1、Designation: E 2125 07Standard Guide forMicrocrystal Testing in the Forensic Analysis ofPhencyclidine and Its Analogues1This standard is issued under the fixed designation E 2125; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、and distinguish 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 th
4、e analysis 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.1.2 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 This guide offers an organized collection of informationor a series of options and does not recommend a specificcourse of action. This document cannot replace education or
6、experience and should be used in conjunction with professionaljudgment. Not all aspects of this guide may be applicable in allcircumstances. This ASTM standard is not intended to repre-sent or replace the standard of care by which the adequacy ofa given professional service must be judged, nor shoul
7、d thisdocument be applied without consideration of a projects manyunique aspects. The word “Standard” in the title of thisdocument means only that the document has been approvedthrough the ASTM consensus process.1.4 This standard does not purport to address all of thesafety concerns, if any, associa
8、ted with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Terminology2.1 Definitions:2.1.1 aggregationthe collecting of units or parts into amass or whole.2.1
9、.2 birefringenceproperty of some crystals having morethan one refractive index. This will result in interference colorswhich are viewed through a polarized light microscope.2.1.3 grainsthick tablets having nearly equal width,breadth, and thickness.2.1.4 habitthe external morphology of the crystal.2.
10、1.5 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 microliters.2.1.6 nailsa skeleton of some kinds of triangles, elon-gated, usually pointed with a short head usually thicker orbroader.2.1.7 needl
11、es (acicular)long, thin crystals with pointedends.2.1.8 nuggetsirregularly formed grains without sharpfaces or edges.2.1.9 plierscrystals resembling pliers, generallyX-shaped.2.1.10 razor bladesthin oblong crystals with length abouttwice the width, resembling a safety razor blade.2.1.11 sheaveselong
12、ated 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 Criminalistics.Current edition approved March 1, 2007. Published March 2007. Originallyapproved i
13、n 2001. Last previous edition approved in 2001 as E 212501.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.2.1.12 skeletal crystala crystal in which all of the spacesin the crystal lattice are not occupied.2.1.13 spindlesshorter than
14、 course needles, but moresubstantial cross-section.3. Summary of the Technique3.1 A small sample of the material containing the suspectedphencyclidine or its analogues is dissolved in a dilute acid andthe appropriate precipitating reagent is added. The crystals thatare formed are observed and distin
15、guished utilizing a lightmicroscope.4. Significance and Use4.1 The technique produces a chemical-precipitation reac-tion between the phencyclidine or its analogues and theprecipitating reagent. The habit and the aggregation of thecrystals formed may be used to distinguish phencyclidine or itsanalogu
16、es from other drugs.4.2 The technique can be utilized on phencyclidine or itsanalogues present in either the salt or free base form.4.3 The technique does not distinguish between salt and freebase forms.5. Interferences5.1 Diluents/adulterants present in combination with phen-cyclidine or its analog
17、ues 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 separate thephencyclidine or its analogues from the diluents/adulterants orto use other testing methods to analyze for phencyclidine or itsanalog
18、ues.6. Apparatus6.1 Standard light microscope capable of varying magnifi-cations including 1003 is needed for viewing the crystals.Polarized light attachment is not essential, but is desirablebecause crystals resulting from the precipitation reaction arebirefringent.7. Reagents and Materials7.1 10 %
19、 v:v acetic acid.7.2 10 % v:v hydrochloric acid.7.3 2 % w:v potassium permanganate in 0.5 % v:v phospho-ric acid.7.4 Gold bromide (HAuBr4) in diluted perchloric and aceticacids 0.55 g HAuBr4, 42 mL water, 37 mL concentratedperchloric acid, 21 mL glacial acetic acid.7.5 Gold chloride (HAuCl4) in acet
20、ic and sulfuric acidsHAuCl4in HOAc-4(1+1)H2SO4; 2 g. HAuCl4, 20 mL glacialacetic acid, 40 mL concentrated sulfuric acid, 40 mL water.7.6 Authentic phencyclidine PCP; 1-(1-phenylcyclohexyl)piperidine.7.7 Authentic pyrrolidine analogue of phencyclidine PCPy,PHP, 1-(1-phenylcyclohexyl)pyrrolidine.7.8 A
21、uthentic morpholine analogue of phencyclidine PCM,1-(1-phenylcyclohexyl)morpholine.7.9 Authentic thiophene analogue of phencyclidine TCP;1-l-(2thienyl)cyclohexylpiperidine.8. Calibration and Standardization8.1 The reagents utilized for these microcrystal tests are tobe tested for reliability using a
22、uthenticated phencyclidine or itsanalogues and negative controls following the prescribedprocedure. Only when it is determined that the reagents areproducing the expected response may the reagents be used inthe testing procedure.9. Procedure9.1 Potassium Permanganate9.1.1 Place a small sample (a few
23、 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.9.1.2 Dissolve the sample in a few microdrops of 10 %acetic acid or 10 % hydrochloric acid.9.1.3 Add a few microdrops of 2 % acidified p
