X-ray diffraction studies of cocaine and its substitutes

Sections

Abstract
Introduction
Experimental
Experimental data
Conclusion
Acknowledgements
Bibliography
MISCELLANY
NOTIFICATION OF DRUG ADDICTS IN THE UNITED KINGDOM

Details

Author: Robert C. SULLIVAN, Kevin P. O'BRIEN
Pages: 31 to 40
Creation Date: 1968/01/01

X-ray diffraction studies of cocaine and its substitutes

Robert C. SULLIVAN New York City Police Laboratory
Kevin P. O'BRIEN Assistant Professor of Police Science at Monroe Community College, Rochester, New York

Abstract

The identification of cocaine and its many substitutes of local anaesthetic effect by the use of X-ray diffraction using the goniometer is discussed. It is important in fighting the illicit traffic to be able to differentiate conclusively between cocaine, which is a narcotic and the many cocaine substitutes which are non-narcotic.

The data presented is an attempt to provide useful information to establish a reference chart for the purpose of identification of cocaine and its many substitutes where no such identification charts of standardized values exist today. The developed patterns are expected to facilitate the identification of these chemical substances in an attempt to increase the usefulness of X-ray diffraction techniques specifically for law enforcement agencies.

Introduction

There is no discussion attempted in this paper of X-ray optics, crystallography or the interpretation of diffraction patterns due to the preponderance of this material in the literature. The assumption is made that those to whom this paper can prove helpful will have long past the elementary stages in X-ray diffraction theory and, therefore, it presumes a good knowledge of X-ray diffractometry.

The present diffraction equipment at the New York City Police Laboratory consists of two powder cameras and the associated electronic circuits for the goniometer. The X-ray unit contains a copper target tube mounted on a standard Norelco 50 Kv power unit. The Norelco X-ray diffraction unit and goniometer are used extensively at the New York City Police Laboratory. Almost all of the cases coming within the purview of the Instrumentation Section require rapid, accurate and absolute identification. The tech-dques of identifying crystalline material by other means than X-ray diffraction have been found not o be sufficiently specific when one is working with small amounts of complete chemical unknowns. The x-ray unit very often supplies information difficult or impossible to obtain otherwise. The questioned crystalline material can be identified more conveniently, more surely and with less labor than with other more standard methods. In the normal problem situations confronting the forensic chemist, the evidence is usually extremely limited and often contaminated. The information obtained through the use of diffraction instruments yields very useful investigative leads and constitutes valuable evidence for presentation at a future trial.

In attempting to identify unknown compounds with X-ray diffraction techniques, the ASTM card index is sufficient for most cases. However, in the cases where there are no existing ASTM cards available, extra and repetitious identification procedures become necessary. At the New York City Police Laboratory it has become apparent that there is a need for additional and adequate physiochemical characterizations of cocaine and its substitutes. It is with this realization of the need for additional reference patterns of unknown crystalline substances not yet supplied in the ASTM index file that this paper is written.

Experimental

Methods and Materials

Quite acceptable diffraction patterns have been obtained from small amounts of sample in this study. In adapting the Norelco X-ray diffraction unit and the electronic circuits to this problem, 50 mg of dried, pure, known powder was sprinkled on to a glass slide that had been previously moistened with a silicone lubricant. This random sprinkling of the powder keeps to a minimum the problems arising from insufficient orientation of the sample being tested. A qualitative spectra of the crystalline sample may be obtained by recording the intensities at all the pertinent angles. The major elements responsible for the prime peaks obtained on the goniometer recorder can be determined accurately by measuring the net intensities above the standard background level.

Sample preparation:

- 50 mg of chemically pure, dried powder of known identity

- Mix well in agate mortar to pass a 200 mesh screen

- Glass slide to fit, with a silicone lubricant

- Random sprinkling of the powder

Excitation:

- Emission from a copper tube (1.54A) operated at 35KvP and at 18 ma

Lines measured:

- Descending pattern 75 degrees to 3 degrees

Calculations:

- Net intensities above background level

Slits used:

- Divergence 1 degree

- Receiving 0,03 inch

- Scatter 1 degree

Scanning rate:

- One degree per minute (this seems to be a convenient compromise which provides fully usable data, without the loss of important information)

Experimental data

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Conclusion

Satisfactory working charts for an identification file for Cocaine and its substitutes have been developed using the goniometer and the glass slide technique.

