27th SEMI-ANNUAL SEMINAR (Spring 1966)
CALIFORNIA ASSOCIATION OF CRIMINALISTS
May 6-7, 1966
SANTA ANA, CALIFORNIA
DRINK-KHANA - A DEMONSTRATION OF THE EFFECT OF ALCOHOL UNDER ACTUAL DRIVING CONDITIONS
John Davidson, San Bernardino County Sheriff's Office
This 26 minute color-sound movie was edited primarily for presentation to service clubs for public education of the fact that relatively low blood alcohol concentrations do significantly impair driving ability. The film shows a complete sober lap of one driver running the gymkana course with no errors and then shows a full lap of the same driver after drinking, when he made 9 errors even though driving 10 per cent slower. This film also gave a very detailed description of the driving course outline and stressed that an individual does not have to be staggering drunk before losing his normal driving skills.
Copies of the film can be obtained at the cost of copying (approximately $130.00). A copy of the film will also be available for single showings by interested members or for previewing before ordering copies.
DRINK-KHANA, RESULTS AND COMMENTS
James M. White, San Bernardino County Sheriff's Office (Co-authored by Robert G. Cranston, Anthony Longhetti and John Davidson)
The two-page handout gave the course outline, course details and the data of the results of the drink-khana on 6 male subjects who reached alcohol levels of 0.07 to 0.12% (Breathalyzer).
The purposes given for the study were:
- demonstration to judges, attorneys and law-enforcement personnel that significant driving impairment is developed, at relatively low blood alcohol concentrations,
- production of the movie for showing to the general public,
- background information for criminalists testifying on the interpretation of blood alcohol levels, and
- to serve as a pilot study for future studies.
The course included parallel parking, stopping at a pedestrian stop, parking in garages, making a U-turn, negotiating many turns and passing through a narrow lane. The drivers practiced the course the day prior to the actual test which consisted of driving the .56 mile course, two laps sober and two laps after drinking.
White concluded that the course could be improved by reducing the U-turn area width from 32 feet to about 24 feet, eliminating the straightaway used for braking tests (not satisfactory due to speed control inaccuracy and driver anticipation) and increasing the number of traffic cones on the course.
The main features of the course that were believed to be of particular value were its length, varied driving skills required and its simplicity. The cost of the demonstration was $178.00 which could probably be reduced. Much use was made of loaned services and equipment. Success of demonstrations of this type depends on preplanning, making results readily available to attending audience via P.A. system and crowd control.
Discussion of the movie and the drink-khana centered about whether the study was a scientific study or a demonstration. Not all variables can be controlled or factually considered (i.e., effect of audience on driver attitude, use of placebos, limited number of subjects, social and psychological factors, etc.) in a study of this type. It was therefore generally agreed that studies of this type would best be termed demonstrations; but, demonstrations of this type are still of value both to the public and to the expert interpreting blood alcohol levels.
EFFECT OF PHASING ON SIMULATED TOOL MARKS; A NEW TEST FOR INDEPENDENCE IN STOCHASTIC PHENOMENA
James Brackett, San Mateo County Coroner's Office
Brackett reported on his continuing study of mathematical analysis of simulated toolmark striations and related his synthetic mathematical models to Biasotti's bullet comparison data.
Brackett stated that the purpose of the study is to develop a basic understanding of tool marks which will enable us to determine the interrelationship of the underlying factors and make a more realistic approach to evaluating a toolmark in actual case work. Eventually he expects to develop means of considering the striae, the effect of different densities of two otherwise identical marks and the effect of superimposed marks.
CONSIDERATIONS OF IDENTIFICATION POSSIBILITIES BEYOND THE CONVENTIONAL BULLET AND SHELL STRIAE
C.M. Wilson, Wisconsin State Crime Laboratory, Madison, Wisconsin (co-authored by W.J. Cadman, Orange County Sheriff's Office)
This presentation actually covered several topics relative to firearms problems, all of which are quite noteworthy.
