SEMI-ANNUAL SEMINAR (Fall 1960)
CALIFORNIA ASSOCIATION OF CRIMINALISTS
November 4-5, 1960
LAMP FILAMENT EXAMINATIONS IN TRAFFIC ACCIDENT INVESTIGATION
Discussed appearance of lamps and filaments broken when hot or cold or under other conditions and illustrated
various experimental tests made with color slides. No abstract furnished.
THE STATISTICAL STUDY OF HEEL MARKS
Reported a statistical study of the frequency of matching accidental marks on heel prints with respect to spatial
relationship. Study made with Dillon, Parker, and Kirk. Matching marks were expressed in terms of percentage of
matching coordinates per comparison. The results ranged from 0-44% for comparison of prints from same heels. The
study demonstrated that taking just one feature of an accidental characteristic (approximate location of mark)
there is a wide difference in the comparison of marks made by different heels and marks made by the same heel.
PYROLYSIS IN USE OF GAS CHROMATOGRAPH
Don Nelson and Paul Kirk
Reported on study of pyrolysis of barbiturates by means of the
Chromatograph. A few tenths of a mg of barbiturate is pyrolyzed by electrically heating the platinum cup
supporting the sample in the stream of argon. Results are reproducible. No salts give more characteristic peaks on
chart than the iron acids. It appears, from work in progress, that a mixture of an alkali and a free barbiturate
acid will give substantially the same products as the corresponding in salt. Twelve barbiturates so far examined
are readily distinguishable by this method.
A SURVEY OF THE PRESUMPTIVE TESTS FOR BLOOD
Duayne Dillon and Arlen Jee
Conducted benzidine, luminal, phenolphthalein and leuco-malachite green tests on all substances previously reported
in the literature as giving false positive tests. The phenolphthalein test appeared to be most specific, failing to
give false positive reactions in the majority of instances when such reaction encountered in one or more of the
other three tests. Complete paper should be studied by all interested persons. If copy not obtained at Seminar,
DIFFERENTIATION OF BARBITURATES BY CRYSTAL TESTS
Described development of a crystal test reagent and procedure for distinguishing various barbiturates. Scheme
involved "salting out" of drug (from KOH with phosphoric acid; from conc. H₂SO₄ with water;
etc.) plus use of Wagenaar's reagent (5% CuSO₄ soln. with ethylenediamine added) and the final use of a
reagent devised by Davis. The latter was a 10% aqueous solution of AgNO₃ to which ethylenediamine is
added (15% by volume). Silver reagent described was capable of giving characteristic crystals with about 17 of 19
barbiturates tested. In application, reagent utilized (with some exceptions) by adding a fair quantity of
powdered drug to a drop of liquid reagent. Crystals may form quickly or may require as much as 45 minutes.
Cover glass may be used with some tests but are found to alter the form in other cases. Stronger or weaker
silver solutions will affect ability to obtain crystals and their form as well. Technique is important.
Reaction crystals obtained illustrated with slides.
A STUDY OF ION EXCHANGE SEPARATION OF POISONS FROM LIVER TISSUES
Kenneth Parker and Paul Kirk
Results of study presented. An aqueous ammonium sulfate extraction method described as well as an organic method
utilizing a defatting procedure. Isolation by ion exchange showed possibilities but the conditions of exchange and
elution gave results which do not warrant the time and labor for general use.
THE IDENTIFICATION OF SALIVA
Don Nelson and Paul Kirk
The most characteristic constituent of saliva appears to be amylase which may be demonstrated by hydrolysis of
starch. Salivary amylase may be distinguished from amylases in takadiastase and malt by their activities in buffers
of different pH. Mention also made of thiocyanate, nitrite and phosphatase tests.
GAS CHROMATOGRAPHIC SEPARATION OF ALKALOIDS
Kenneth Parker and Paul Kirk
Reported the separation of steroids and alkaloids using 2-3% SE-30 (General Electric methyl silicone polymer) in
Chromosorb W as the column packing. An argon ionization detector system and temperature of 210°C was employed
to separate 45 alkaloids giving single peaks and elusion times from 2 to 90 minutes. Separation of alkaloids as free
bases under various conditions of temperature, gas flow rate and % stationary phase have been accomplished. Samples
were introduced as solid free bases and as chloroform solutions. Salts of the alkaloids appeared less
satisfactory. Separation of steroids and alkaloids, using SE-30, suggest the possibility of application to other
compounds. Preliminary experiments indicate separations of various barbiturates as free acids. (References: J.
Am. Chem. Soc: 7-20-60 and Chem. & Eng. News 7-25-60).
REPLICA FIREARMS EVIDENCE
Described the development of a procedure for making metallic-looking bullet replicas suitable for use in
microscopic comparison. A mold of specimen made in RC 900 silicone rubber after which it is internally coated with
fine lining of aluminum powder applied with a cotton swab (no brushes). (Davis now using "Gloria Aluminum Bronze"
powder produced by Baer Brothers, N.Y.). Cast made of 100 g rosin, 80 g parawax and 105 g carnauba wax. Pouring
melted mixture into aluminum powder coated silicone mold results in a cast faithfully reproducing even finest
striae on bullets. When used for bullet or tool mark comparison, such casts have metallic appearance of original
markings on lead or other metal. Davis suggested use of method to produce casts of evidence bullets for
distribution to other agencies. Photomicrographs of comparisons made between bullets and casts showed
identification detail as well as between two bullets. Complete paper to be published in J. Crim. Law & Crim.
IDENTIFICATION OF H FACTOR IN DRIED BLOOD
Fred Silva and Paul Kirk
Data presented that demonstrates that plant lectins for blood group factors H, O, A1, A2, and N may be used in such
a manner as to provide complete specificity. Only that for A1 is inherently specific to a degree that it need not be
calibrated for time of reaction with cells from corresponding and different blood groups. As earlier found true of
lectins for H, O, A1 and A2, the H lectin is readily applied to adsorption grouping of dry blood. When used in
conjunction with satisfactory anti-M serum, it is readily possible to determine group of either fresh or dry blood
in the MN system, as indicated by the study of 100 randomly selected blood samples.
ULTRAVIOLET ADSORPTION SPECTRA OF PHYSIOLOGICAL FLUIDS
Donald Nelson and Paul Kirk
UV absorption curves of perspiration, saliva, seminal fluid and urine studied to ascertain whether curves could be
used as an aid in identification. The effects of dilution, pH change and drying were investigated. Method appears to
be potentially useful as an aid in identifying urine stains and distinguishing urine from perspiration stains.
LABORATORIES OF EUROPE
Presented a short review of his observations made last summer in the laboratories of Scotland Yard in London and
the French Sûreté in Paris.
NATIONAL SAFETY COUNCIL COMMITTEE ON ALCOHOL AND DRUGS
Lowell Bradford, who is a member of this committee, presented information obtained at the last committee meeting.
On October 20, 1960, they recommended that the prima facie limit for driving under the influence of alcohol be
dropped from 0.155% to 0.10%. The Committee is also studying the feasibility of establishing some type of national
certification committee for alcohol analysts. Bradford also requests that any persons having data on cases
involving drivers, dead victims, etc. under the influence of drugs and/or alcohol forward the same to him.
Include number of cases, whether or not tests made for alcohol or drugs, test results, and all other pertinent
THE CHEMICAL IDENTIFICATION OF MARIJUANA
Charles Kingston and Paul Kirk
Aromatic aldehydes show color reactions with hemp resin when acidified with HCl. Similar color reactions produced
when resorcinol derivatives are used. This suggests the mechanism of the Duquenois test to be similar to the
aldehyde-phenol condensation reaction. Work is being done to confirm this. Hemp resin has been separated into two
fractions, each giving a different color sequence with the Duquenois reagent. Variations in reactions to the
reagent may be due to different proportions of components present.
DETERMINATION OF DRUGS IN URINE
The method of Mannering et al. was used for the determination of drugs in urine after a survey of a number of
methods. It consists of a hydrolysis end extraction procedure together with a paper chromatographic stage for
additional separation, purification, and preliminary identification. Excellent results were obtained in the
detection of narcotics. Sensitivity is high. Specificity is achieved by the large number of criteria inherent in
the method, i.e. the fraction Rf and color with the spray reagent are reliable clues to identification while
still permitting recovery of the drug for confirmation by UV, crystal, color, or other test methods. Other drugs
detected and identified in sub-lethal or lethal quantities are quinine, codeine, morphine, aminopyrine,
chlorpronazine, nicotine, strychnine and carbon.
Improvements have been made in the development-solvent system increasing the speed and reproducibility of the Rf
values. A solvent mixture of the same composition as the equilibrium mixture of the Mannering solvent system is
prepared for immediate use. The composition of the new system is available to those interested.
Disadvantages encountered are recovery of metabolites that survive the hydrolysis, thus with codeine ingestion
both codeine and morphine are recovered and identified.
A MATTER OF FACT and THE SILENT WITNESS
Films produced by the William S. Merrill Company and the American Medical Association. “A Matter of Fact -
Post Mortem Examinations” and “The Silent Witness - Breath Tests in Drunk Driving Cases” were shown.