26th SEMI-ANNUAL SEMINAR (Fall 1965)
October 22-23, 1965

Charles E. Harvey, College of Engineering, Washington State University

Mr. Harvey's presentation covered some general methods and particularly micro sample spectroscopy including collection and handling techniques and a micro combustion-metallic distillation flask.

  1. Considered a micro sample as anything less than 20 mg and 10 mg (powder wt) as a standard size sample.
  2. Industry is primarily interested, in keeping the major constituents of its products within certain specified limits while the criminalist is primarily interested in the minor and trace elements for identification of the manufacturer batch or in some instances the particular portion of a lot.
  3. By using cup sizes appropriate for the sample size available, identical Spectra can be obtained on sample sizes ranging from 10 mg down to 0.5 mg. Preformed 10, 5, 2, 1 and 0.5 mg cup sizes are now commercially available in standard dimensions from Ultracarbon Products and the National Carbon Co.
  4. Likes to use split exposures to get an unfiltered portion of the first quarter of burn and a filtered exposure of the entire burn to take advantage of fractional distillation of the elements by the arc. Uses two apertures, the first being half clear and half with filter. After 1/4 of the burn flips to a second aperture with filter to record entire burn.
  5. Down to 1/2 mg can essentially have full sensitivity (can determine most elements down to 1/1000%) and as you go lower in sample quantity you loose proportionate sensitivity of detectability.
  6. When trying to recover minute quantities (down to 5mg) it's generally necessary to add a collector such as Li₂CO₃.
  7. Spectra of sera samples (cancer patient series) showed quite some variations in both qualitative and quantitative aspects of trace elements (i.e.. bismuth in only one; nickel in all but different concentrations). Pointed out the possibilities of utilizing trace elements in blood as an additional means of individualization of blood.
  8. Spectra of light and dark hair from three different cows, about 1 - 2mg of dry powder ash showed differences in the light and dark of each animal and greater differences between hair from the different cattle. Some differences in hair sources can be quite exceptional, such as the presence of boron in one animal and not others.
  9. Surface sampling of an object such as transfer paint on bridges or cars can be collected by rubbing with powdered diamond (relatively inexpensive and can be obtained in quite pure form) and mopping up with clear cellophane tape. Loose materials can be picked up from a surface (such as arson or explosive residues from glass) with scotch-tape. The tape is folded and ashed and eliminates trying to recover scrapings from envelope or pill box.
  10. Samples are normally ashed in porcelain crucibles and, when concerned with low fusing materials, the sample is placed on high purity filter paper, sprayed with plastic spray which keeps it from catching fire as fast and increased the carbon residue which acts as a cushion between the sample and crucible. Crucibles can be reused if clean and shiny without discoloration or dulling of the surface. In major cases it would be good insurance to use brand new crucibles.
  11. "The world's smallest vacuum cleaner" (a hypodermic needle with a small piece of filter paper over the tip and attached to a water line aspirator) can be used to reach into collection of debris to pick out a single speck of material that would be hard to segregate otherwise.
  12. Occasionally uses fine drills, available down to size 80 for something like 25 - 30 cents.
  13. He has a complete set of all the elements of the periodic system detectable by Emission as oxides or non-deliquescent salts in pure form and in graphite dilutions from 20% down to 1/1000% by factors of 1/2. These are used to synthesis a composition to prove up an analysis.
  14. An arc combustion chamber was described which was developed to distill and collect micro quantities of volatile elements on the chamber, walls as a means of breaking the elements out of the sample and for concentrating or purifying. Arsenic and mercury are very nicely quantitatively collected on the chamber walls.