IDENTIFICATION OF MULTIPLE EXTRACTOR DRAG MARKS
over the rim of unfired cartridges caused by the repeated hand ejections of a live round from automatic weapons.
IDENTIFICATION OF "MONKEY'S PAW" IMPRESSIONS on the primer cup of unfired cartridges which result from the chattering of the firing pin on the primer. These marks can only be expected in cartridges that have been hand ejected in an unfired condition, as the deep firing pin impression from firing would obliterate the light chatter marks. This type of mark is produced by semi-automatic weapons that use the firing pin as the ejector. Seven .25 automatics use the firing pin as the ejector and produce this type of mark. These include the Belgium Baby Browning, Ortgies, Galesi, Beretta, Duo and Colt Vestpocket.
IDENTIFICATION OR COMPARISON OF CARTRIDGE LOTS BY MANUFACTURING MARKS; Cartridges are manufactured in a series of totally separate operations, each of which may have produced individualizing marks of the tools at the particular times that step was performed.
BUNTER DIE is the die used to impress the headstamp impression on the cartridge head, and it is in turn produced from a single master die. The bunter die, therefore, starts with some master die characteristics which will be present on each new bunter die. Through use, accumulation of scale and cleaning of the die with crocus cloth, changes occur in the original characteristics from the master die, with the production of numerous new individual characteristics. Wilson has noted significant changes within a run of 70,000 cartridges, with changes having taken place in characteristics after each 10,000 which were selected and examined.
TURNING MARKS on the edge of the rim and in the recess forward of the rim of semi-rimless cartridge cases. The head and the recess are trimmed by a turning operation with a knife which has to be reground quite frequently. The regrinding, of course, produces new characteristic s on the trimming knife, so that only cartridges turned at about the same time will have Identical characteristics In this area.
OTHER MANUFACTURER'S MARKS which apparently haven't been extensively studied at this time but which may be of value in identifying cartridge lots include these produced in forming the seating cannelure and primer pocket, in trimming the cartridge mouth and in drawing the cartridge case, as well as marks produced in the formation of the anvil of the primer itself.
USE OF SOFT X-RAYS in examining clothing and tissues can produce information of value in many cases. Wilson recommended the use of M-type X-Ray film and a Beryllium window X-Ray tube at potentials of 14,000 to 30,000 volts.
EXAMINATION OF CLOTHING; Using a modified X-Ray cassette in contact with the clothing, it is possible to locate and identify metal shearings present from the proximal discharge of a weapon and supplement the powder pattern comparison. Sand grains are easily differentiated from metal fragments by their surrounding diffraction pattern.
TISSUE AND BODY RADIOGRAPHS may be useful in determining at least some of the characteristics of embedded bullets, which sometimes are not removed for medical reasons or because the shooting victim refuses their removal. Actual measurements of the radiograph cannot be made, but the curvature and ratio, measurements can be compared to standard bullets to elicit some information, particularly if a good profile is obtained. Secondarily, body x-rays may show metal fragments along the wound tract following striking of bone, which is indicative of the projectile having been a non-jacketed bullet.
COMMENTS ON BUREAU OF DRUG ABUSE CONTROL (BDAC)
Patric V. Fuller, United States Food and Drug Administration, BDAC, Western States Field Station, Los Angeles
The new Federal laws on dangerous drug controls are formally known as the Drug Abuse Cosmetic Amendments of the Pure Food, Drug and Control Act. At the time of the seminar, the new publication of the Act with Amendments was not available, but Fuller promised to furnish copies to all laboratories.
The Amendments specifically cover barbiturates and amphetamine and provide for an administrative process to add to the control list other dangerous and potentially habituating drugs. It now includes 7 tranquilizers, 1 CNS stimulant and 6 hallucinogenic agents.
