29th SEMI-ANNUAL SEMINAR (Spring 1967)
CALIFORNIA ASSOCIATION OF CRIMINALISTS
May 25-27, 1967
SAN DIEGO, CALIFORNIA
NEUTRON ACTIVATION ANALYSIS OF BULLET LEAD
H. Richard Lukens, General Atomic Division, General Dynamics Corporation, San Diego
Examination of small samples of bullet lead by rapid nondestructive instrumental neutron activation analysis shows promise as a useful tool for the criminalist.
In a preliminary study, ten samples of bullet leads, each from a different caliber or manufacturer, have been examined; no two samples showed the same composition.
The method used in this work consisted of irradiating weighted (˜10mg) samples for 15 seconds in a thermal-neutron flux of 4.3 x 10¹² n/cm²-sec., followed by counting for 30 seconds with a 3 inch by 3 inch sodium iodide (thallium activated) counter coupled to a multi-channel pulse-height analyzer. The resulting gamma-ray spectra gave information concerning levels of antimony, tin, silver, copper, and aluminum in the samples.
The analyses proved to be very precise, as compared to the more conventional emission spectroscopy method. Antimony, for example, at the 3% level in lead was determined with a standard deviation of ± 3% of the value. Thus, two samples, each nominally containing 3% antimony, were easily distinguished from one another on the basis of the antimony determination, because the true levels of antimony were 2.8 ± 0.1% and 3.1 ± 0.1%, respectively. The latter sample also contained 0.21 ± 0.03% tin, grossly more than the former sample, which confirmed that the samples were not alike.
The NAA method should prove useful in comparing even a very tiny bullet fragment with unfired rounds in a particular weapon or box of cartridges.
- Cadman comment: Bullets from different batches may be encountered in a given box. In manufacture, a pool of bullets is subjected to continuous addition and withdrawal. This could complicate the Interpretation of the results.
- Bradford comment: Some manufacturers (such as Sierra) exercise greater control over minor fluctuations in composition.
- Cadman comment: Emission spectrograph may furnish as much information as the activation analysis, although quantitation is a problem.
- Lukens comment; Emission spectrography is valuable, but NAA affords greater precision and may be used as a nondestructive adjunctive method.
SOME INTERESTING RECENT CASE STUDIES INVOLVING NEUTRON ACTIVATION ANALYSIS OF DIFFERENT KINDS OF EVIDENCE MATERIALS
Donald E. Bryan, General Atomic Division, General Dynamic Corporation, San Diego
Physical evidence from four different cases were recently analyzed by neutron activation analysis. The first case Involved was the comparison of grease samples. One sample was obtained from a bicycle chain and was compared to grease found in a bicycle chain impression on the suspect's trousers. The chain was removed from a bicycle found at the scene and was allegedly used by the suspect. Al, Ca, Mn, Ha, and Cl were found in grease from both sources and were observed to agree closely with respect to the relative proportions of these elements. Grease from the trousers, however, showed the presence of Au, which did not appear in the grease from the bicycle chain.
The second case involved the comparative analysis of three buttons. One button was found at the scene of the crime and the other two were removed from a sweater belonging to a suspect. Neutron analysis indicated that one button was decidedly dissimilar to the others, and was actually mother-of-pearl instead of plastic as initially believed.
The third case, a kidnap-murder of a small girl, involved the analysis of two samples of fecal natter. One sample was removed from the raincoat of a suspect and was compared to a sample from the victim's panties. Comparison of the samples from the two sources by NAA proved inconclusive.
In the fourth case, two samples of hair were analyzed. One sample was known head hair removed from the victim. It was compared with hair found at a location suspected to be the crime scene. One hair was observed to have a substantial Br content, while the other hair was devoid of Br. One hair had either Sb or as, which could not be compared with the other due to the spectrum of the other being obscured by the Br.