Charles W. Keller, Applications Chemistry, Perkin-Elmer Corporation, Los Angeles

Mr. Keller covered the use of several instruments capable of utilizing microsamples:

  1. Atomic Absorption Spectrophotometry:
    Mr. Keller briefly covered the theory of atomic absorption spectrophotometry - the absorption of specific characteristic wavelengths of light by elements in a flame, the instrument light source being a cathode tube made of the same material being analyzed. Some of the advantages of atomic absorption mentioned were:
    1. quantitative, follows Bohr's Law and is largely free of interferences such as matrix effect
    2. general ease of sample preparation which must be in solution to aspirate it into the flame
    3. generally don't have to concentrate sample and can select wavelengths of different intensities to quantitate different concentration ranges
    4. very many elements can be extracted into organic solvent for aspiration with the advantage of concentrating and actual enhancement of the response in organic solvents
    5. the greatest use of atomic absorption in the toxicology field is doing arsenic, lead, thallium and mercury which are difficult to determine by the emission technique. Cadmium, mercury and zinc are easily done by atomic absorption.
    6. Eldon Means of Wichita, Kansas, has analyzed paraffin casts for lead and antimony; identified lead in gasoline arson residues and worked out an analytical technique for paints, determining the ratio of lead, chromium, iron and zinc.
    7. Recent publication available from Perkin-Elmer sales office: "Analytical Biochemistry and Toxicology Using Atomic Absorption Technique" discusses what atomic absorption is and gives some of the values obtained on typical types of samples. Also available are newsletters, possibly including Mr. Means' work on gunpowder residues.
  2. Microanalysis In Infra Red:
    Mr. Keller covered some general considerations in utilizing infra red absorption and microsampling techniques and accessories:
    1. first try to use the sample in a standard instrument and technique without any accessory optical aids
    2. get the sample in KBr in a small aperture such as the hole in IBM card
    3. put the sample in as near as possible to the focal point of the sample beam (this is a very desirable feature to look for in choosing an IR instrument)
    4. discussed P-E's 4X beam condenser which reduces the sample beam by a factor of 4 to 1 and spectra obtained. With the 6x beam condenser can go down to microgram quantities of material
    5. showed slides of 3X ATR Unit (Attenuated Total Reflectance Unit) which is a rather new technique. The sample is pressed against the back of the hemisphere of the ATR and at the interface the light penetrates about 1 micron into the sample before being reflected back into the optical system. Could be used on paint chips. Has run samples as small as 1 mm square. 20 reflectance units are not at all (?) applicable to criminalistics because of the quantity of material needed.
    6. Collection of micro samples on Millipore filters is a technique used in ATR work.
  3. Colorimetry to measure the thermal profile of materials - what heat the material has been subjected to in the past was very briefly discussed by Mr. Keller.

Gordon Damant, Furniture and Bedding Inspector's Laboratory, Sacramento, California

The primary purpose of the California F.B.I. Laboratory is to serve as a consumer control laboratory to verify that the labeling of furniture required by law is actually correct as to composition and claims. The types of materials analyzed fall into four major categories: (1) all types of animal, vegetable and mineral fibers, (2) feather identification, (3) foam analysis, (4) control of sterilization of second hand furniture. They do both qualitative identification of the type of material and quantitative determinations of each type in mixtures, whether it be mixtures of fibers, feathers, or rubber sprayed hair, and in some furniture can get mixtures of all types of materials involved. Analytical techniques have been worked out for quantitating various mixtures.

Some other types of examinations carried out to verify the labeling of furniture include tests for mildew proofing, moth proofing, water proofing, washability, grease content of cotton, chromium content of feathers, ammonia content of second hand and used cotton, chromium content of feathers, ammonia content of second hand and used cotton, moisture contents, oxygen number of feathers and residual formaldehyde and urine content in second hand furniture.

For quantitative analysis the laboratory uses mostly vet chemical methods, although some (such as fibers) must be done by hand. IR spectrometry is used primarily for identification of synthetic materials. Of the instrumental techniques, microscopy is probably used more than anything else; but also include visible and U.V. spectrophotometry, digital fibrograph (for classifying cotton), moisture balance, tensile strength testor, gas chromatography, a garnett machine (for making synthetic blends of fibers for standards) and photomicrography. They are investigating applications of differential thermal analysis and gas chromatography pyrolysis.

The California F.B.I. Laboratory has a reference collection which is perhaps unique in the United States. They have approximately 1140 standard samples in their library including samples of each of the approximate 60 synthetic fibers on the market, 550 samples of feathers and down, 140 samples of vegetable fibers from all over the world, large samples of hair, different cottons, different wools, and foam materials.

