22nd SEMI-ANNUAL SEMINAR (Fall 1963)
CALIFORNIA ASSOCIATION OF CRIMINALISTS
October 25-26, 1963
SAN MATEO, CALIFORNIA
IDENTIFICATION OF MODERN EXPLOSIVES
J.I. Reilly, E.I. DuPont Co.
Stated that 1.35 billion pounds of commercial explosives were used in the United States in 1963; some bound to come to the attention of law enforcement. Listed and discussed types of explosives:
- Dynamite - over 100 manufacturers' grades of nine basic categories: (DuPont's names) Straight, Red Cross Extra, DuPont Extra, DuPont Gelatin, High Velocity Gelatin, Special Gelatin, Gelex, Scimograph, and Permissible. (Ammonium nitrate - fuel oil mixture, boosted with a small amount of dynamite. Is now being used extensively in place of straight dynamite.)
- Blasting agents - insensitive compounds without nitroglycerine; must be boosted
- composition Explosives - first developed by British; are basically RDX type material.
- Rubber-based explosives - sheets or extruded, olive drab or red in color.
- Safety fuse - black powder in column of textile material with water repellent substance; always leaves residue of fabric. Two types: 30 and 40 sec./foot burn rate.
- Blasting caps (true explosives) - two basic types: Non-Electric - a metal cap with train-type explosive material ignited by safety fuse. Electric - composed of a basic charge, a primer load and an ignition load with electrical ignition by l)heating of bridge wire, 2) spark, or 3) exploding bridge wire. All caps can be instantaneous or with a delay up to 15 seconds (pyrotechnic burning).
- Squibbs - identical appearance to Blasting Caps; a non-explosive charge but with a pressure flame charge (i.e., black powder).
- Shaped charges - either RDX, waxed RDX, or Composition Explosive.
- Mild detonation fuse (MDF) - metal tube (Pb, Cu or Al) with explosive core of 1 - 20 grains/foot PETH, RDX, Tacot. Detonating rate: 2300 ft./sec.
- Flexible linear shaped charge - similar to MDF, only shaped (chevron shape in cross-section) and loaded with 5, 20 or 150 grains/foot.
- Pyro cord - similar in appearance to MDF. Core of ignition mixture with a violent flame train.
- Explosive Release - basically a detonative cap designed to do work; e.g., break bolt.
- Hole Cutter - as on a fuel tank to dump load.
- M₄ and M₆ Assemblies
- Minidet Detonators - minaturized detonating cap (.090" x 1/2").
- "Davey Crockett" - mild detonating fuse assembly.
- Fuses and Detonating Fuses - The Ensign-Bickford Co., Sinsbury, Connecticut
- Blaster's Handbook - (request from the speaker) Explosives Dept., 2930 E. 44th Street, Los Angeles (LU 206464)
- Manual of Military Explosives - U.S. Govt. Printing Office, Army #TM 9-1910, Air Force #TD 11A-1-34* or through liaison with local military.
Suggested that DuPont Laboratories would give assistance in identification.
UNUSUAL FIREARMS IDENTIFICATION
L.L. Cheshire, Sacramento
Had a few general comments. No particularly new or technical information presented.
IDENTIFICATION OF THE OPIUM POPPY
John I. Thornton (Duayne J. Dillon, co-author). Contra Costa County Sheriff's Criminalistics Laboratory
From a legal standpoint "an opium poppy is any poppy capable of production of morphine or codeine" and is not limited to the botanical definition of Papaver somniferum.
The paper presented a botanical description of P. somniferum. "Poppy Seed" (Spice Island brand), widely available in grocery stores, is 80 - 90% fertile and will develop into plants producing morphine and codeine.
The authors studied the alkaloidal distribution in developing plants using a few milligrams of powdered material boiled in water for one hour and filtered. The filtrate was evaporated, the resulting residue taken up in 0.1 M HCl and analyzed by thin-layer chromatography using Silica Gel G with 10% CaSO₄ as a binder and a solvent system of Benzene:Dioxane:Ethanol:NH₄OH (50:40:5:5)
It was stressed that for reproducible and generally better results, the TLC plates should be dried 4 to 6 hours at 110° C and allowed to cool (presumably in a dessicator) before use. The atmosphere of the chamber should be saturated with solvent-impregnate filter paper on the sides of the chamber. Also stressed was the need to dry the developed TLC plates with this system (which includes NH₃ ) before spraying with iodoplatinate (decolorized by NH₃ ).