- Guinn comment: These hairs were collected under ideal conditions and external contamination was minimized as much as possible. It is unlikely that one would find differences this large in hairs from one individual. Marked differences are observed in head and body hair.
THE LEVELS OF BARIUM AND ANTIMONY ON THE HANDS OF PERSONS WHO HAVE NOT RECENTLY FIRED A GUN
Kitty I. Perry and Dorothy M. Settle, General Atomic Division, General Dynamics Corporation, San Diego
The purpose of this gunshot-residue Investigation is (1) to increase the number of barium and antimony handblank values for a more complete statistical treatment of the average levels of barium and antimony found on the hands of persons who have not recently fired a gun, (2) to obtain handblank values from a large cross section of persons engaged in different occupations, and (3) to determine if some occupations exhibit a trend with respect to barium and antimony levels.
To date, barium and antimony determinations have been performed on paraffin lifts which were taken from the back of both right and left hands (usual thumb, thumbweb, index finger area) of persons engaged in various occupations: chemists, plumbers, electronic technicians, graphic artists, carpenters, mechanics, painters, electricians, chauffeurs, maintenance men, draftsmen, machinists, and computer operators.
The procedure employed in taking the handblank lifts was to go to the site where the person was working, in order to have a natural environment for the particular occupation. The lift for the handblank was taken in the manner previously described in the gunshot-residue determination procedure. Other information, such as whether the person is right or left handed, and if he smokes, was recorded at the time of taking the lift.
In a number of individuals of different occupations, there was observed on elevated Ba level, above that of "normal". In the instances where the Ba levels were elevated, however, the Sb levels were normal. In instances where the Sb level is elevated, the highest value is not as high as the lowest range of a single firing of a .38 Special revolver.
A thorough statistical analysis is premature due to the limited number of individuals tested in each occupation to date. The study in progress will continue until sufficient data is available upon which to base more meaningful conclusions. The results of this study will be reported upon at a later date.
A PROPOSAL FOB INCREASED COOPERATIVE RESEARCH IN FORENSIC ACTIVATION ANALYSIS
Vincent P. Guinn, General Atomic Division, General Dynamics Corporation, San Diego
In the course of the continuing study of forensic activation analysis at General Atomic, it has become increasingly clear that closer cooperation and coordination with members of the California Association of Criminalists would be of real benefit to everyone concerned. Many CAC members have, from time to time, ideas on studies that might be fruitfully investigated by NAA techniques - but they do not have the equipment, experience with nuclear techniques, time, or funds necessary to try these ideas out. At General Atomic, we have the requisite equipment, experience, and staff; we have a strong desire to develop the potentially useful forensic applications of the activation analysis technique, and, under our continuing U.S. AEC and U.S. Department of Justice research contract, we have the necessary funds.
We wish to propose a sharply increased participation in this research program by members of the CAC - both individually and as an official activity of the CAC. All suggestions of studies received will be first evaluated as to feasibility. If promising, at least an exploratory study will be carried out. There will be no charge to the law enforcement agencies or individuals. If it is feasible, and the person desires to, he will be welcome to participate in the experimental work, at the GA laboratories thus learning something about the method first-hand, and having the pleasure of personally participating in the work. If the study leads to publishable results, the person suggesting the study will be listed as the senior co-author of the paper. This proposal, of course, is limited to research and development studies it does not apply to actual case samples (other than samples from closed cases that might be appropriate samples for study). In some instances, where apropos, we are prepared to include electron microprobe, electron microscope, atomic absorption, emission spectrograph, and/or x-ray fluorescence measurements in addition to activation analysis measurements.
NATIONAL RESEARCH INSTITUTE OF POLICE SCIENCE
A film was introduced by Dr. Guinn describing the operations of the Japanese National Research Institute of Police Science. The Institute is organized into eight sections as follows:
- Legal medicine
- Chemical section (toxicology)
- Activation analysis
- Physics section
- Fire section (explosives, arson)
- Machine section (firearms, traffic accidents)
- Documents section
- Psychological section (polygraph)
The function and the operations of the various sections were described in the film.