Any criminalist that has a problem in identifying or quantitating any fiber or other furniture or bedding material should take advantage of the facilities of the Furniture and Bedding Inspector's Laboratory or at least confer with them. There is no charge for analysis for any governmental agency and $20 for non-governmental. They would be prepared for court testimony if needed. Address; 1020 N St., Sacramento 14, California.

Keith Sorenson, District Attorney, San Mateo County

The 1955 Cahan decision regarding unreasonable search (bugging) and the 1961 Mattas vs. Ohio case decision by the U.S. Supreme Court extending unreasonable search doctrine to all State and Federal courts were cited by Mr. Sorenson as the principal cases on which other decisions have come regarding admissability of evidence obtained by search.

Mr. Sorenson stated there are three ways to follow legal search and seizure:

  1. Search incidental to a lawful arrest (most common); to constitute a lawful arrest it must be by an officer (1) with an arrest warrant; (2) without warrant but based on reasonable cause to believe the person had committed a felony; or, if by private citizen, the felony must have been committed.

    The search incident to arrest can include (1) immediate premisses (outhouses), (2) house only if arrested in house or (3) car if arrested in car. The search of the car if not arrested in the car is very controversial at the present time, with the courts excluding the evidence more and more frequently as should have been done by search warrant. This is not always practical and each case must be judged by the particular sit-uation and immediate need. In a drunk driver arrest, can search interior of car and glove compartment for alcoholic beverage (but probably not the trunk).

  2. Search with Search Warrant!

    A search warrant cannot be contested like a search on a legal arrest or by consent. A search warrant will issue on probable cause. Courts are holding more and more that the warrant must be specific as to what is being sought and cannot search for other items. However, evidence found regarding other crimes is valid if the search location of the other evidence is consistent with valid search areas for the evidence specified in the warrant. (Narcotics found in a 3" deep kitchen drawer would not be allowed if warrant specified search for a stolen office typewriter.)

  3. Search by consent:

    Consent may be implied by victim or by family (best to have signed) [Editor's note: or by suspect, also preferably signed].

    Fingerprints, clothing, hair, photographs, voice and shoes are not considered self incriminating.

Vincent P. Quinn, General Atomics, San Diego

  1. Gun Shot Residue: Can almost always detect Ba and Sb at low levels from firing either a revolver or automatic. There have been a few cases in the continued hand blank survey where more than the usual amount of one of the elements was found, but only one case (a mechanic) has shown more than the usual trace amounts of loth. Estimated. 90 - 95% of known firings have shown positives. Kits available for collection and submitting of casts.
  2. Paint Investigation: Good reproducibility on same batch. Only slightly higher variations in paint from different batches borderline for batch identification.
  3. Hair Studies; Have cut back on this work because both Jervis and Coleman are surveying 1000 individuals.
  4. Photonuclear Activation: All work so far has been by Neutron Activation. G.A. is now planning to also work with Photonuclear Activation which produces different isotopes by knocking out neutrons instead of adding. Get different sensitivities and greatly reduces sodium interference in biological samples.
  5. A new motion picture film is being produced, directed toward Law Enforcement and Legal Profession. Probably available in January from AEC.
  6. Forensic service of G.A. is available to law enforcement on a non-profit basis with the usual case cost of $200 to $300 for the analysis.

Herman Muron, Alcohol and Tobacco Tax Laboratory, San Francisco

The San Francisco laboratory is one of 8 regional laboratories. The Alcohol and Tobacco Tax Division of the U.S. Treasury Department is responsible for the collection of alcohol taxes and also does some narcotics work and covers the National and Federal Firearms Acts.

Samples submitted to the A & TTD laboratory often require distillation to eliminate the effect of dissolved solids, but many samples can be measured fairly accurately directly without distillation.

