California Association of Criminalists
Since 1954
THE ISOLATION OF SPERMATOZOA FROM DRIED SEMINAL STAINS
W. Jack Cadman, Orange County Sheriff's Office
Report on initial work indicates millipore filter paper may be of value in recovery of spermatozoa, particularly in more difficult cases.
Background material of stain is digested in Schweitzer reagent in 3 cc centrifuge tube. Sediment is washed in concentrated base, stained with Giemsa stain, recentrifuged. The resuspended sediment is then filtered through the screen only of a Swinney Adapter ($5.00), and then through Millipore filter paper (Millipore Filter Paper Corp., Bedford, Mass.; 0.3μm pore size, 13 mm diameter, $22/100). The filter paper is then dried with IR or hot air. Millipore paper is then placed on top of 2 drops of immersion oil on microscope slide. After oil filters through, 1 drop of oil is placed on top, and preparation is examined microscopically (preferably with dark field phase contrast microscope).
Also reported that ultrasonic vibrator has promise of dispersing background material without damage to spermatozoa.
USE OF DERIVATIVES IN THE CHROMATOGRAPHIC ANALYSIS OF NARCOTIC MIXTURES
James Brackett, San Mateo County Coroner's Office
Simple chromatography alone does not measure a unique property of a substance; but use of multiple detection and reaction properties after chromatography greatly improves identification, as does chromatography of derivatives. Reports semicarbazones can be formed directly on spotted chromatogram in μg quantities where usual procedures required up to 100 mg of material. Can also perform KMnO₄ degradation directly on paper and get multiple products (chemical degradation under better control than pyrolytic degradation). 10μl of NaOH hydrolyzes spotted heroin on paper in normal drying tiles. Other chemical derivatives of some drugs may increase sensitivity of detection.
Handout listing approximately 210 drugs and other compounds with Rf values and methods of detection.
CALIFORNIA HIGHWAY PATROL CONDUCTING SURVEY OF CO-INVOLVEMENT IN SINGLE CAR ACCIDENTS
Harry Johnson, State CII Laboratory
CHP has requested Coroner's Offices to submit to specified laboratories blood samples of drivers involved in one-car driver fatal accidents, who have died within 15 minutes of time of accident and in which no fire is involved. Purpose of the survey is to determine what effect, if any, carbon monoxide intoxication may play in fatal accidents. Blood to be checked for alcohol also.
GAS CHROMATOGRAPHIC DETERMINATION OF BLOOD CARBON MONOXIDE - PRELIMINARY REPORT
W. Jack Cadman, Orange County Sheriff's Office for Fred Wynbrandt, Orange County Coroner's Office
Cadman "leaked" procedure under study by Fred Wynbrandt for blood carbon monoxide, a development which should provide greater accuracy than spectrophotometric determinations; particularly for low saturations.
Gases released in 1 cc rubber-stoppered serum vials (à la Scholander) and 2 cc of gas drawn off end injected into GC-2 liquid port using a 4-foot molecular sieve 5A column at 40°C with thermal conductivity detector at 350 mV and 30 psi Helium as carrier.
Hope to have more on this from Wynbrandt in Concord!
GAS CHROMATOGRAPHIC DETERMINATION OF ETHANOL IN BLOOD: SEPARATION OF OTHER VOLATILES FROM BLOOD AND AQUEOUS
SOLUTIONS
Kenneth D. Parker, University of California, Berkeley
Summarized paper submitted to Analytical Chemistry, March 1962 by Parker, Charles H. Fontan, John L. Yee, and Paul L. Kirk.
A gas chromatographic method is described which, applicable to the medicolegal determination of the Ethanol content of blood and aqueous solutions, offers advantages of rapid analysis, improved accuracy, simplicity and specificity. Retention data for 56 volatiles indicate the resolution of the castor wax column used and illustrates its general utility for presumptive identification of volatile materials. Seven minutes were required to prepare and quantitate ethanol in a sample. Use of ethyl acetate as an internal standard obviated the necessity of precise measurement of blood samples. Standard blood and water samples with 0.023 and 0.180 percent alcohol were analyzed with a precision of 2% and an accuracy of about 4%.
Used "Hy Fi" (Wilkins Instrument and Research Co.) with hydrogen flame ionization detector and 0-1 mV recorder with disc integrator. Chromatographic column was 10 foot stainless steel 1/8" OD, 0.093" ID, packed with 60-80 mesh Chromosorb W, acid washed, coated with castor wax 40% by wt., and preconditioned at 190° for 8 hours.
Mimeographed handout gives details of procedures, equipment and experimental results.