INQUIRY INTO STANDARDS OF PRACTICE OF BLOOD ALCOHOL ANALYSIS
Lowell W. Bradford, Bryan S. Finkle, Alfred A. Biasotti, Don M. Harding, William C. Smith, Santa Clara County District Attorney's Office
A discussion of conclusions derived from samples of blood containing alcohol circulated to laboratories on this continent, Europe and Australia. These samples have been analyzed by various analysts as blind tests and the results have been studied with regard to standards of practice.
|Group A: Those laboratories doing traffic blood alcohols with a volume of over 200 per year.|
Group B: Those laboratories with a volume under 200 per year.
|Jan '67 Sample
||Range of values
||Std. Dev. as % of Mean
|Group A less GLC
|GLC Section of Group A||.247||.038||.0083||3.3||.014||.024
- Cadman comment: The GLC values are scattered, possibly due to the fact that as seen by GLC, alcohol added to blood is not exactly the same as Ingested alcohol. Evidence of this is seen when compared directly with Kozelka-Hine analysis. The difference may be of the order of 0.02.
- Kirk comment: A number of laboratories using GLC do not use internal standards in their analyses.
IDENTIFICATION AND COMPARISON OF PAINT BY X-RAY DIFFRACTION AND SPECTROGRAPHY
Charles R. Fontan and John F. Williams, San Francisco Police Department
A search of the literature failed to reveal any XRD data on paint pigments and their corresponding trace metallic components. The work undertaken by the authors attempts to correct this omission and is directed toward use in the criminalistics laboratory. Samples were not purified, recrystallized, or ground, as the raw material is that which is encountered in paint and as such is of interest to the criminalist.
Information was presented relating to the chemical composition of a number of paint pigments as determined from information supplied from the manufacturers, XRD and emission spectroscopy. A summary of the data collected was presented in an extensive handout, additional copies of which may be obtained from the authors.
A GLASS DENSITY METHOD UTILIZING MARKER DYES AND STAINS
John E. Davis, Oakland Police Department
A procedure wag described for the preparation of density columns for comparison of glass fragments. The Improvements over previously described methods Include (1) Dye-staining the various layers within the tube as a means of detecting accuracy of layering and degree of diffusion, and (2) Dye-staining glass particles to be compared as a means of conveniently locating them within the tube.
Crystal Violet is used to color the various layers of Bromoform and Bromobenzene. When the gradient is made up using the colored layers, mixing of the layers may be detected by the difference in the color of the layers.
Particles of glass may be identified by staining the fragments with a solution of eosin in methanol. The particles are air dried before being placed in the gradient tube. Other particles may be dyed with Indigo Carmine. In time, both Eosin and Indigo Carmine will dissolve off the particles, though the latter is slower to dissolve. By the time the stains do dissolve, the positions of the fragments will have become more or less fixed, and observation of specific fragments is facilitated. The stains do not significantly alter the density of the particles.
Cooper comment: A quick and convenient demonstration of the density gradient method may be accomplished by making a solution of saturated aqueous NaCl, adding a blue dye to half and a red dye to the other half. With mixing, a third layer (violet) is obtained. Pieces of waxes and resins are added to demonstrate the difference in density of these materials.