The legislative intent of the new amendments was one of control, and they specifically exclude possession for family use. All manufacturers, wholesalers, jobbers and distributers are required to register. Exempt from registration are retail pharmacies, hospitals, clinics, public health agencies, physicians, research institutes (including educational institutions) and law enforcement. Both the registered and excluded industries and professions must keep records on the type, size, number, source, and distribution or disposal of the specified dangerous drugs.
BDAC will carry out an audit program from manufacturer to ultimate consumer to find diversions of legitimately manufactured drugs and will be searching undercover for the diverted, counterfeited and illegally imported drugs.
Presently, 9 billion pills are produced annually, approximately half of which are diverted to wrongful use.
First offenses are misdemeanors, and second offenses are disposing to a minor (16-21 years) are felonies. A prescription can only be filled 5 times and is valid for only 6 months. A counterfeit clause allows the seizure of all related manufacturing materials and equipment and also covers counterfeit labeling.
PAINT ANALYSIS AND THE USE OF THE INFRARED SPECTROPHOTOMETER
David Q. Burd, Department of Justice, Bureau of Criminal Investigation and Identification
A general review of standard methods used in the comparison of paint particles in the Criminalistics Laboratory. Special emphasis was placed on the infra-red technique using KBr pellets. Valuable information can be obtained from very small traces of paint (even less than 0.1 mg). In bit-run investigations such studies rapidly identify which of the commonly used automobile paints is involved. When concerned with house or related paints, an infra-red analysis has even more value due to the great variation in oils, plastics and other paint vehicle components used by manufacturers. These are also occasionally changed in the same type of paint vehicle components used by manufacturers. These are also occasionally changed in the same type of paint as developments and improvements occur in the paint industry. Although IR analyses do not result in conclusive identification of paint, they materially aid in laboratory analyses, rapidly indicate basic differences or similarities in paint specimens which have the same color and appearance and supplement other analytical procedures. (Abstract furnished by author).
NEW YORK STATE IDENTIFICATION AND INTELLIGENCE SYSTEM
Charles Kingston, Consultant, NYSIIS, Albany, New York. (In absentia)
This black-and-white film narrated by Jack Webb (formerly of Dragnet) presented the record retrieval system being initiated by New York State. This is a centralized record system by which any of 3600 agencies in New York State can obtain information by the tie lines needed for the investigation of a crime (i.e.; M.O., physical descriptions, developing listings of possible suspects, obtaining criminal records, etc.) or background information on the defendant needed by the prosecution or for probation or parole.
REPORT OF THE 4TH INTERNATIONAL CONFERENCE ON ALCOHOL AND TRAFFIC SAFETY
Lowell Bradford, Santa Clara County District Attorney's Office (Handout prepared by Anthony Longhetti, San Bernardino County Sheriff's Office)
Bradford went over the titles of the papers presented at the conference and made short comments about many of them. Anyone interested in the drinking driver problem or who is testifying on interpretation of blood alcohol levels should obtain copies of the Proceedings of this and earlier meetings.
Bradford also noted that the Committee on Alcohol and Drugs of the National Safety Council has changed membership requirements and will now admit to membership people who are testifying on blood alcohol interpretation. Any member "on the firing line" that is interested in joining the committee should contact Bradford.
HISTORICAL DEVELOPMENT OF CRIMINALISTICS
Duayne J. Dillon, Contra Costa County Sheriff's Office
The purpose of the paper was to trace the history of criminalistics in California and compare it to the rest of the United States. Dillon's research of the history is not completed and time did not allow him to present all the information that he has developed so far, so we can expect to hear more from him in the future on this.
Dillon expressed the opinion that criminalistics developed as a separate discipline at the beginning of the 20th Century, although many of the sub-divisions date back much further; e.g., fingerprints, toxicology, documents, firearms.
The Los Angeles Police Department Laboratory was reported to be the first laboratory in California, with the first police chemist appointed in 1923. In fact, the first in the United States and perhaps the first in the world, although law enforcement had made use of consultant scientific examinations in many isolated cases earlier.
