. Summary of the Technique4.1 A small sample of the material containing the suspectedphencyclidine or i
16、ts analogues is dissolved in a dilute acid andthe appropriate precipitating reagent is added. The crystals thatare formed are observed and distinguished utilizing a lightmicroscope.5. Significance and Use5.1 The technique produces a chemical-precipitation reac-tion between the phencyclidine or its a
17、nalogues and theprecipitating reagent. The habit and the aggregation of thecrystals formed may be used to distinguish phencyclidine or itsanalogues from other drugs.5.2 The technique can be utilized on phencyclidine or itsanalogues present in either the salt or free base form.5.3 The technique does
18、not distinguish between salt and freebase forms.6. Interferences6.1 Diluents/adulterants present in combination with phen-cyclidine or its analogues in the sample to be tested may resultin crystals that are distorted or otherwise rendered unidentifi-able. In these instances, it will be necessary to
19、separate thephencyclidine or its analogues from the diluents/adulterants orto use other testing methods to analyze for phencyclidine or itsanalogues.7. Apparatus7.1 Standard light microscope capable of varying magnifi-cations including 1003 is needed for viewing the crystals.Polarized light attachme
20、nt is not essential, but is desirablebecause crystals resulting from the precipitation reaction arebirefringent.8. Reagents and Materials8.1 10 % v:v acetic acid.8.2 10 % v:v hydrochloric acid.8.3 2 % w:v potassium permanganate in 0.5 % v:v phos-phoric acid.8.4 Gold bromide (HAuBr4) in diluted perch
21、loric and aceticacids 0.55 g HAuBr4, 42 mL water, 37 mL concentrated per-chloric acid, 21 mL glacial acetic acid.8.5 Gold chloride (HAuCl4) in acetic and sulfuric acidsHAuCl4in HOAc-4(1+1)H2SO4; 2 g HAuCl4, 20 mL glacialacetic acid, 40 mL concentrated sulfuric acid, 40 mL water.8.6 Phencyclidine PCP
22、; 1-(1-phenylcyclohexyl)piperidinestandard.8.7 Pyrrolidine analogue of phencyclidine PCPy, PHP,1-(1-phenylcyclohexyl)pyrrolidine standard.8.8 Morpholine analogue of phencyclidine PCM, 1-(1-phenylcyclohexyl)morpholine standard.8.9 Thiophene analogue of phencyclidine TCP; 1-l-(2thienyl)cyclohexylpiper
23、idine standard.9. Sampling, Test Specimens, and Text Units9.1 The general handling and tracking of samples shouldmeet or exceed the requirements of Practice E1492 and GuidesE1459 and E2548.10. Calibration and Standardization10.1 The reagents utilized for these microcrystal tests are tobe tested for
24、reliability using phencyclidine or its analoguesand negative controls following the prescribed procedure. Onlywhen it is determined that the reagents are producing theexpected response may the reagents be used in the testingprocedure.11. Procedure11.1 Potassium Permanganate:11.1.1 Place a small samp
25、le (a few particles of powder, lessthan one (1) milligram (mg) or a small drop of liquid, allowedto dry) of the suspected phencyclidine or its analogue on amicroscope slide.11.1.2 Dissolve the sample in a few microdrops of 10 %acetic acid or 10 % hydrochloric acid.11.1.3 Add a few microdrops of 2 %
26、acidified potassiumpermanganate to the edge of the acid solution on the micro-scope slide. Add a coverslip.11.1.4 Observe the formation of crystals using a properlyaligned and adjusted light microscope. The observation can bedone between crossed polars, if desired. If crossed polars areused, care sh
27、ould be used to orient the polarizer in theeast-west direction and the analyzer in the north-south direc-tion, verified by a black background.11.1.5 The crystal formed will depend on the drug present,if any. The formation that can be expected for phencyclidineand its analogues are as follows:11.1.5.