An experienced X-Ray Diffractionist must always be aware that there is a slight discrepancy index due to internal characteristics of each particular instrument and the various parameters used in each instance. These small variations from the normal or expected readings are present when one wishes to reexamine or to duplicate anothers experimental data. The dis-crepancy index should allow a slight correction to be made for the chance variations in the numerical inten-sities observed and here reported. These deviations do at times, necessitate a wider selection of the number of stronger lines than one might wish, in order to iden-tify the unknown substance. (This method is in no way different from the normal searching procedure used when one wishes to identify an unknown chemical substance.) The extent or seriousness of this correlation is considered relatively small and completely indepen-dent among the many materials measured. This.problem is not unique to this area of investigation or to any other field of endeavor, where attributes capable of numerical measurement are involved.

To the accomplished X-Ray Diffractionist, the methods used are simple and at the same time they produce the most valuable of analytical characteristics in modern forensic science.

40 Miscellany

Acknowledgements

The authors of this paper gratefully acknowledge and wish to thank Professor Lewis Wright, Chairman of the Department of Police Science at Monroe Col lege and Captain Joseph P. McNally, Commanding Officer of the New York City Police Laboratory for their continued interest and encouragement in our endeavours to apply scientific investigative tools as additional aids in modern criminal investigations.

Bibliography

Azaroff, L. V. and Buerger, M. J., The Powder Method (McGraw Hill Book Co., New York, 1958).

Bradford, M. and Gabarino, J. J., Journal of Criminal Law, Criminology and Police Science, Volume 44, 1954, Northwestern University School of Law.

Cloutier, J. A. R. and Manson, Jane M., Applied Spectroscopy, Volume 15, 1961 ("Identification of Barbiturates by X-Ray Diffraction ").

Hanawalt, J. D. and Renn, H. W., Industrial and Engineering Chemistry, Analytical Ed, 8, 1936.

Henry, N. F. M. and Lipson, H., Interpretation of X-Ray Diffraction and Diffraction Patterns, D. Van Nostrand, Amsterdam, 1951.

Hull, H. W., Journal of American Chemical Society 1168, 1919.

Klug, H. P. and Alexander, L. E ., X-Ray Diffraction Procedures, John Wiley & Sons, New York, 1954.

Parker, J. B., "A Statistical Treatment of Identification Problems", Journal of Forensic Science Society, Volume 6, 1966.

Parker, J. B., "The Mathematical Evaluation of Numerical Evidence", Journal of Forensic Science Society, Volume 7,1967

MISCELLANY

ESTABLISHING THE PRESENCE OF COCAINE IN NOVOCAINE MIXTURES-QUALITATIVE ASPECT

An analysis for the detection of cocaine in the presenceof procaine has been developed by Dr. Manual A. Guatelli, Professor, and Juan C. Garcia Fernandez, Assistant Professor, School of Pharmacy and Biochemistry, Buenos Aires. The report of the analysis of three cocaine samples submitted to expert examination shows the usefulness of the recommended method; two of the three samples were adulterated with procaine (novocaine), and this seems to be a frequent characteristic of cocaine passed in the illicit traffic today.

The paper contains detailed description of the physical examination and chemical tests useful for the detection of an eventual adulterating agent in a sample of cocaine (examination under UV light, solubility tests, potassium permanganate test, detection of basic acid), and the recommended specific chromatographic method for the separation and identification of cocaine and procaine. ( International Criminal Police Review, 1967, No. 211, p. 211-228.)

NOTIFICATION OF DRUG ADDICTS IN THE UNITED KINGDOM

Under the Dangerous Drugs (Notification of Addicts) Regulations [ 1] which came into operation in the United Kingdom on 22 February 1968, medical practitioners are required to send particulars of addicts to narcotic drugs to the chief Medical Officer of the Home Office.

A doctor will not be required to notify addicts who need the drug for relief of pain or those for whom particulars have already been provided in the previous twelve months. To help in doubtful cases of addiction, the Ministry of Health has appointed an advisory panel with 65 members providing wide geographical coverage throughout England and Wales; after a consultation the panel member will provide the referring doctor with a written report, sending a copy to the Ministry of Health. If nothing further has been heard about a case within twelve months of the notification being received, further inquiries will be made of the notifying practitioner. This notification procedure paves the way for further Regulations which will limit the prescription of specific drugs for addicts to licensed doctors at special treatment centers ( The Lancet, 1, 7538, 1968.)

r001

1 Dangerous Drugs (Notification of Addicts) Regulations 1968. S.I., 1968 No. 136. H.M. Stationery Office, 6d.