REFILLED LIQUOR BOTTLES
Herman Meuron, Alcohol and Tobacco Tax Division, United States Internal Revenue Service, San Francisco (Abstract furnished by Author)
Refilling of liquor bottles is a Federal offense, as well as a State offense. Refilling, if done at all, is generally done at the retail outlet level - the bar. It is an economic cheat of the consumer, generally a cheaper or less popular brand being poured into a bottle of a more desirable or higher priced brand and then served to the customer.
The chemical tests made consist of proof, total solids, total acids calculated as acetic, total esters calculated as ethyl acetate, aldehydes as acetaldehyde, fusel oil, color calculated as Lovibond 1/2" cell, and Organic Soluble Color. All tests are in the AOAC Book of Methods.
The analytical values of the questioned samples are compared with control bottles of authentic liquor and also by reference to previously compiled data and a decision is made based on how closely the figures match or differ. Partial refilling is a problem and also the same analytical values are found for a small number of different brands. Watering is easily detected as well as evaporation. Gas chromatography, UV spectroscopy and neutron activation are useful only in a few special cases.
PHOTONUCLEAR ACTIVATION ANALYSIS IN FORENSIC STUDIES
Dorothy M. Settle, General Atomic, San Diego
Photonuclear activation is a new method of activation analysis which produces different isotopes than neutron activation and thus furnishes another means of elemental determinations with different sensitivities and interferences. Its main advantage lies in the fact that sodium does not interfere, thus allowing direct examination of many samples such as glass and biological materials.
The work with photonuclear activation has just begun, and it will be necessary to run standards to identify peaks, determine optimal activation conditions and determine the sensitivities and calibrations.
Settle showed several example samples that she has run on such items as plant material, glass and paper. She requested suggestions of types of materials that criminalists would like surveyed.
NEUTRON ACTIVATION ANALYSIS IN CRIME DETECTION
Donald Bryan, General Atomic, San Diego
This film, "The Nuclear Witness", was produced by the Atomic Energy Commission, Division of Isotope Development, in conjunction with General Atomic. Bryan stated that the film was aimed at the educated lay-man and is not a training film, but is designed to show the applications of N.A.A. to law enforcement.
The film implied that a single hair is sufficient for identification. It portrayed the San Mateo paint case (previously extensively discussed in seminars) using the same probability numbers and the statement that "we can talk very accurately in terms of probability" and implying that the paint probability identification was similar to fingerprint identification. The film also showed the use of N.A.A. of paraffin casts for gun shot residues and possibly implied conclusions stronger than warranted. It similarly compared numerous marijuana seizures. A statement is made in the film that one of the most important developments of N.A.A. is in the characterization of human hair.
In the discussion following the showing of the film, some of the comments included:
- just because identical chemical values are obtained doesn't necessarily mean that they are from the same source,
- what is acceptable in court is what is acceptable to the profession,
- the overall impression left after viewing the film Is that N.A.A. does produce conclusive identifications and the conclusions offered in the film are in many cases probably not warranted, and
- General Atomic will be doing themselves and criminalistics a disservice in the general showing of this film.
RESULTS OF INTERNATIONAL N.A.A. COMPARISON OF HAIR
Don Bryan, General Atomic, San Diego
Six N.A.A. laboratories examined samples of hair from the same individual, and the analytical results for both bulk samples and for single strands were compared. None of the laboratories agreed on either quantitative or qualitative results on even the bulk hair samples. General Atomic results on multiple single strand analysis showed considerable variation of hair from the same person. Different methods of washing the hair cause considerable variations in the analytical results.
Bryan expressed the opinion that neutron activation analysis of hair is not of sufficient value at the present time to warrant the time and considerable expense, except possibly in the examination of bulk hair samples.
Bryan also expressed the opinion that N.A.A. is not the cure-all, end-all ultimate examination of evidence, but is merely another method of analysis through which additional information of value can be obtained, and, in some cases of minute evidence, it is the only method of determining elemental content.