The TLC plates shown were excellent, with good separations and little or no tailing.
It was suggested that it might be of interest to study plant morphology and alkaloid production and distribution of seeds (common source) when grown in the many different climatic areas of California.
An excellently prepared and detailed mimeographed paper was distributed, one copy per laboratory. It included photocopies of graphs and poppy morphologies.
MORPHINE AND CODEINE IN BLOOD AND URINE BY GAS LIQUID CHROMATORGRAPHY.
K.D. Parker, Hine Laboratories, San Francisco
Parker reported experimental detection of 10 micrograms of morphine. He was able to detect morphine in 86% of subjects 36 hours after injection of 15 mg of morphine. Procedure required multiple extraction of 20ml of blood or urine. Expected to publish details.
IDENTIFICATION OF PHENOTIAZINES BY PYROLYSIS-GAS CHROMATOGRAPHY
Charles Fontan (co-authors: Naresh C. Jain and Dr. Paul L. Kirk), University of California
Equipment utilized included Hy-Fi Gas Chromatrograph (Wilkens Instrument & Research) with hydrogen flame ionization detector, Aerograph Model 600; Leeds and Northrup Speedomax H recorder, Model S; Jennings and Dimick (Wilkens Unit) pyrolysis unit [An. Chem.: 34, 1943 (1962)]; and 5’ x 1/8” o.d. (.093” i.d.) stainless steel column packed with 60-80 mesh Chromosorb W, acid washed, coated with Silicone Oil No. 500 (5% by weight) and preconditioned at 110 degrees C plus/minus 1 degree C; flow rate of carrier gas (Nitrogen) 33ml/min.; flow rate of hydrogen 22 ml/min.; inlet pressure 20 p.s.i.; attenuation xl (recorder 0-1 mv).
Procedure: 15 mg of sample (as HCl) dissolved in 1 ml 2% H₃PO₄ (or when necessary, in 2% methanol solution of H3 P O4 ) or as free base dissolved in 2% H₃PO₄ 2% HC1.
Use vials covered with aluminum foil to protect from light. Five .01 of solution (75 mg of sample) dried on platinum coil of Wilkens pyrolysis unit with a 2 amp. Current. After placing unit in g.c. chamber and allowing 3 minutes for equilibration, the sample was pyrolyzed at red heat for 10 seconds.
The 19 phenothiazines pyrolyzed gave peak patterns by which they could be distinguished. Three major pyrolysis products from chlorpromazine and promethazine were tentatively identified as methene, ethene and propene.
BLOODSTAIN TYPING TECHNIQUE
Charles Morton, P.L. Kirk and Associates
Presented the following micro bloodstain typing technique requiring a speck of blood approximately 0.4 mm square in depression of silconed depression slide. This is a modified Nickolls and Pereira procedure (Medicine, Science and the Law: 2, 3, p 172, 1962:
- Add two drops 95% ethanol and allow to evaporate at ambient or slightly elevated temperature
- Add one drop of the appropriate anti-serum
- Place depression slide in moist chamber in oven at 50°-55° C for 20 minutes
- Remove from moist chamber and wash with three drops of cold saline; the first drop being added to the anti-serum, removed, and followed by two washes of one drop each. This washing is most expeditiously carried out with a fine-tipped capillary tube (hard glass) attached to a vacuum line
- Add one drop of a 0.5% cell suspension of the appropriate cells in Bovine Albumin in physiological saline to the bloodstain fragment and rotate the slide for 1-2 minutes; and
- Add two drops of cold saline to the cell suspension and rotate the slide until the cells are evenly dispersed or the speck is in an area of low cell concentration (removal of a portion of the original cell suspension prior to addition of the cold saline aids in reading the results by providing a cleaner background).
Of the 30 samples, all but two gave clear-cut correct results. (The two were typed as O whereas the recorded true types were AB). Some doubt was expressed as to the correctness of the true blood type of these two AB's.
A MODIFIED NINHYDRIN PROCESS
David A. Grown, U.S. Postal Department, Postal Inspection Service, San Francisco
Considering that both latent fingerprints and the ink lines on a document many may be important, it was desirable to develop a ninhydrin process that would not cause the inks to run, as is the case when using ninhydrin in polar solvents (e.g., acetone). Of all the combinations tried. Crown reported the following as the most effective and easiest to mix:
- Dissolve 7.5 gm ninhydrin in 40 cc methanol.
- When completely dissolved, add 960 cc petroleum ether (B.P. 30-60° C) and stir for several minutes.