Mr. Muron discussed in general the following methods supplemented with Vu-Graph slides:

  1. Hydrometer reported to 0.1 proof
  2. Pycnometer reported to 0.05%
  3. Ebulliometer reported to 0.05 - 0.1%
  4. Refractometer - An immersion or dipping refractometer is the only type that will give results reliable to ca. 0.1%. An Able refractometer can be used for small samples, but is not reliable enough for tax determination.
  5. Bichromate Oxidation - Similar to blood alcohol determinations, using 1 ml samples. It is not an A & TTD laboratory approved-method but is commonly used by wine chemists.
  6. Williams and Etienne Tests - These are two rather obscure A & TTD methods depending on the estimation of alcohol by distribution of ethanol between two immiscible solvents. For field use only, the readings are reliable to only 1 or 2%.
  7. Gas Chromatography - Analysis has not been sufficiently reliable in their experience for use in determining alcohol tax and is not an "official method", although it is useful in "moonshine" and certain other type cases.
  8. Qualitative methods include iodoform, ethyl acetate and G.C.

The "official" methods of the A & TTD laboratory are found in the Book of Methods. AOAC, 9th Edition (10th available shortly) and in Treasury Department Publications. Hydrometer readings are interpolated to 60°F using an NBS table (Gauging Manual, Treasury Department Publication 455, 1962 Edition, $2.50 Superintendent of Documents).

Lowell W. Bradford, Santa Clara District Attorney's Office Criminalistics Laboratory

Mr. Bradford first reviewed the development of interpretation of B.A. levels from the original National Safety Council recommendations through the Indiana University Symposium on Alcohol and Road Traffic, the International Conference on Alcohol and Road Traffic and New York law making driving with a .10% B.A. level a crime without raising the question of alcoholic influence.

Strongly recommended for study and reference were:

  1. Role of the Drinking Driver in Traffic Accidents. Robert F. Borkenstein, published by Department of Police Administration, Indiana University
  2. Alcohol and Traffic Safety. Bernard H. Fox and James H. Fox, Public Health Services Publication Ho. 1043, national Institute of Health
  3. Proceedings of the International Conference on Alcohol and Traffic Safety (the 4th being held Dec. 5 - 9. 1965 in Indiana)

Other changing concepts and considerations covered were:

  1. Implied consent legislation necessitated by increasing refusal rates. (In 1948 only 2% refusal to give blood sample in Santa Clara County, now up to about 40% and in some areas as high as 10% some months).
  2. Not only are concepts changed by increased scientific information but by other pressures including disposing of work load, crowded court calendars; changing laws on search and seizure and due process, training and experience of prosecutors and changing attitudes of jurors.
  3. Changing attitudes in punishment have included increased fines, periods of greater percentage given jail terms, revocation of driver's license and psychotherapy as a condition of probation.

None of the educational and enforcement methods have been truly successful. The drinking driver has not changed. Bradford raised the question of who is the drinking driver, that is, what do they have in common by which they can be identified and thereby reached in an effort to attack this social problem.

Dr. David Roberts, M.D., Nevada Safety Council, 129 Ho. Center St., Reno, Nevada

A commercial movie filmed at Sparks by Charles Cahill Associates (Los Angeles, about $120) as a safety film presenting the concept of alcoholic influence on driving was first shown. The primary value of this movie to any crime laboratory would be for use at service club talks and introduction of the drinklng-driving problem in police training schools. It is non-technical but fairly well put together.

Very little detailed information was given in the discussion of the study following the film. (The full report is now available from the Nevada Safety Council at the above address for $1.00).

Edward A. Olson, Chairman, Nevada Gaming Control Board

Most illegal gaming in California have crooked operators. Showing the game to be crooked will make a conviction of illegal gaming easier.

Mr. Olsen introduced one of his investigators to give a very informal talk and demonstration of some illegal ("crooked") dice.

  1. Manufacturers guarantee dice to be within .0002 inch tolerance but Commission considers tolerance of .002 as legal - not affecting probability of roll significantly.
  2. Dice classifications (first two only legal dice):
    1. "Razor Edge" - 90° edges
    2. "Bevel Edged" - exact 45° level at edges
    3. "Flat" - face(s) shaved so that two sides more favored by being larger
    4. "Beveled" - one or two faces flat and others very slightly rounded to favor the flat sides
    5. "Raised Edge" - edges of one or two surfaces burred away from favored surface, slightly increasing the surface area of the two sides and also increasing the probability of the burr causing the die to trip over to smooth side
    6. Beveled at other than 45°; usually at 60°
    7. "Concave" - one or two sides concaved, giving them a slight suction action holding them from tripping
  3. Marked cards demonstrated were marked primarily for "21" (Black Jack) as high or low cards and included:
    1. "Punched" - not readily visible pin prick, but relatively easily felt
    2. "Smooth-Ruff" - texture of back of cards varied, relatively easily felt and visible by proper illumination
    3. "Corner-Crimp" - very slight crease in corner visible with lighting angle
    4. "Red Reading Glasses" - coding visible through red filter (operators may use red contact lenses).
    5. "Dobbed" - a very faint smudge like mark on card backs that with practice can be read when almost imperceptible.