PRESENT STATUS OF ATOMIC ABSORPTION SPECTROSCOPY
J. Ramirez-Munoz, Ph.D., Beckman Instruments, Fullerton, California
Atomic absorption instruments can be used for both qualitative and quantitative analysis. Its advantages are simplicity, sensitivity, rapidity, accuracy, and expense. Dr. Ramirez-Munoz discussed the general parameters of analysis that must be considered by the user. Possible applications given for criminalists included
- toxicology-heavy metals (As, Sb, Hg),
- classification of paints in art paintings (Zn, Ag or Ti whites),
- identification of Fe in iron gall inks,
- bronze and zinc alloys,
- paints, and
- Sb and Ba in paraffin casts (especially Ba).
Editorial Secretary note; not all papers scheduled could be presented due to the late hour. Four of these were presented to the Editorial Secretary to include with the abstracts, and copies are attached.
A RAPID SPOT TEST FOR DIFFERENTIATING AMPHETAMINE AND METHAMPHETAMINE
W.Jerry Chisum, Kern County Sheriff's Office, Bakersfield, California
It is often desirable to obtain a rapid presumptive identification of amphetamine in pill form. It is generally known that amphetamine and methamphetamine give a golden brown color with Marquis reagent. Both are common sympathomimetics used in many commercial drug forms, including white, double-scored tablets. The use of Marquis reagent and the following described test will differentiate amphetamine and methamphetamine and thus aid the tentative identification pending further specific identification by other more time consuming methods.
|1.||5% CuSO4|| Combine 1 and 2 before use, adding sufficient ammonia to form the bright blue complex|
Crush a small amount of the tablet to be tested in a spot plate. Add a drop of the CuNH4SO4 reagent. Stir. Add a drop of CS2. A black or dark brown color indicates a secondary amine (methamphetamine).
Barbiturates and starch do not interfere; however, as any secondary amine will react, further identification is necessary.
Fiegl, F.: Spot Tests in Organic Chemistry, 8th Ed.
INDIVIDUAL AND CLASS CHARACTERISTICS OF TOOLS
David Q. Burd and Allan E. Gilmore, Criminalistics Laboratory, California State Bureau of Criminal Identification and Investigation
Care must be taken when conducting toolmark comparisons to distinguish between class and individual characteristics of tools. Some mass produced tools, particularly those formed in a punch press or by the die forge process may contain identical surface structure which will result in correspondences between impressions made by different tools. In the case of abrasion markings made by new and unused tools there are usually sufficient differences, due to accidental damage, to distinguish between them. In some instances, however, markings which appear to be highly characteristic of a tool may be found in marks made by more than one tool; thus, great care must be taken in conducting such examinations. A thorough study of the tool in question is always essential to establish which markings present are class and which are individual characteristics.
Several slides were shown to illustrate this subject. These included photographs of three new screwdrivers formed by dies in die stamping or forging equipment. Comparisons of abrasion markings produced by these tools were also shown. Some of these corresponded exactly, and others were quite different depending upon the area of the tool employed in producing the abrasions. Thus, some markings were truly individual marks of the tools while others were only class characteristics.
RESTORATION OF OBLITERATED HANDWRITING
L.B. Miller, Criminalist, Los Angeles Police Department
The problem of restoring the original handwriting of a document which has been obliterated by overwriting has long been a problem of the questioned document examiner. Many successful attempts at restoration have been made by means of the application of various wave-lengths of various solvents and/or solvent mixtures, the use of lighting techniques, or the location of pressure indentation of the underwriting have also succeeded in restoring the original writing. A new successful technique is added to this list which can be called the "pin-prick" method.
It is the purpose of this paper to relate the simple pin-prick method of restoring obliterated writing caused by overwriting. This technique should supplement current valid methods used for restoration.
In the application of this technique, one prerequisite is necessary; the color of the overwriting of the questioned document must be visually discernible from the color of the original writing with the aided eye. The necessary tools are limited to a low-power microscope and a dissecting or teasing needle with a short shaft and a relatively sharp point.