AN IMPROVED GAS CHROMATOGRAPHIC COLUMN FOR BARBITURATES
Kenneth D. Parker, University of California, Berkeley
Reports on improvement of column previously reported [San Francisco Seminar and Anal. Cham.: 33, 1378 (1961)] in which an SE-30 5% column was used. New column (1.5% SE-30 and 2% Carbowax 20M coated on dried acid-washed firebrick, 100/200 mesh) achieved substantial improvement in peak symmetry. Sample charts of mixed barbiturates also showed generally good separations and sharp peaks.
Two-page mimeographed handout gave conditions and comparative data for old and new column.
SIMPLE MICRO SOLID SAMPLE INJECTOR
Kenneth Parker, University of California, Berkeley
An unscheduled informal presentation of micro solid sample injector made from 22 gauge and 26 gauge hypodermic needles and a 26 gauge stylus in which the stylus can be "loaded" with solution (or dried) of material. After being showed to dry it is withdrawn into 22 G needle, assembly inserted into injection port and stylus pushed out into gas stream in chamber for 6 seconds, and assembly withdrawn.
It was suggested that derivatives could be prepared directly on the stylus in micro quantities for injection and further identification.
VACUUM SWEEPINGS
C.M. Wilson, Wisconsin State Crime Laboratory
Described vacuum sweeper being used by WSCL in which preliminary separations are obtained with near elimination of the generally unusable fine dust through which the examiner must normally search to find hairs, fibers, chips and fragments. First used metal screens with .020, .063, and .093 pore size; but has shifted to perforated metal plates. Has advantages over filter paper of extreme increase of air flow. Collector illustrated appeared rather heavy to handle and time consuming to assemble. The increased vacuum, air flow, and initial separations certainly have merit.
Cadman suggests teflon-coated paper has low air flow resistance and is perhaps worthy of trial.
Kirk reports MISCO is, or will soon be, out with a smaller tube type collector using a filter paper sock that will be capable of getting into pockets and confined areas (glove compartments) more readily.
LOCKS
William Lee, Los Angeles Police Department
Lee presented a general summary of the 5 lock types, but the paper was not readily abstractable. The types discussed were: warded, wafer, pin tumbler, lever, and combination locks.
LOS ANGELES POLICE DEPARTMENT EXPERIENCE WITH BREATHALYZERS
Ray Pinker, Los Angeles Police Department
The Los Angeles Police Department has had 16 breathalyzers in full operation for about 4 months. With the exception of one mobile unit, all are in fixed locations at booking stations. When the 15 new instruments were received, the LAPD laboratory obtained widespread results with a 0.15% standard synthetic breath sample (0.12 - 0.17%), with some instruments fairly reproducible and others very poor. The irregular results were found to be due to a series of malfunctionings of the instruments: 1) piston sticking problems due to oil and metal turnings in the aluminum rubber bulb adapter, 2) bubbler tube movement when switching to "analyze" position, and 3) backlash in the instrument due to loose Teflon bearings. After cleaning out the grease and aluminum turnings, freezing loose bubbler tube to the chassis, and eliminating backlash with "Gunslick" (a thick graphite emulsion), all the instruments were found to reproduce results and could be properly standardized. Many correlation studies with the instruments show 2/3 of the breathalyzer results the same as, or within 0.01%, of the blood level; and the remaining 1/3, .01% to .03% lower than the blood level.
Several hundred police personnel have been trained by the laboratory staff to operate the instruments, and only such personnel certified as competent are allowed access to the instruments. In the 4 months of the full Breathalyzer program, the Laboratory has been called for expert testimony on1y 30 - 40 times for the 1500 or more tests performed. It has been estimated that Los Angeles City will save several thousand dollars this year over the cost of the Intoximeter program (including the cost of the 15 new instruments) to say nothing of the more reliable results and the saving of laboratory personnel time.
The department uses the Breathalyzers only as corroborative evidence of alcoholic influence, sometimes booking subjects as low as 0.03%.
The new model of the instrument is priced at $695 and test ampules at $0.70. Test ampules are good for a total readout of .60 - .69%, so duplicate tests can be run on subjects with .30% or less without changing ampules.
Pinker passed out individual copies of the LAPD Breathalyzer Training Manual.
As a side note, Pinker stated that Intoximeter correlation studies with blood showed 2/3 of Intoximeter readings to be within 0.02% of the blood, but the remaining 1/3 showing - 25% error. This is sufficient reason to drop Intoximeter test programs, even if they are used only for corroboration of physical impairment noted by an officer.
CLASS CHARACTERISTICS OF EUROPEAN TYPEWRITERS
David H. Crown, U.S. Post Office Department, San Francisco
Typewriter classification never was a certainty, due to Smith Corona's (and other manufacturers) placing any manufacturer's T.W. fonts on their machines on special request and private brand typewriters; i.e., Sears Roebuck TOWER T.W., manufactured by different companies on apparent short term contract basis.