FORMULAS FOR DENATURED ALCOHOL - A REVIEW
Herman J. Meuron, U.S. Treasury A&TT Laboratory, San Francisco
The Federal Government closely regulates the production of alcohol and authorizes a number of materials to be added to alcohol to prevent human consumption of untaxed alcohol. In various concentrations, either alone or in conjunction with another agent, the following materials may be encountered in denatured alcohols:
|Acetaldol||Methyl isobutyl ketone|
|Acetone||Methyl propyl ketone|
|Almond oil||Methyl salicylate|
|Ammonia water||Methyl violet|
|Animal oil||Methylene blue|
|Arnica flowers extract ||Mustard oil|
|Bergamot oil||Phenyl mercuric salts|
|Cassia oil||Pyridine bases|
|Cedar leaf oil||Pyronate|
|Cloves oil||Salicylic acid|
|Ethyl ether||Sodium iodide|
|Lavender oil||Wood alcohol|
SIMULTANEOUS BLOOD, BREATH, AND URINE ALCOHOL CORRELATION DATA
James M. White, San Bernardino County Sheriff's Department
A description was presented of a study conducted over the 1966 Labor Day weekend in which simultaneous blood, urine, DPC, Intoximeter, and Muni-Quip Breath Tester samples were obtained from subjects arrested for 23102a and 647f. An extensive handout was distributed containing a summary of the data collected. Additional copies of this data may be obtained from the author.
- Bradford comment: Errors may be expected to be larger with the DPC since only 1/10cc of blood is used. Bradford will report later on the GLC analysis of the vapor over DPC.
A 1 ml sample of headspace over the urine is analyzed by GC on a 3.8% Hallcomid-0.5% Carbowax on 35 mesh Teflon 6 column at 140° with 63 ccs N₂/min. The retention time of toluene is approximately 4 minutes.
- Kirk comment: The apparent lack of uniformity in the ampoules may be due to irregularity in the glass.
- Turney comment: A still later shipment of the Stephenson ampoules checked out satisfactorily. The problem with the one batch may have been a lack of care in filling.
- Biasotti comment: Santa Clara Co. Laboratory of Criminalistics has been successful in the identification of toluene in headspace over blood in cases involving glue sniffing.
- Briglia comment: The Hine Laboratories has been successful in the identification of toluene by having the subject breathe into a plastic bag, which is later sampled for GC analysis.
BREATHALYZER EXPERIENCES UNDER OPERATION CONDITIONS RECOMMENDED BY THE CAC
William C. Smith, Don M. Harding, Alfred A. Biasotti, Bryan S. Finkle, and Lowell V. Bradford, Santa Clara County Laboratory of Criminalistics
A summary was given of operator disciplines, supervising techniques, and results of breath alcohol analyses in the Drinking Driver Enforcement Program of Santa Clara County since October 6, 1966. Points discussed included operator ability to analyze blind reference standards, variation in consecutive duplicate breath tests, and correlation between duplicate breath tests and blood tests on the same arrestee at the same time.
THE STRUCTURE AND OPERATION OF THE NEW YORK STATE IDENTIFICATION AND INTELLIGENCE SYSTEM
Charles C. Kingston, NYSIIS, Albany, New York
The New York State Identification and Intelligence System is divided into two major sections, the Administration and Field Services Section, and the Systems Development and Operations Section. The latter section is divided into the following:
- Criminalistics research
- Planning and research
- Bureau of Identification
- Data conversion
- Bureau of Design and Operations
At the present, a rationale is being developed to justify the expenditure of funds for further criminalistics research. Some resistance has been encountered due to the application of a "cost-effectiveness" policy, with material benefits foreseen within a specified period of time.
A computerized automatic fingerprint scanning system may be in operation in 5 years if the necessary resources are put into it. In the earliest stages, it will not be susceptive to single latents.
CRIMINALISTICS EXAMINATION OF PORNOGRAPHIC STILL AND MOVIE PICTURES
J. Robert Davidson, San Bernardino County Sheriff's Department
A recent case was outlined involving the identification of photographic equipment used by a defendant in the production of pornographic pictures. In this particular case, most of the original negative material was not recovered; most of the seized material being positive transparency copies of full film size of the original negatives and both positive and negative copies of movie films.
Specific considerations discussed and Illustrated in the presentation were:
- The type of camera used to produce a particular negative may be determined from the class characteristics of the negative (Film size, general format and/or orientation, exact measurements of the frame size and, in some instances peculiarities of the framing of a particular manufacturer camera back.)