The questioned document is examined preliminarily under the microscope and a determination is made as to the color of the original writing. The document is placed on a pad which will allow the needle to easily make a hole in the document. * Thin cardboard, such as is found backing a note pad, has been found to be satisfactory for this purpose. While viewing the document under magnification, the needle point is located over the document at a point where the fibers show contamination by the color of the original writing. Holding the needle as vertical as possible, a small hole is made. The needle is then moved to an adjacent area showing the same color and another hole is made. Care should be exercised not to place the holes too close together as it may be necessary to enlarge them to record the results and, if they are too close originally, the resultant enlarging will cause the paper to part in a continuous tear. It is usually necessary to enlarge the holes for recording the results when the paper stock is thick.
After completing the task of placing the holes in all the areas where the original color is found, the document can be read by holding it to the light. Recording the results are effected by photographing the finished document using transmitted light.
* If the document must be preserved a color photograph can be used.
The salient features of two investigations which have come to the attention of this laboratory are summarized below.
Case No. 1
An obscene note was sent to a female via Inter -Departmental mail. The sender employed the use of an Inter-Departmental Correspondence envelope on which the point of origin of the obscene note was indicated by a previous red pencil address. Inasmuch as the sender of the obscene note obliterated the red pencil address with a blue pencil, no part of the red writing was visible when the document was received in the laboratory for examination. Following examination of the document and application of the known techniques without success, an attempt was made to remove the heavy layer of blue pencil using a solvent. The fourth application of the solvent revealed the presence of illegible red writing. One fiber contaminated with the red was checked in various solvent systems for solubility against the solubility of the blue. Unfortunately, both colors showed identical reaction in all the solvents tried. Further attempts using the standard methods of restoration were unsuccessful. Restoration was made using the pin-prick method.
Case No. 2
In this example we have a non-criminal matter in which a gag letter was addressed to the laboratory. It was felt that the pin-prick technique of restoration could be applied as an illustration of the restoration method. Again an Inter-Department Correspondence envelope was used to transport the letter and the question - academic at this point - was: in what office had the envelope originated? The last three entries, or addresses, are of particular interest. The first of these entries, written in red, is the address of the individual who had sent the envelope to the culprit. This red address was lightly overwritten with a black ballpoint pen when this party addressed the envelope to the cul-prit in the same black ballpoint ink. The next entry is, therefore, the culprit's address which has been heavily overwritten with a purple ballpoint pen ink completely obliterating the writing. The same purple ink was then used in addressing the envelope to the "Crime Lab". Thus the color of the two inks in which we are interested can be seen clearly in the first and third entries and the black color, which is of primary interest, is seen in the first entry. Direct application of the pin-prick method resulted in restoration of the unknown address. In addition to the restoration, an attempt was made to determine who wrote the restored writing to see if enough characteristics of the writer would show in the pinpricked restoration. Handwriting exemplars of the three individuals assigned to the office shown as the first entry were obtained and compared with the restored address. As there were sufficient individual characteristics present in the restored writing to make an identification, there was no difficulty in determining who had written the address.
A simple technique is offered whereby original handwriting obliterated
by overwriting with a writing implement of another color can be restored by making small holes at places on the document where the original color is found.
John Ragle, Criminalist, Orange County Sheriff's Department
This procedure is based on the suggestion of Gonzales1 indicating the separation of steam distillable drugs from tissue. Using a modified micro Kjeldahl steam distillation apparatus (suggested by F. Wynbrandt), 25 to 50 ml of urine is distilled from base to acid and the final sample plotted in the UV. The pH of the sample is shifted. If the results dictate, the sample is re-extracted, reduced to dryness and crystal tests performed on the residue.
UV Spectrophotometer, 340 millimicrons to 220 millimicrons Micro Kjeldahl distillation unit (Available from Van Waters and Rogers Cat. #51100, page 820.)