In the late 1950's, typewriter imports greatly increased, and American companies started to manufacture in Europe. R.C. Allen reportedly imported European T.W. Fonts, and European manufacturers started adopting American T.W. pitch (.212 & .254).
Currently, most European T.W. manufacturers buy type fonts from a relatively few manufacturers, and this often appears to be haphazard buying. Rapidly changing type fonts on European T.W. and multiple trade names (European as well as American imports) on the same typewriter have made complete listing of classification groupings impractical, if not impossible. (Ed. Note: but increases individualization value of typeface match alone in some cases.)
Crown promises to mail out probably the most extensive type face classification ever compiled for distribution.
U.V. ABSORPTION CURVES OF SOME SYMPATHOMIMETIC AMINES AND RELATED COMPOUNDS
J. Robert Davidson, San Bernardino County Sheriff's Office
Many of the sympathomimetic amines have similar UV absorption curves in acid (0.2 N H₂SO₄); however, basic absorption curves (3 drops saturated NaOH added to 3 cc of 0.2 N H₂SO₄ solution in curvettes used for acid curve) may be useful in differentiation, particularly if curve shapes indicate relatively pure solutions.
18 drugs studied -- could not, of course, differentiate the d-, 1-, d1- amphetamines; the 1-, d-, & d1-ephedrines (ephedrine, pseudoephedrine, racephedrine), nor desoxysphedrine from Catron (L-Metbylphenethy Mazine) except by first basic minimum shape. Can readily differentiate amphetamines, desoxyaphedrine, ephedrines, phenylpropanolamine, mephenteramine (Wyamine), phenyl-t-butylamine, phenmetrazine, benzphetamine, hydroxyamphetamine (Paredrine), phenylephrine (Neosynephrine) and others.
Has extra mimeographed handouts of method, absorption peaks, absorptivity and differentiative data. Passed out photocopies of curves (1 set per laboratory) and will print reasonable number of additional copies if requested.
PROGRESS REPORT -- INDIVIDUALITY OF BLOOD
Paul L. Kirk, University of California, Berkeley
Recent studies have been in the area of immunoelectrophoretic patterns of human blood (precipitin tests on protein electrophoretic patterns obtained on cellulose acetate support). Has obtained up to 35 precipitin bands on a single blood serum specimen run. Running blood pairs simultaneously to guarantee identical conditions, has obtained consistent similarities when same blood compared. Of 29 comparisons of different bloods, only one pair was considered to give similar patterns.
First work was on fluid serum. Dried blood shows only a few less precipitin bands, so prospects are promising.
REPORTS ON AAFS METHODS COMMITTEE REPORT
Anthony Longhetti, San Bernardino County Sheriff's Office
The most startling portion of the past year's methods committee study was that 2 of 18 participating laboratories made mis-matches in the bullet comparison study (all labs had comparable material - Davis type of wax replicas from same mold). Several labs failed to "make" some matches. Twelve of the labs do not take photographs of matches for court use.
Ed. Note: Perhaps CAC should consider such studies also, not as a check on other laboratories' reliability, but on the reliability of your own work.
REPORT ON AAFS IMMUNOLOGY SECTION MEETING
Tom Wieland, Ventura County Sheriff's Office
All paternity blood typing should be done in at least duplicate, using different sera sources.
Some difficulties may arise from non-specific anti-sera (especially "ce" combination in supposed anti-c or anti-e.
MN false exclusions usually due to subgroups of N (Dr. Kirk suggests N-lectins more reliable than anti-N serums).
"MOBAT"
Ray Pinker, Los Angeles Police Department
Luckey Laboratories of San Bernardino have recently introduced "new" breath alcohol test kits. MOBAT I is a dichromate field screen test unit along the lines of the German ALCOTEST. The MOBAT I appears to be an improvement in that finer mesh dichromate is used along with splintered glass plugs at both ends and in middle (separating 0.15% level). MOBAT II appears to be a redesigned INTOXIMETER, perhaps more convenient to handle; but still maintaining the basic difficulties of breath tests utilizing carbon dioxide as a measure of the quantity of alveolar air in the breath sample.
