California Association of Criminalists
Since 1954
DRUG IDENTIFICATION
Don Fletcher, Liaison Officer for Law Enforcement, Smith, Kline & French Co.
All heart-shaped SKF products manufactured for exclusive sale in Mexico have three small dots in the score.
Scientific Information Department has on IBM all available information on a number of subjects from all American and foreign medical and scientific journals. Offered that SKF can run special reference studies on some aspects of drugs.
Again offered to supply any crime laboratory pure ingredients of SKF products.
Again offered the use of the Product Identification Laboratory, Philadelphia, for identification of manufacturer of drugs (particularly amphetamines and barbiturates) as an aid in tracing illegal traffic.
SKF formerly used tracers in their products, but now identify products by score, contour and excipient material. Excipients commonly used are sucrose, lactose, calcium sulfate and calcium phosphate.
Terra alba in SKF heart-shaped tablets won't burn, most counterfeits will.
EXAMINATION OF ALTERED DICE
Allen E. Gilmore, Dept. of Justice, Criminal Investigation and Identification Laboratory
Dice sent to CII Laboratory by Nevada State Gaming Commission were found to be what are known as "trick dice", where all four sides of the 1 and 6 are burred. If die sliding on any surface other than 1 or 6, there is a greater tendency to trip over. Burring probably was produced by rubbing on felt or table cloth, probably using some sort of jig (uniformity). Burring caused a 2/1000-inch variance in size (1/1000 tolerance allowed).
POSTMORTEM ANT BITES
Allan E. Gilmore, Dept. of Justice, Criminal Investigation and Identification Laboratory
Wounds of hand originally identified by police and played up in newspapers as being the results of torture. Body had laid on ground overnight and "wounds" were identified as being due to ant bites. Photographs of wounds shown.
DIFFERENTIAL THERMAL ANALYSIS IN SOIL COMPARISONS, PRELIMINARY REPORT
Duayne Dillon, Contra Costa Sheriff's Office, Criminalistics Laboratory
Differential thermal analysis is based upon the fact that substances absorb heat in a characteristic manner which is a function of various chemical and physical changes that occur in the material as it is being heated. The phenomenon of heat absorption is somewhat characteristic of a given material and serves as a means of distinguishing between materials dissimilar in constitution.
Internal reference material (alumina) and sample are heated in a furnace. Temperatures are determined by thermocouples, and the temperature differences of the sample and reference material are recorded as a function of the furnace temperature.
Changes taking place when material is heated may be endothermic (crystalline transitions, fusions, vaporization, sublimation, dehydration, thermal decomposition) or exothermic (crystalline transitions, solidification, absorption, hydration, corrosion and direct oxidation),
One preliminary study showed good differentiation but very poor reproducibility, primarily attributed to differences in weight of alumina and sample sizes. Another study involving four samples from different areas of one flower bed, showed the samples could be differentiated; and, in this study, duplicate samples gave good reproducibility.
Indications from this study are that differential thermal analysis will provide another parameter in the examination and comparison of soil samples.
COMPARISON OF COMMERCIAL GREASES BY GAS CHROMATOGRAPHY OF THEIR PYROLYTIC PRODUCTS
Duayne Dillon, Contra Costa Co. Sheriff's Office, Criminalistics Laboratory
(Handout, one per laboratory)
Used Wilkins Instrument and their pyrolytic attachment. Couldn't control combustion and sample size when putting grease directly on coil. Used hydrogen disulfide as a solvent (poor response to hydrogen flame detector), 15 mg/mL sample, 1-U lambda on coil, alkamide column, oven temperature 50° C, injector block 150° higher than oven (normally needs to be 50° higher; but, when using pyrolysis oven heated from injector block by conductivity, need 150° higher in block to get 50° higher in pyrolysis oven), pyrolysis at 1000° C for 12 seconds.
Three standard brand chassis greases all had the same peaks with peak area ratios so slightly different that it is doubtful if the technique is a desirable one to use, because instrumental and technical variations from day to day would probably give as much difference as shown in the three samples.
Comparison of various types of greases (chassis lubricant, cup grease, hair preparation, margarine, ointment, and vasoline) showed no unique peaks, but greater differences in relative peak areas, so the technique would be an aid in characterizing grease samples.
COMMENTS by Dr. Vincent P. Guinn: General Atomics survey of 16 different sources of automobile greases showed 11 or 12 trace elements in considerably different combinations and concentrations. Doesn't appear to be any difficulty in differentiating greases by activation analysis. Problem is separating grease sample from contamination. So far, have not come up with successful method of separation.