125 ml Separatory Funnels
100 ml Graduate Cylinders
Compound Microscope 100x
Saturated KOH (100 gms in 100 ml H2O)
Dilute HC1 (258 ml (36%) to one liter)
CaCO3, Reagent grade
Chloroform Reagent grade
0.2 NH2SO4 (5.6 ml of conc H2SO4 to one liter)
Sat. NaOH (42 gms in 100 ml H2O)
Sat. Picric Acid Reagent (1.4 gm per 100 ml)
Gold Chloride-Phosphoric Acid Reagent - 5% AuCl3 - Phosphoric Acid 2 to 1
.01% nicotine sulfate solution
Dow Corning Antifoam Spray
25 to 50 ml of urine is acidified with 1 to 2 ml of concentrated HC1.
The sample is placed in distillation apparatus with a "shot" of the anti-foam spray.
The sample is distilled and fraction #1 is collected and saved for later study if necessary.
Three (3) ml of saturated KOH is added by means of the stop cock on top of the distillation flask.
Fraction #2 is collected by placing the tip of the condenser into a 150 ml beaker containing 10 ml of dilute HC1.
The tip should be under the surface of the acid so that all volatile basic materials are salted out. Fifty (50) to seventy-five (75) ml are collected.
Fraction #3 is collected as was Fraction #2 and saved for possible analysis.
Fraction #2 is made basic by adding CaCO3 (enough to saturate and bring the pH to around 8.5).
The sample is extracted with 100 ml of CHC13.
The CHC13, is extracted with 0.2N-H2SO4(2), and plotted or read in the UV 340 mμ to 220 mμ. using a blank of 0.2N-H2SO4 saturated with CHC13
If the UV information indicates a sympathomimetic amine, the pH of the sample is shifted by adding 2 to 3 drops of saturated NaOH. The shift may be indicative of any of the S.A. as based on the information supplied in a paper by J. Davidson (3).
If the sample contains amphetamine, the first maximum at 263 shifts to 267 mm. There is a shoulder at 263, a new inflection at 260.5, and the absorptivity at 262 is decreased relative to the major peak at 257 which remains. The major point of identification is that the minimum which was at 228 shifts to 232-233. If the sample contains desoxyephedrine, the shift is the same as above with the exceptions that the minimum at 228 shifts to 238. If precipitate appears, add 2 drops of HO to each cell. (These shifts must be exact for an identification, since other sympathomimetic amines not mentioned in 23105 CVC may be present).
If the shifts are present, the basic sample is placed back into the original CHC13- and shaken. The aqueous is discarded.
Two (2) drops of concentrated HC1 is added to the CHC13, and it is reduced to dryness.
Place a small quantity of the residue on a micro-slide and add one drop of the Reagent. There should be an immediate precipitate visible followed by yellow oily beads visible (100x) around the inside edge of the drop. By scratching or tapping the drop with a micro-probe, the crystal should appear. Make crystals with known pure compound for comparison.
The major interfering material encountered is nicotine (259 mm), which steam distills along with the amphetamine. For a rapid test to see if there is a sympathomimetic amine under the dense nicotine peak at 259, it is suggested that dilute aqueous nicotine sulphate be added drop-wise to the blank. This differential procedure has met with limited success if the added nicotine does not use all the available reference energy. It is suggested that a chromographic separation of one type or another be made if justified by the results up to this point, since the nicotine from the urine will still interfere with the crystal tests.
1 Gonzales, Vance, Helpern and Umberger. Legal Medicine - 2nd Edition - Appleton-Century-Crofts.
2 Bradford and Brackett. Systemic Procedure for the Identification of Dangerous Drugs, Poisons and Narcotics by U.V. Spectrophotometry - Microchimica acta 1958/3.
3 J. Robert Davldson. Ultraviolet Absorption Curves of Some Sympathomimetic Amines and Related Compounds - San Bernardino Sheriff's Office - Unpublished.