Pinker performed two correlation determinations between BREATHALYZER and MOBAT during after hours of the seminar. It can be seen from the following chart that if these are representative, MOBAT II is no more reliable than Intoximeter determinations.
| BREATHALYZER | MOBAT I | MOBAT II | |
| Subject # 1 | 0.14% 0.145% |
0.15%* | 0.18% | Subject # 2 | 0.22% 0.22% |
0.18% | 0.26% |
TYPES OF FINISHES ON AMERICAN AUTOMOBILES
Duayne J. Dillon, Contra Costa County Sheriff's Office
Dillon passed out a limited number of copies of a letter dated 2/14/62 from Nason Products Division, W.P. Fuller & Company, San Francisco. The general information was:
| Manufacturer | Paint |
| Ford Motor Company Products | Synthetic Enamel |
| Chrysler Company Products | Synthetic Enamel |
| Studebaker Motor Company | Synthetic Enamel |
| American Motors (Nash) | Synthetic Enamel |
| All truck manufacturers | Synthetic Enamel |
| General Motors (Before 1956) | Nitrocellulose Lacquer |
| General Motors (during the years 1956,'57,&'58) some cars were painted with others with |
Nitrocellulose Lacquer Acrylic Lacquer |
| General Motors (1959 to present) | Acrylic Lacquer |
The above information is true for approximately the last ten to fifteen years.
GENERAL ATOMIC ACTIVATION ANALYSIS PROGRAM - SEMINAR AND TOUR OF FACILITIES OF G.A. DIVISION OF GENERAL
DYNAMICS, SAN DIEGO
Dr. V.P. Guinn
The third day of this CAC semi-annual seminar was held at the General Atomics Laboratories near San Diego. The G.A. staff discussed the theory, methods, and applications of neutron activation analysis and conducted a tour and demonstration of their facilities, including their two TRIGA reactors.
Basically, the principal method of analysis consists of creating radioactive isotopes of the elements present in a sample by bombardment within a high flux neutron field (TRIGA) and measuring disintegrations (Gamma Ray Spectrometry) of the radiated specimen. The disintegration rate (half life) and gamma ray energy (MeV) are characteristic for each element. This method has the advantage of being non-destructive, usually rapid, and has general sensitivities in the order of 1 to less than .001 μg. (sensitivity is dependent on total sample size examined and not on the per cent of element of interest).
A second method of analysis is by radiochemical separation, which must be resorted to in some cases due to elemental mixtures that are not readily separated or identified by gamma ray spectrometry. In this type of analysis, to the radiated specimen is added a known quantity of non-radioactive element of interest and separated by standard chemical methods. The recovered purified element is quantitated and from amount of activity present the quantity of original element in the sample can be calculated.
Applications of neutron activation analysis performed by General Atomic have included analyses of petroleum and organic solvent residues, alloys, trace elements in Silicon and Germanium semi-conductors, in plastics, agricultural products, and in biological and medical samples including toxicology.
Ray Pinker announced the Los Angeles Police Department and General Atomics were recently successful in obtaining an Atomic Energy Commission short term research grant for study of applications of activation analysis in the field of criminalistics and have high expectations of having the grant renewed in October. (This is the only grant in this field that has been approved at this time from three applications to AEC).
In discussing the possible applications in criminalistics, Dr. Guinn pointed out that it will be no panacea. However, activation analysis can do many things which are not otherwise possible. It can extend the range to smaller samples which can be adequately analyzed, it can detect smaller traces of most elements than other methods and it is non-destructive.
Some of the areas of possible applications in criminalistics are comparisons (and later cataloging commercial sources) of plastics, rubber, paint, hair, paper, ink, grease smears, petroleum residues, etc.
The current project of the Los Angeles Police Department is the recovery and identification of powder residues from firing weapons. Pinker and General Atomics have expressed the desire of obtaining from any of our members' materials and evidence in which activation analysis may be of assistance. Pinker requests that any interested criminalist communicate directly with him first so that the work and costs could be included under the research grant if it falls within the scope of the grant.
This is certainly a fine opportunity to get in on some possible major basic atomic research and help Pinker, and perhaps improve your position on a particular case.
Dr. Guinn and Ray Pinker have offered professional publicity to the California Association of Criminalists for our cooperation in supplying ideas and materials for their research grant. Let's earn it.
The Los Angeles newspapers covered our seminar meeting at General Atomics and gave good coverage. It was our understanding that wire service reporters were also present, so perhaps the California Association of Criminalists got national coverage for our seminar an well as making it in the San Diego and Los Angeles newspapers; even if somewhat sensationalized.
From the Herald Examiner, Sunday May 27, 1962, page B-l (2nd front page) "Crime Fighters Use Reactor to Riddle Alibis." Leading paragraph -- "Sherlock Holmes, Hawkshaw, and Dupin would have turned in their magnifying glasses if they'd had a chance to attend today's session of the California Association of Criminalists." See, also, general discussion in TIME, June 22, 1962, page 48.
I'm sure that such publicity for the CAC and expert witnesses should improve our professional standing and make the public more aware and appreciative of our jobs, abilities and testimony.