Charles E. Harvey, Washington State University

Mr. Harvey is constructing a new special purpose 8 meter spectrograph utilizing a 360,000 line 8 x 12 inch B & L grating with a dispersion of 1 A/am.

Lowell Bradford, Santa Clara District Attorney Office

Water recovery is superior to cotton, waste cotton, oiled sawdust and etc., especially for lead bullets, particularly .22 bullets. Water eliminates fibrous polishing and offers much greater ease of recovery. .45 Autos are stopped in 4 feet of water and .30-06 are easily stopped in 12 feet. Shotgun pellets can also be recovered in water tank.

Normal load, soft-point rifle bullets generally mushroom badly and full Jacket bullets show collapsed sides. Rifle loads should be reduced to muzzle velocities of 1700 - 1800 feet/second to eliminate this distortion. Example: 23 1/2 grains of 4198 powder gives a muzzle velocity in this range. This loading will also work for soft-points.

No pellets recovered from a shot gun are, perfectly spherical. The pellets are dimpled from compression and some are deformed from wiping the barrel.

Flattened Deformed Normal
Cutt's cylinder 24%37%39%
Cutt's 1/2 Choke 344531
Cutt's 1/2 Choke 21 5523

Santa Clara's bullet recovery tank has a 4 foot diameter (4 foot deep tapered funnel) section at top with sound insulation around margin and with top flush with floor. The muzzle is pushed through a rubber gasket in floor above tank center. Below the top 4 foot gas blast area is a 12 foot long 2 foot diameter tank. The bottom is tapered with 60° cone which nicely accepts a large plastic funnel for recovery.

James W. Brackett, San Mateo County Coroner's Office

The criteria for matching toolmarks and bullet striations have not been well defined. The problems of developing proper criteria have included:

  1. How to describe striations mathematically
  2. How to inter-relate striations to each other
  3. What degree of similarity can be expected by chance

Brackett went through a series of mathematical derivations of general distribution equations. Although he is only still in preliminary analysis of the problems, Brackett appears to be on an approach that may well put striation comparison on a firm basis and allow probability determination of the significance of an observed "match".

Duayne Dillon, Contra Costa Sheriff's Office

Gryojet weapons are actually miniature rocket launchers (hand launch = pistol, shoulder launch = carbine and spear gun). They were developed for possible military applications and are now to be made commercially. There are 1000 specially made handlaunchers for collectors ($250) and the mass production handlaunchers will have a production cost of about $2.50, with the rockets about 15% each.

Recent articles in magazines have been exaggerated and inaccurate.

The advantages of the system are the very low recoil, low noise level, light weight, simple low cost design and high rate of fire.

The launch tube is a smooth bore seamless and vented tube with an I.D. of .512 inches. The hammer drives the rocket back into a fixed, machined firing pin.

The rocket is .50/inch in diameter, copper-coated steel with a steel disc (containing 4 ports at 15° angle) crimped into the base. The nor-mal nuzzle velocity is between 100-200 f.p.s. so it would be impossible to commit suicide with the weapon. The spin rate is 2.1 inches/foot and burn out is in 40 feet in 0.12 seconds, at which time the rocket is at maximum velocity and its energy is about equivalent to a .357 magnum. At 40 feet, accuracy is very good and at 100 feet give patterns of about 7 inch diameter (but won't go through much).

The only probable means of identifying the launcher from which a rocket was fired is by the firing pin markings. Contact of the rocket between the tube and barrel is random. Hammer marks on nose (if any) would generally be destroyed on impact.

If rocket strikes victim while still burning, the inner surface of the clothing will probably bear four smudge patterns from the streaming gas of the spinning rocket.