- Allow to stand in separatory funnel 5-10 minutes and then discard the deep yellow aqueous liquid at the bottom.
The pale petroleum ether solution will not cause inks to run. This solution is not stable, and Crown recommends using freshly mixed solutions, or a maximum storage of one week.
A mimeographed handout also included other related information.
PROGRESS REPORT ON NEUTRON ACTIVATION ANALYSIS OF FIREARMS DISCHARGE RESIDUE
Dr. V. P. Guinn, General Atomic Division, General Dynamics Corp., San Diego
Method previously reported does satisfactorily detect Barium and Antimony, common in all American-made primers.
Residue is removed by normal washing.
Also reported on work by others in the field of Activation Analysis applied to Criminalistics problems, including:
- Jervis - Hair Study - Nine elements detected, each in wide ranges. Four hundred individuals studied. Arsenic was the only element showing significant variation along the length of the hair. Presence or absence and quantity of elements were apparently independent. Even with an analytical accuracy of 10% the elements and concentrations were of great significance in identification.
- Jervis - Glass - 15 automobile glasses examined. A total of seven trace elements were found.
A NEW AID IN BREATH-ALCOHOL TESTING
Dr. Glenn C. Forrester, The Intoximeter Association
Conceded that CO₂-ratio "loophole" needed plugging.
New instrument development has a double piston in cylinder to collect two samples of breath (210 cc = 1/10 cc blood) virtually simultaneously. One sample is used for passing through dichromate tube, the other sample passed through a 2-section perchlorate tube (the first section collects all the alcohol, the second is used as a control). Operation temperature of instrument is 103° F. The instrument has a waste bag to bypass the mixed expired air so that only alveolar air is captured in the cylinders.
Dr. Forrester presented his opinions on blood alcohol interpretation.
In writing the text of his manual. Dr. Forrester stated the "...should never be used alone" (page 75) was written for the information of the patrolman. The only purpose of the statement was that he felt the officer might rely on the chemical test and fall to note objective symptoms. It was not written with the intention of stating that his position was that the chemical test should never be relied on alone. Dr. Forrester made the following statement to clarify his position: "Unequivocally, 0.10% or higher (blood alcohol percentage) is sufficient to prove alcoholic influence even without objective symptoms."
ELECTRON CAPTURE GAS CHROMATOGRAPHY
K. I. Parker, The Hine Laboratories, San Francisco
Electron capture gas chromatography is based on absorption of electrons by absorbing materials in gas column. The method is extremely sensitive for alkyl halides, mono- and dinitrohydrocarbons, nitrated metals and hetero-cyclics. It is insensitive to hydrocarbons, amines, etc. Needs more control than other types of detectors.
USE OF STATISTICS IN CRIMINALISTICS
Charles Kingston, University of California
Defined probability as a degree of belief and as a decision-making device. Its application has long been in our laws; "the probable consequence of an action", "preponderance of evidence", "beyond a reasonable doubt", etc. We use probability by an intuitive process based on experience and personal evaluation.
For proper statistical study, certain conditions must be met:
- Planning to get the data needed for the particular problem
- Independence - if factors are not independent, then their relationship must be mathematically shown.
- Uncertainty must exist.
(Editors note; Kingston has, since this meeting, completed his Doctorate Thesis and is the second recipient of the Doctor of Criminology degree.)
BLOOD BARBITURATES BY GAS CHROMATOGRAPHY
Naresh Jain, University of California
0.14 cc of blood is triple-extracted with 1:1 acetone-ether. The extracts were dried down in a 5 ml. beaker. The extract was then dissolved in 50 ul., injected into the G. C. (Hy-Fi with Flame Ionization detector?) with a 2-1/2 foot column of 100-120 mesh firebrick with SE-30 1.5% carbowax 20 mesh 2%. Nitrogen, 15 sec/10 cc, carrier. Oven temperature 230° C; Injection Temperature 250° C. Barbiturate peaks occur some time after the solvents. The procedure, as given above, would not pick up 10 ppm phenobarbital (actually analyzing .08 ug) but would pick up 0.5.ug
George Roche, Dept. of Justice, CII Laboratory, Sacramento
Passed out mimeographed abstract of Federal Trade Commission Identification Act, 1958, listing the mandatory generic names and definitions of man-made fibers. Each laboratory also received a keyed reference collection of fiber samples.
(Editors' Note: Handouts such as these take but a few minutes at our seminars but the individual packaging for so many labs often represents as much, or more, work as the finest research project. Thank you, George.)