- Specific identification of the camera used to produce a particular negative can be determined by comparison of individualizing imperfections on the frame edge (including roll film backs, sheet film holders, film packs and adapters and movie cameras.)
- Similarly, contact printers and enlarging easels can be identified by comparison of the framing edges.
- Photocopies of pictures may be identified to a particular original picture by comparison on the imperfections in the cut edges of the picture to the photocopy of the edges as well as by other individualizing characteristics on the original picture resulting from mistreatment.
- Movie film copiers of the 16-8, enlarging-reducing type may be identifiable to a particular film copy. Quick elimination of a particular copier is not possible inasmuch as debris accumulates around the framing rather rapidly during the copying procedure and may obscure the true individual characteristics.
- Film splicers may be identified by the cut edges and by the marks made by the emulsion scraper.
- Processing equipment could possibly be identified by scratch marks it produces on processed film; however, the very large processor in this particular investigation was not seized.
COLLECTION AND CLASSIFICATION OF HANDWRITING EXEMPLARS ON A ROUTINE BASIS
Anthony Longhetti, San Bernardino County Sheriff's Department
A keysort card procedure for the collection and classification of handwriting exemplars was described. The exemplars are collected as part of the normal booking procedure from all prisoners booked in San Bernardino County. The cards are filed by offense classification and punched by date-of-birth for general retrieval purposes. Handwriting, handprinting, and check form characteristics are punched for potential "general unknown" searches.
- Thornton comment: Strictly speaking, a handwriting exemplar form is not a public record as there is no legal requirement for their maintenance. As they are not a public record, the "same name-same person" presumption no longer exists under the new evidence code. To be admissible in court the sheet must be witnessed or a thumbprint Included.
THE LABORATORY IDENTIFICATION OF LSD
Donald W. Hessel, Bio Laboratories, Colton
A short history of Lysergic Acid Diethylamide was presented, with a discussion of commonly encountered forms on the illicit market. For purposes of screening for LSD, the author suggests the use of UV spectrophotometry and/or a color test with p-Di-methylaminobenzaldehyde. For purposes of purification, the following scheme is proposed:
0.1 N HCl; CHCl₃
TLC CHCl₃; MeOH (9:1)
Further analysis of the purified material may be accomplished by UV spectrophotometric and spectrophotofluorometric analysis. Several different solvent systems have been found suitable for TLC, including Methanol; Acetone; CHCl₃ (4:1), Benzene: Methanol (4:1), and CHCl₃: Methanol (9:1). A standard of 0.4 micrograms of LSD is run simultaneously. 0.2 micrograms may be detected with the p-dimethylaminobenzaldehyde reagent. Further identification of the material may be accomplished by IR spectrophotometry.
QUANTITATIVE AND QUALITATIVE ANALYSIS OF LSD
Robert J. Martin, Food and Drug Administration, Los Angeles
A short sketch was given of the functions and operations Of the Federal Bureau of Drug Abuse Control. An outline was given of the approach of the FDA laboratories to the analysis of LSD and other hallucinogenics. The presumptive test for screening is a color test with p-dimethylaminobenzaldehyde. Chromatography of the crude material on a Celite column separates LSD and Iso-LSD. Rf values for LSD and Iso LSD in a number of solvent systems was given for Thin Layer Chromatographic identification of these materials. The specific details of the analysis are given in a handout, which is available upon request from the author.
Dimethyltryptamine may be identified most easily by Its IR spectrum in carbon disulfide. Psilocybin has a very characteristic UV spectrum, and may be further identified by TLC and IR spectrophotometry.
IR spectrophotometry is not applied to the identification of LSD unless it is reasonably certain that at least 90 micrograms is available. This is principally because a chloroform blank shows an IR spectrum which may be in part confused with that of LSD.
- Brackett comment: Spectro-grade solvents are often quite impure when large volumes are evaporated. Brackett has observed 15 different compounds in anhydrous ether.
- Martin comment: FDA laboratory uses Burdick and Jackson chloroform, re-distilled from glass.
THE CONNECTING LINK
David Q. Burd, CII, Sacramento
A 16 mm color film was presented which was produced by CII and the CHP and which is available on loan from CII. The title of the film is "The Connecting Link," and deals with physical evidence in general and specifically with the types of physical evidence that may be encountered in hit-run cases.
RECENT DEVELOPMENTS IN CRIMINALISTICS OH THE NATIONAL SCENE
Paul L. Kirk, University of California, Berkeley
The scant but hopeful notice given criminalistics in the report of the President's Crime Commission, combined with increased interest of the Office of Law Enforcement Assistance and of the Congress of the U.S. in consideration of H.R. 5652 which would establish an Institute of Criminal Justice with granting function raises hope of the establishment of significant research facilities supported by federal funds. NYSIIS in New York is already authorized to establish a criminalistics research organization in the state of New York, possibly with federal aid.
To date, none of the effects of this renewed Interest has been felt in California. This is true in spite of the fact that California has been the leader among the states in its criminalistics developments. That leadership is severely threatened, and it appears appropriate for the CAC to give consideration to this fact and its possible consequences.
New York State especially is vying for the leadership at present, as evidenced by its attempt to establish at least two criminalistics training programs in Universities; recent establishment of a group similar to the CAC; and of course, its authorized entry into financed criminalistics research. Some Informed persons now state that Hew York will be greatly ahead of California within about five years. The question as to whether or not this will be accepted as a challenge to the California criminalists is moot. Healthy competition is considered to be welcome.
DETERMINATION OF MORPHINE IN BLOOD
Edward R. Thompson and Jack Villaudy, Los Angeles County Coroner's Office
A method was described for the determination of free morphine in blood in death cases. 250 mLs of blood is made basic with NaHCO₃ and NH₄OH and extracted with Ether: Acetonitrile (2:1). After further solvent extractions, the residue from the basic and amphoteric fractions is spotted on paper and developed with the upper layer of an n-butanol, water, formic acid (100, 40, 1) system. Further tests of a confirmatory nature may be accomplished by means of a crystal test with cadmium iodide, and by UV quantitation. Specific details of the analysis may be found in a handout, which is available upon request from the authors.
DRUG INVOLVEMENT IN DRINKING DRIVING CASES
Bryan S. Finkle, Alfred A. Biasotti, and Lowell W. Bradford
A summary of the drug aspects of 3409 cases of routine drinking driver investigation cases from the 1966 period In Santa Clara County was presented.
683 different drugs were indicated by statements of the subject upon questioning or by police investigation. Of these cases, 19.3% involved the use of ataractics and ataxics, 7.5% involved the use of sedatives and hypnotics, and 3.8% involved the use of analgesic narcotics.
In the segment of these cases in which BA concentration was less than 0.15%, twenty-one percent of the cases were found to have significant amounts of drugs in the blood or urine sample submitted for blood alcohol analysis.
An extensive handout was distributed summarizing the data from this investigation.
TOPICS IN CRIMINALISTICS
Charles M. Wilson, Wisconsin State Crime Laboratory, Madison, Wisconsin
A selected gunshot injury was discussed and a slide of a human skull was shown to illustrate certain considerations in the case. The direction of the shot through the skull was established through a determination of the entry and exit holes. The entry hole was that in which hair from the scalp was carried into the wound. The exit hole was greatly enlarged and tumbling of the projectile was evident. From a consideration of the shape of the entry hole, also elongated, it was concluded that the projectile was tumbling at the Instant of Impact.
A slide was shown of an X-Ray profile of a bullet in a body, illustrating the caliber of the projectile and other discernable class characteristics of the projectile.
Slides were shown of the Wisconsin State Crime Laboratory Mobile Field Unit and Its equipment, and a summary was given of the functions and operations of the unit.
A color slide was presented illustrating a five-layer paint match.