28、1 PCP (phencyclidine) produces purple razor bladecrystals. In high concentrations, the crystals resemble needlesimpaling small spheres.11.1.5.2 PCPy produces purple plier-shaped crystals withembedded nuggets and irregular forms.11.1.5.3 PCM produces unremarkable crystals.11.1.5.4 TCP produces unrema
29、rkable crystals.11.1.6 If a dense cloud of precipitate is formed uponaddition of the precipitating agent, the crystals may not bereadily visible. It may be necessary to repeat the test reducingthe concentration of suspected phencyclidine or its analogue.This is done by either decreasing the sample s
30、ize or increasingthe volume of solvent.11.2 Gold Bromide in Diluted Perchloric and Acetic Acids:11.2.1 Place a small sample (a few particles of powder, lessthan one (1) milligram (mg) or a small drop of liquid, allowedto dry) of the suspected phencyclidine on a microscope slide.11.2.2 Dissolve the s
31、ample in a few microdrops of 10 %acetic acid or 10 % hydrochloric acid.11.2.3 Add a few microdrops of gold bromide in dilutedperchloric and acetic acids reagent to the edge of the acidsolution on the microscope slide. Cover with a coverslip.11.2.4 Observe the formation of crystal using a properlyali
32、gned and adjusted light microscope. The observation can bedone between crossed polars, if desired. If crossed polars areE2125 112used, care should be used to orient the polarizer in theeast-west direction and the analyzer in the north-south direc-tion, verified by a black background.11.2.5 The cryst
33、al formation will depend on the drugpresent, if any. The formation that can be expected forphencyclidine and its analogues are as follows:11.2.5.1 PCP (phencyclidine) produces red-gold coloredsquares with diagonal markings, often elongated along oneaxis; birefringent; in high concentrations, colorle
34、ss nails.11.2.5.2 PCPy produces aggregates of tiny rods andX-shaped crystals; birefringent.11.2.5.3 PCM produces amorphous oily drops which slowlyaggregate into plates.11.2.5.4 TCP produces thin X-shaped crystals, often withgrossly elongated arms; birefringent.11.2.6 If a dense cloud is formed upon
35、addition of theprecipitating agent, the crystals may not be readily visible. Itmay be necessary to repeat the test reducing the concentrationof suspected phencyclidine or its analogue. This is done byeither decreasing the sample size or increasing the volume ofsolvent.11.3 Gold Chloride in Acetic an
36、d Sulfuric Acids:11.3.1 Place a small sample (a few particles of powder, lessthan one (1) milligram (mg) or a small drop of liquid, allowedto dry) of the suspected phencyclidine on a microscope slide.11.3.2 Dissolve the sample in a few microdrops of 10 %acetic acid or 10 % hydrochloric acid.11.3.3 A
37、dd a few microdrops of gold chloride in acetic acidand sulfuric acid reagent to the edge of the acid solution on themicroscope slide. Add a coverslip.11.3.4 Observe the formation of crystal using a properlyaligned and adjusted light microscope. The observation can bedone between crossed polars, if d
38、esired. If crossed polar areused, care should be used to orient the polarizer in theeast-west direction and the analyzer in the north-south direc-tion, verified by a black background.11.3.5 The crystal formation will depend on the drugpresent, if any. The formation that can be expected forphencyclid
39、ine and its analogues are as follows:11.3.5.1 PCP produces unremarkable crystals.11.3.5.2 PCPy produces yellow X-shaped crystals.11.3.5.3 PCM produces H-shaped plates with widened ends.11.3.5.4 TCP produces yellow thick needles, some withshort, perpendicular central arms.11.3.6 If a dense cloud is f
40、ormed upon addition of theprecipitating agent, the crystals may not be readily visible. Itmay be necessary to repeat the test reducing the concentrationof suspected phencyclidine or its analogue. This is done byeither decreasing the sample size or increasing the volume ofsolvent.12. Interpretation o
41、f Results (9)12.1 The three precipitating reagents utilized in this tech-nique, that is, potassium permanganate, gold bromide indiluted perchloric and acetic acids, and gold chloride in aceticand sulfuric acids, are capable of distinguishing PCP (phency-clidine), PCPy, PCM, and TCP from each other.1
42、2.2 If crystals structurally similar to those formed byphencyclidine and phencyclidine analogue standards areformed by at least two of the precipitating agents, the samplemay be considered positive by this technique for the presenceof either PCP, PCPy, PCM, or TCP.12.3 All observed crystalline preci
43、pitates must be docu-mented and included in the analysts notes for each itemanalyzed.12.4 The forensic identification of phencyclidine or itsanalogues requires the use of multiple uncorrelated techniques,see Practice E2329.13. Precision and Bias13.1 No information is presented about either the preci
44、sionor bias of this technique.14. Keywords14.1 microcrystalline testing; morpholine analogue of phen-cyclidine, PCM; phencyclidine, PCP; pyrrolidine analogue ofphencyclidine, PCPy; thiophene analogue of phencyclidine,TCPREFERENCES(1) Fulton, Charles C., Modern Microcrystal Tests for Drugs, Wiley-Int
45、erscience, New York, 1969.(2) Clarke, E. G. C., Isolation and Identification of Drugs, Pharmaceu-tical Press, London, 1971, pp. 139141.(3) Chamot, E. and Mason, C., Handbook of Chemical Microscopy,Volume 1. John Wiley, New York, 1930.(4) Evans, Hiram K., “Microcrystal Tests for the Characterization
46、of Some1-Arylcyclohexylamines,” American Academy of Forensic Sciences,Cincinnati, Ohio, 19 Feb. 1983.(5) Harris, H. et al., “Vegetable Matter Coated with a Barbiturate and aVeterinary Anesthetic,” Microgram, Vol. 10, No. 1, Jan. 1977, pp.910.(6) Epstein, R. L. and Lorimer, P., and Sloma, E. J., “Ide
47、ntification ofPhencyclidine-Related Drugs,” Microgram, Vol. 22, No. 1, Jan. 1977,pp. 6169.(7) Koles, J. E., “Some Microcrystal Tests for Drags” in Progress inChemical Toxicology, Vol. 5, ed. A. Stolman, Academic Press. SanFrancisco, CA, 1974.(8) “Miscellaneous Tests and Procedures,” Microgram, Vol.
48、7, No. 2,Feb. 1974, p. 20.(9) Nichols, Ronald “Drug Proficiency Test False Positives: A Lack ofCritical Thought,” Science and Justice, Vol. 37, No. 3, pp. 191196,1997.E2125 113ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item menti
49、onedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments wi
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