24、otassiumpermanganate to the edge of the acid solution on the micro-scope slide. Add a coverslip.9.1.4 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 should be used
25、 to orient the polarizer in theeast-west direction and the analyzer in the north-south direc-tion, verified by a black background.9.1.5 The crystal formed will depend on the drug present, ifany. The formation that can be expected for phencyclidine andits analogues are as follows:9.1.5.1 PCP (phencyc
26、lidine) produces purple razor bladecrystals. In high concentrations, the crystals resemble needlesimpaling small spheres.9.1.5.2 PCPy produces purple plier-shaped crystals withembedded nuggets and irregular forms.9.1.5.3 PCM produces unremarkable crystals.9.1.5.4 TCP produces unremarkable crystals.9
27、.1.6 If a dense cloud of precipitate is formed upon additionof the precipitating agent, the crystals may not be readilyvisible. It may be necessary to repeat the test reducing theconcentration of suspected phencyclidine or its analogue. Thisis done by either decreasing the sample size or increasing
28、thevolume of solvent.9.2 Gold Bromide in diluted Perchloric and Acetic Acids9.2.1 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.9.2.2 Dissolve the sample in a few microdr
29、ops of 10 %acetic acid or 10 % hydrochloric acid.9.2.3 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.9.2.4 Observe the formation of crystal using a properlyaligned and adjusted light
30、microscope. The observation can bedone between crossed polars, if desired. If crossed polars 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.E21250729.2.5 The crystal formation will depend o
31、n the drug present,if any. The formation that can be expected for phencyclidineand its analogues are as follows:9.2.5.1 PCP (phencyclidine) produces red-gold coloredsquares with diagonal markings, often elongated along oneaxis; birefringent; in high concentrations, colorless nails.9.2.5.2 PCPy produ
32、ces aggregates of tiny rods andX-shaped crystals; birefringent.9.2.5.3 PCM produces amorphous oily drops which slowlyaggregate into plates.9.2.5.4 TCP produces thin X-shaped crystals, often withgrossly elongated arms; birefringent.9.2.6 If a dense cloud is formed upon addition of theprecipitating ag
33、ent, 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.9.3 Gold Chloride in Acetic and Sulfuric Acids9.3.1 Place a sm
34、all 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.9.3.2 Dissolve the sample in a few microdrops of 10 %acetic acid or 10 % hydrochloric acid.9.3.3 Add a few microdrops of gold chloride
35、 in acetic acidand sulfuric acid reagent to the edge of the acid solution on themicroscope slide. Add a coverslip.9.3.4 Observe the formation of crystal using a properlyaligned and adjusted light microscope. The observation can bedone between crossed polars, if desired. If crossed polar areused, car
36、e 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.9.3.5 The crystal formation will depend on the drug present,if any. The formation that can be expected for phencyclidineand its analogues are as follows:9
37、.3.5.1 PCP produces unremarkable crystals.9.3.5.2 PCPy produces yellow X-shaped crystals.9.3.5.3 PCM produces H-shaped plates with widened ends.9.3.5.4 TCP produces yellow thick needles, some withshort, perpendicular central arms.9.3.6 If a dense cloud is formed upon addition of theprecipitating age
38、nt, 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.10. Interpretation of Results10.1 The three precipitating reage
39、nts 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 (phen-cyclidine), PCPy, PCM, and TCP from each other.10.2 If crystals structurally similar to those f
40、ormed byauthenticated phencyclidine and phencyclidine analogue stan-dards are formed by at least two of the precipitating agents, thesample may be considered positive by this technique for thepresence of either PCP, PCPy, PCM, or TCP.10.3 All observed crystalline precipitates must be docu-mented and
41、 included in the analysts notes for each itemanalyzed.11. Precision and Bias11.1 No information is presented about either the precisionor bias of this technique.12. Keywords12.1 microcrystalline testing; morpholine analogue of phen-cyclidine, PCM; phencyclidine, PCP; pyrrolidine analogue ofphencycli
42、dine, PCPy; thiophene analogue of phencyclidine,TCPREFERENCES(1) Fulton, Charles C., Modern Microcrystal Tests for Drugs, Wiley-Interscience, New York, 1969.(2) Clarke, E. G. C., Isolation and Identification of Drugs, PharmaceuticalPress, London, 1971, pp. 139-141.(3) Chamot, E. and Mason, C., Handb
43、ook of Chemical Microscopy,Volume 1. John Wiley, New York, 1930.(4) Evans, Hiram K., “Microcrystal Tests for the Characterization of Some1-Arylcyclohexylamines,” American Academy of Forensic Sciences,Cincinnati, Ohio, 19 Feb. 1983.(5) Harris, H. et al., “Vegetable Matter Coated with a Barbiturate an
44、d aVeterinary Anesthetic,” Microgram, Vol. 10, No. 1, Jan. 1977, pp.9-10.(6) Epstein, R. L. and Lorimer, P., and Sloma, E. J., “Identification ofPhencyclidine-Related Drugs,” Microgram, Vol. 22, No. 1, Jan. 1977,pp. 61-69.(7) Koles, J. E., “Some Microcrystal Tests for Drags” in Progress inChemical T
45、oxicology, Vol. 5, ed. A. Stolman, Academic Press. SanFrancisco, CA, 1974.(8) “Miscellaneous Tests and Procedures,” Microgram, Vol. 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. 191-196.E2125
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49、ittee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).E2125074
