20th SEMI-ANNUAL SEMINAR (Fall 1962)
October 26-27, 1962

David Q. Burd, CII California Department of Justice

A general information paper on the practical application of IR spectra for comparison purposes rather than specific chemical identification. Use of IR for comparison of paint, plastics, greases, waxes and other petroleum products. Pointed out that it is possible to identify automobile paint type by IR, regardless of color. It is of particular value in comparing organic dye paints where Spectrograph is useless.

Burd uses 0.1 mg (or more) of paint mixed with KBr in a hardened steel sample holder in a Wig-1-Bug. The pellet can be formed in a 1x5 mm slit in aluminum foil pressed between polished metal plates in a shop vise.

Reference material of value cited; Infrared Spectra of Plastics and Resins; R.E. Kagarise and L.A. Weinberger; NRL Report 4369, 1954; Dept. of Commerce #PB 111438; $1.50 - gives 92 IR curves, available from the Office of Technical Services of the United States Department of Commerce.

James Brackett, San Mateo County Coroner's Office

This paper reflects the continued research being done by Brackett in paper chromatographic identification of narcotics and drugs.

Used conventional 2-dlmensional chromatography, except the same solvent is used in both directions. After first development, non-destructive detection procedures (visible, UV reversible spray reaction such as iodoplatinate reversed by NH₃ fumes) are used. From the Rf on the first development, derivatives are made on the paper which will give the most information after the second development.

Examples of useful conversions:

  1. Morphine-treat with nitrous acid
  2. Procaine-brominate (excess bromine water)
  3. Heroin-hydrolyze at room temp. with 1N NaOH

Note: each original spot on first development can be converted locally to a different derivative.

Rodney R. Ruch, General Atomics

Gave review of general theory of activation analysis.

Problems in criminalistics investigated to date include: plastics, greases and tire rubber.

Also, preliminary report on firearms discharge residues. The elements detected, common to gunpowders, are barium, antimony, and copper. The main difficulty has been developing a method of removing the residues from the hand.

Reference available; General Atomics Publication GA 3491 to include tables listing ppm of elements detected in different samples and data and extraction procedure for firearms discharge problems. Write to General Atomics, Activation Analysis Group Participation, San Diego on official letterhead requesting being put on mailing list for publication GA 3491.

Panel Discussion

Laboratory administration was broken down to physical plant, personnel, security, technical operations, logistics (supplies), services (janitorial, etc.), training and research. Views expressed varied from some directors suggesting a detailed duties and methods manual, a general policy manual, to fear of having any printed laboratory administration or "standard" procedure manual as some "law enforcement personnel give too much respect to the printed word."

Subject deserves further discussion.

Albert Laudel, University of California

Published in Science, write Dr. Kirk for reprints.

This was a further progress report on what Dr. Kirk presented at the San Diego Seminar (Spring 1962). Reviewed the method of immunoelectrophoresis on cellulose acetate base and utilizing anti-β and anti-β globulin antisera. (Editor's note: Not to be confused with β and β antisera of ABO system.)

Useful in differentiating bloods of different individuals.

Charles R. Fontan, William C. Smith and Paul L. Kirk, University of California

Mimeographed handout on procedure.

Used "column" packed with 60- to 80- mesh Chromosorb W, acid-washed, coated with carbowax 20M 2% (w/w) with potassium hydroxide 10% (w/w).

Noted that with continued use of column absolute retention times for antihistamines became 14% shorter, but relative times remained almost constant.

Published - See Analytical Chemistry, Vol. 35, No. 4, p. 59 (1963) with improved method of preparing column which is more stable.

Edward C. Jennings, Jr., Wilkens Instrument and Research, Inc.

Illustrated typical chromatograms obtained with hydrogen flame ionization chromatographs of drugs, vulcanized rubber, silicone treated glass fibers, an organic stabilizer used in tire manufacture, hair spray residue on a single hair, and automobile paint using pyrolysis.