IDENTIFICATION OF MEPROBAMATE BY THIN LAYER CHROMATOGRAPHY
Fred Wynbrandt, Department of Justice, Criminal Investigation and Identification Laboratory
Extract of blood, spotted on TLC and developed with Methyl Alcohol: Butyl Alcohol (60 : 40), gives no trailing.
Spraying technique:
IDENTIFICATION OF MATCHES BY INCLUDED FOREIGN MATTER
John A. (Tony) Kearns, Santa Ana Police Department, Criminalistics Laboratory
Matchbooks are made of reclaimed paper and include small pieces of emulsion and paint chips. These inclusions are usually difficult to see; however, a method was described which makes them readily visible and photogenic.
A simple holder to hold two matches side-by-side on edge can be constructed from a piece of cardboard and three thumb tacks in a row, the center tack just slightly out of line to accommodate the two matches. The holder with the matches is placed in a Petri dish and covered with benzene. There will then be visualized hundreds of points of identification (some much more prominent than others).
The method is particularly adaptable for color photography for court presentation as well as for point by point comparison.
The benzene causes no swelling or distortion of the evidence. It rapidly dries out with the evidence returned to its original condition.
UNUSUAL TOXICOLOGY CASE
James W. Brackett, Jr., San Mateo County Coroner's Office Laboratory
Case in which routine toxicological examination was negative except for the presence of 15% methemoglobin. Victim did not have access to a large number of compounds capable of producing methemoglobin (sodium and calcium hypochlorite and hydrogen peroxide). Causative agent was found to be sodium nitrite, without question (1.2 grams recovered from gastric lavage...also present in the urine). It was theorized that the victim had taken a mixture of 6% hydrogen peroxide and an ammonical solution of a detergent (a mixture being used to bleach the manes and tails of animals being exhibited for show). In vitro experiments have, however, failed to produce sodium nitrite with these chemicals.
Chromatography System:
Silica G TLC plates, Developing System 65:20:10:5 :: Acetone:n-Butyl Alcohol: Ammonium hydroxide; water.
Locating reagents:
SEMINAL STAINS
Duayne Dillon, Contra Costa Sheriff's Office, Criminalistics Laboratory
Considers acid phosphatase as conclusive for the presence of semen whether or not a Florence Test and/or spermatozoa examinations are negative.
Comparison of recovery procedures, using standard stains on cotton. Field counts on recovered material made. Using water recovery with intermittent agitation for 10 minutes as reference, the following relative results were obtained:
| water, 2 minute Intermittent agitation | .63 |
| water, no agitation, 10 minutes | .45 |
| 1% aerosol solution, intermittent agitation | 1.8 |
| .5% CMC (carboxymethylcellulose) in water, manual agitation, 10 minutes | 2.36 |
| Ultrasonic vibrator, water only, 2 minutes | 2.12 |
| same with additional time | lower |
| Ultrasonic, 0.1% aerosol, 2 minutes | 3.75 |
| CMC, ultrasonic | very high background, unable to see actual precipitate on slide |
| CMC with aerosol and ultrasonic |
Under none of the conditions did the ratio of intact sperm to sperm heads change.
Anti-Seminal Precipitin Serum:
Initial titer of anti-serum much lower than anti-blood. Anti-seminal serum will react with blood, so the antiserum must be absorbed with human blood serum. Tried to use conventional micro-precipitin ring test, but unable to get good rings except with full strength semen. Agar diffusion in capillary tubes not successful in lower concentrations. Ended up using immuno-diffusion on oxide paper (cellulose acetate paper), using 1 lambda each of extract and anti-serum.
Details of procedure were in handout (one per laboratory). Anti-Serum by Mann.
THE TALKING CORPSE
Raymond H. Pinker, Los Angeles Police Department, Criminalistics Laboratory
Speaker has participated in 8-10 autopsies of disinterred bodies in 35 years, bodies buried from 1 week to 8 years. Particular case discussed had been entombed for approximately 9 months.
First investigation had shown one wound in chest from two shotgun blasts, with heavy powder smudging. 12-gauge shotgun, auto-loading. Also wound in right temple from a .38 Special. Smudging on middle and ring finger of left hand. Case written off as suicide; but, with $40,000,000 involved and no apparent reason for suicide, question arose in some quarters whether it was actually a suicide. Two "eminent" medical authorities opinioned that a man shot in the abdomen with a 12-guage shotgun would be rendered incapable of having inflicted additional wounds on himself.
Second autopsy, with 9 pathologists and 2 criminalists. Entire tissue on right side of head was excised, and x-rays showed lead splattered into surrounding tissue. Entrance hole also showed sooting and possible charring. Powder particles were also present in the wound. Curiously, none of the pellets of the two blasts of shotgun in the abdomen struck vital organs or large blood vessels. X-rays of the left hand showed a couple of tiny lead fragments arising from holding the cylinder of the gun at the time is was fired into the head. Other investigation developed the fact that the ammunition was low base ammunition for skeet shooting and the weapon was defective - it fired full automatic. It was the general conclusion of all present that this was an undoubted case of three self-inflicted wounds and was undoubtedly a suicide.
DIFFERENTIATION OF SHORT AND LONG ACTING BARBITURATES IN BLOOD
Jack Villaudy, Los Angeles County Coroner's Office Laboratory
No handout, no abstract submitted.
Identification of short or long acting barbiturates based on relative densities at 240 and 270 mμ of extractions with 0.5 N NaOH and NaOH-NH4Cl. Where recovery intermediate, it is necessary to chromatograph to determine if intermediate acting or mixture of short and long acting. If mixture, can calculate from readings approximate quantities of mixture of two barbiturates.
EXTRACTION METHOD FOR DARVON
Edward Thompson, Los Angeles County Coroner's Office Laboratory
Have found in every case of death due to Darvon an unidentified derivative which has a completely different U.V. curve. It has a maximum at 252 mμ and a sharp inflection point at 295 mμ. In base, the solution becomes cloudy and can't be read.
Usual extraction procedure, paper chromatography and iodoplatinate spray gives a blue spot (Rf 0.8), as does Darvon, but never able to cut spots off paper and get normal Darvon curve. Using method of Clarke (reference is in Lundquist's latest book) with buffered paper, noticed when chromato-graphed that Darvon was irradiated with ultraviolet light of short wavelength for an hour, a yellow fluorescent spot was obtained in area where blue spot would develop with iodoplatinate. When this spot is cut out (without spraying with iodoplatinate), it gives a 252 mμ maxima with inflection at 295 mμ. If sprayed, the fluorescent spot can't be removed from the paper. The derivative is not only chloroform soluble from basic solution but also from hydrochloric acid solution. The sulfate salt is only partially soluble in chloroform.
Extraction procedure for Darvon: Homogenize 50 grams of tissue and 50 mL 0.5 N NaOH, and extract with two 100 mL chloroform. Filter and evaporate chloroform to dryness. Take up residue in two 20 mL portions of 0.5 N HCl, filter and extract with two 100 mL chloroform. Filter and evaporate CHC13 to dryness. Spot is put on buffered citrate paper and chromatographed. The paper is then exposed to U.V. light for one hour, the spot cut off and read in spectrophotometer. Calculate the amount of Darvon by comparing to Darvon standards treated the same manner.
Liver seems to be the tissue of choice. In some cases, Darvon was recovered from both blood and liver; in other cases, it was recovered only from the liver. Found in the kidney in one case. Levels found have ranged from 2 to 12.6 mg%. Some cases were complicated with alcohol and one with barbiturates .
Histories that have been obtained indicate Darvon is a rapidly acting poison, ingestion being just a few hours before death. Amounts taken in some known cases have been 15, 24, and 31 65-mg capsules. In a couple of cases there were histories of convulsions following ingestion.
FAR ULTRAVIOLET SPECTROPHOTOMETRY
Lowell Bradford, Criminalistics Laboratory, Santa Clara District Attorney's Office
Original ultraviolet data on 169 compounds appeared in Mikrochimica Acta, 1956. Now, using a modified Beckman DK-2 on a National Institute of Health grant, have already found that there are significant, practical and useful absorption data under 220 mμ. Absorptivity is far greater than in the range above 220 mμ; i.e., morphine at 208 mμ has 50X greater absorption than at 285 mμ. Can therefore detect much smaller quantities of material. Has just done very preliminary work so far. Many technical problems with far U.V.
SUMMARY OF RECENT NEUTRON ACTIVATION ANALYSIS WORK APPLICABLE TO CRIMINALISTICS
Dr. V.P. Guinn, General Atomic, Division of General Dynamics, San Diego
A. Gun Powder Residues:
Studied possible application of method already developed to the Oswald case (Kennedy assassination). Two sets of paraffin casts were made after firing similar type of rifle single shot and after three rapid shots. Of 8 cases from one set (both hands, both cheeks, single and multiple firings), only one gave positive diphenylamine test, and it was possibly questionable. The other set examined by activation analysis showed positive (in all casts) in the case of triple firings and fairly strong indications of firing in the casts from single firing. The set tested with diphenylamine was then examined by activation analysis: The barium was pretty well washed off by the diphenylamine test. The antimony on the single firings was about the same as the untreated set, and the triple firing set showed a little lower (60%) antimony, but still quite significant amounts. The results indicated that the Dallas P.D. Oswald casts could still be run by activation analysis for antimony.
B. Tagging Gun Powder:
There are about 16 rare elements with high sensitivity to activation analysis that would be particularly suitable for tagging gun powder itself. It would be rather simple and would involve virtually no expense to have gunpowder manufacturers tag their products with these elements (perhaps 3 of them) at levels of less than 1 p.p.m. Could actually go farther by having each ammunition manufacturer tag each caliber differently. By activation analysis, it would be possible not only to then determine if an individual had fired a gun recently, but also the make and type of ammunition used. (Reloading powder would be tagged differently). From experiments with tagging powder, have found the amount of gunpowder residue left on the firing hand is between .001 and .01% (at least in .33 caliber) of the powder charge.
ACTIVATION ANALYSIS IN BURGLARY CASE PAINT TRANSFERS
Donald Bryan, General Atomics, Division of General Dynamics, San Diego
Lug wrench left at scene had brown paint specks grossly similar to paint from door of burglary. The wrench also had blue paint similar in color to suspect's vehicle. The blue paint was found by activation analysis to have five elements (titanium, aluminum, sodium, copper and manganese: the first two in parts/hundred and the latter three in p.p.m.). Three trace elements agreed within range of error. Apparent discrepancies in Ti and Al values were attributed to manipulation difficulties related to the very short half-life and to static causing minute samples from lug wrench to stick on sides of polyethylene vial away from counter more than the standard paint.
Ten samples of light blue automobile enamels ("very similar in color to the suspect's vehicle") showed substantial differences by activation analysis. (Five were dupli-color touch-up paints manufactured by the same company).
IDENTIFICATION OF WIGS
Don M. Harding, San Mateo Sheriff's Office, Criminalistics Laboratory
Wigs fall into natural classifications: all human hair, all animal hair, synthetic fiber (nylon basically) and combinations of others. Further classification by method of manufacturing: hand tied or machine made.
Europe is primary source of human hair. Indian and Oriental hair are of decreasing quality because of increasing coarseness. Animal hairs used are yak (excellent for white and light-colored hair) and angora (used in front portion of toupees).
Wefting is a long strip of fabric to which hair is sewn into the edge at right angles and the material machine sewn onto cap for wigs. The spacing between weft is one item determining quality and cost of wigs.
Hair color is highly standardized in wig industry, using standard color hair samples on rings.
Identification of single hairs from wig is complicated by wigs being made from a mixture of human hair.
HAIR STUDY OF AMERICAN ACADEMY OF FORENSIC SCIENCES
Raymond Pinker, Los Angeles Police Department, Criminalistics Laboratory
One questioned and four sources of standard hairs used in study. By neutron activation analysis, the questioned hair closely matched one of the standard hair sources and the other three were very easily eliminated.
SCREENING METHOD FOR BARBITURATES
W. Jerry Chisum, San Bernardino Sheriff's Office, Criminalistics Laboratory
Reference: A.S. Curry, Brit. Medical J., Oct. 26, 1963, pages 1040-1041 Durry's rapid (5 minute) screening test for barbiturates was described.
Apparatus was described as a 100 mL beaker on a magnetic stirrer with a distilled water reservoir set up above beaker with spring clip on rubber tubing leading to glass pipet delivery tip. An aspirator tube with the hole in the side (not tip) is used in the washing process (clamped in position to leave 10 mL volume in beaker).
Method: To 10 mL chloroform in beaker add 2.0 mL blood and 2.5 mL phosphate buffer (M/15, pH 6.95 [0.624 g Na2HPO4: 3 H2O + 0.363 g KH2 PO4/100 mL water]). After vigorous mixing with magnetic stirrer for 2 minutes, allow layers to separate and syphon off the blood. Complete removal of all blood color is accomplished by washing 3 or 4 times with approximately 50 mL of water. Syphon off water, removing all but traces of water by manipulating beaker. Add 1 mL mercury reagent (Stock is 0.5 g mercuric chloride/50 mL water with 3 drops HNO3 added; working solution is made by diluting 1 mL of stock to 50 mL and adding 0.42 g. NaHCO3 ). Chloroform-soluble mercuric barbiturate is formed with vigorous 2 minute stirring. Syphon off excess mercuric chloride and wash twice with 40 mL water. Add 1 mL dithizone (chloroform solution prepared fresh every 2 weeks and adjusted to give an optical density of 2 at 605 mμ, 1 cm) carefully under the chloroform and distribute the color evenly by slow rotation. Observe color immediately.
Unchanged green color implies absence of barbiturate and a clear orange is seen when drug is present.
Chisum commented that difficulty develops from attempting to use dithizone that is not freshly prepared.