W. Jack Cadman, Orange County Sheriff's Office

Gas chromatography generally not sufficient for identification of a compound; but by its use when coupled with other instrumentation, identification can be made. Gas chromatography purification (with tentative identification), followed by infrared to specifically identify, has been used with success on barbiturates in Orange County laboratory.

Procedure given: Extract 5 cc blood 4 x 25 ml CHC1₃ evaporate on rotary evaporator, wash down with 2 x 1 ml CHC1₃ transfer to centrifuge tube and dry to near dryness with hair drier, add 20μl CHC1₃. One ml used to determine peak time, then rest injected and collect peak time sample only. Collected sample dried in a Boron Carbide mortar and allowed to crystallize. Grind with KBr and form 1 x 5 mm IR pellet.

Chromatography on 2 1/2 ft. 1/2% neopentoglycoladipate on Teflon T-6 + 2% SE-30 column in modified GC-2 for sample collection, 190°C.

Details of modification and procedure should be requested from Cadman.

Don Nelson, University of California

An earlier paper presented at the 1960 Fall Seminar in Berkeley and later published (Analytical Chemistry Vol. 34, No. 8, p. 899 [1962]) showed how pyrolysis and gas chromatography could be used for barbiturate identification, even though the pyrolytic products were not identified. This presentation by Nelson gave the identity of principal products detected and some of the mechanism of pyrolytic breakdown of the barbiturates.

The principal products formed are nitriles which include varying carbon numbers and carbon chain rearrangements of the barbituric acid #5 radicals, and also on most cases included HCN, acetone, H₂O, benzene and propene nitrile. Amines may also be formed; however, the column used was not very satisfactory for amines.

Lowell W. Bradford, Santa Clara County Laboratory of Criminalistics

Law Enforcement in general looks to the criminalist to lead the program. Many new labs may be started primarily for Drinking Driver Program, but must consider legislature, public, physiological impairment and enforcement as well as the chemical test to be used.

Bradford reviewed the historical background of chemical tests and interpretation since the National Safety Council work of 1938 which led to the establishment of the 0.15% level. (Original work incomplete and conflicting and high level set to assure defendant benefit of any doubt). Since the establishment of 0.15% as the level at which all persons under influence, continued study has been made so that the 1958 Indiana Symposium on Alcohol and Road Traffic recommendation of 0.10% level has now been adopted by the NSC, AMA, Uniform Vehicle Code, IACP, and others.

The often-used figures of "for every 0.05% there is 1 oz. of alcohol in the system (150 lb. individual)" is often misinterpreted to mean that for each 2 oz. of 100 proof liquor the alcohol level goes up 0.05%. Santa Clara studies on 35 subjects (wt. 125-220 lbs; avg., 180) given 10 oz. of 100 proof liquor drunk in 50-90 minutes showed B.A. levels of 0.11 -0.19% (avg. 0.14%) one hour after last drink.

Frequency curves on drinking driver arrests on 6,662 cases show a bell-shaped curve with a mean of approximately 0.22%. The high levels actually represent an intake of 20 oz. to a fifth of whiskey and are levels normally obtainable by alcoholics. Time studies show that weekends (10:00 P.M. - 1:00 A.M.) are the high days for drinking driver arrests.

Other factors pointed out by Bradford as being part of the Drinking Driver program are: Liquor is more available in California than any other state, there are 6,000,000 alcoholics in America, the alcoholic beverage industry is a very important segment of our economy. California does not have a prima facie law.

The legal aspects brought out were: about 20% now refuse blood drawn, implied consent law recommended by Uniform Vehicle Code, drawing blood is not a violation of the self-incrimination rule (this applies only to statements), blood can be taken even if subject unconscious and medical privilege does not apply in criminal cases.

Bradford pointed out that any B.A. program should be coordinated, and personnel in all phases (laboratory technologist, police officers, etc.) properly instructed. Santa Clara County has a training procedure manual available.


Dave Burd supplied the following as a supplement to Duayne Dillon's information given at the San Diego Seminar, Spring, 1962: