California Association of Criminalists
Since 1954
A DYE SALT METHOD OF ALKALOID ASSAY USING PICRIC ACID
Jack O. Carter, Los Angeles Police Department
The method described is based on the principle that an organic base such as Codeine can be combined with an organic acid to form a colored salt through controlling the pH. Since Codeine has a pKa of 7.95 and Picric acid has a pKa of 3.8, a buffer solution of pH 4.3 was chosen to form the dye-salt.
The absorptivity of Codeine picrate at 400 millimicrons was said to be 5.08.
A STUDY OF TRANQUILIZERS FROM THE STANDPOINT OF A CRIME LABORATORY
Ron Briglia, Orange County Sheriff's Office
Five cases were cited in which blood alcohol determinations were low (0.04% to 0.11%) in spite of strong objective symptoms of intoxication in each ofthe subjects at the time of arrest for 502 CVC. In each of these cases extracts were made of the blood by the method of Brackett and Bradford. The ultra-violet absorption spectra were negative for barbiturates. Each of the bloods exhibited an absorption curve in the acid fraction with an absorption maximum at 235 millimicrons and a lesser maximum at 310 millimicrons in pH 9.5 buffer.
Although other indications were strong that one of the tranquilizers was responsible for the objective symptoms shown by the drivers in question, no tranquilizer was found which gave an identical curve in vitro. It was considered possible that the unknown substance represented a metabolite of some drug. Further work is indicated.
EXAMINATIONS FOR THE SELECTION OF CRIMINALISTS
Anthony Longhetti, San Bernardino Sheriff's Office
The steps in the composition and evaluation of an adequate Civil Service Examination to fill the position of assistant criminalist were described.
ASPECTS OF SECONAL CRYSTALLIZATION
James W. Brackett, Jr., Santa Clara County District Attorney's Office
It was pointed out that heating to avoid supercooling can be employed to materially improve the rate of Seconal crystallization. Seeding and recording the rate of crystal growth at different temperatures gave the following results:
| Rate of Growth | Temperature |
| .08 mm/hr | 25oC - 28oC |
| .38 mm/hr | 50oC |
| .8 mm/hr | 71oC |
Sublimation onto Seconal seeds at 100oC was recommended as no isomorphous substance has been found yet that will give characteristic crystals.
WHAT CONSTITUTES BEING UNDER THE INFLUENCE OF BENZEDRINE?
Martin Klein, Los Angeles County Sheriff's Office
The dilemma of the law vs. the practical aspects of the enforcement of that law was discussed. A relatively new section of the vehicle code (506.1 CVC) makes it a felony to drive while under the influence of amphetamine.
Although the Army and the Air Corps did some research during World War II their findings were said to still be classified. Very little is available on the symptoms exhibited by a person under the influence of amphetamine.
Research using chemical tests or the body fluids to correlate levels with symptoms was proposed. Sydney Kays's method as set forth in Gradwohl's Legal Medicine was given as a starting point.
THE EASTMAN TYPE C COLOR PROCESS
Lt. John Bigham, Los Angeles Police Department
The principles by which acceptable color photographs can be made were discussed. Flat lighting (not more than 1:3 ratio) is important. Light sources should not be mixed, i.e. daylight and fluorescent, etc. For photomicrography a strobe or 3800K light was recommended.
For court purposes it was recommended that key shots be duplicated in black and white in the event the color is kept out of evidence.
The Type C color process is said to represent a saving of time and money over other methods used by L.A.P.D. Examples of the work were passed around.
A NEW MICRO TECHNIQUE FOR DIFFERENTIATING BARBITURATES
George Stevenson, M.D., Asst. Prof. of Pharmacology, School of Medicine, U.C.L.A.
The method presented is based on partition coefficients of the various barbiturates between chloroform and water. A solution of 10 to 15 μg of the questioned barbiturate in 25 ml of chloroform is extracted successively with 5 ml each of the following buffers:
A. pH 9 Borate buffer (National Bureau of Stand.) diluted to 0.025M
B. pH 10 Carbonate buffer (National Bureau of Stand.) diluted to 0.025M
C. pH 11.8 Phosphate buffer (National Bureau of Stand.) diluted to 0.025M
The Ultra-Violet absorption spectra are read in alkali and acid. The percentage of barbiturate in each solution is calculated from the absorption at 240 millimicrons.
A table of partition coefficients for the various barbiturates was given.
In order to differentiate pairs in which the partition coefficients were close, Potassium Permanganate oxidation is employed. Ultra-Violet absorption spectra of the extract of the treated and untreated chloroform is used to calculate the percentage recovery. The percentage recovery enables an identification between the pair to be made.
Amobarbital is identified by its resistance to hot sulfuric acid. Pentobarbital is identified by its resistance to chronic acid. Phenobarbital is identified by nitration using conc. nitric acid. The nitrophenyl absorption curve then appears as a hump at 265 millimicrons when the acid extract is read in the ultra-violet.
THE SYNTHESIS OF HEROIN FROM BASIC ORGANIC MATERIAL
Clifford C. Cromp, Los Angeles County Sheriff's Office
A case was cited in which the Defense Attorney claimed a Federal Narcotics Law was unconstitutional. The law states that possession of heroin is Prima Facie evidence of illegal importation. The attorney claimed that because heroin could be synthesized it could have been made in this country and that the Federal Law was therefore unconstitutional.
It was shown that the amounts synthesized were very small and that all had been done as basic research into the structure of morphine.
THE DETERMINATION OF ETHANOL AND OTHER VOLATILES FROM THE BLOOD USING GAS CHROMATOGRAPHY
Jack Cadman, Orange County Sheriff's Office (Co-authored by Theron Johns, Beckman Instruments, Inc.)
A method was presented by which ethanol and other volatiles present in the blood are extracted into a solvent which is injected into the Gas Chromatograph and read quantitatively and qualitatively. N-propyl acetate is employed as the solvent vehicle which is added 1:1 ml to the blood in a 5 ml capped centrifuge tube together with 1 gram of anhydrous potassium carbonate. Vigorous shaking to dissolve the potassium carbonate and centrifuging to break the resulting emulsion results in a clear solvent layer containing the ethanol and other volatiles.
The 12 ft. column employed in the determinations is packed with 42-60 mesh C-22 firebrick impregnated with 28 grams of liquid to 100 grams of firebrick. The liquid used for impregnation is a mixture of 15 parts by weight of Flexol 8N8, 10 parts of diisodecyl phthalate and 3 parts polyethylene glycol 600. Ethyl ether, methanol, acetone, ethanol, and isopropanol are separated by this column.
Blood alcohol determinations by the method of Kozekla and Hine were shown to correlate with those made by the subject method.
BLOOD PATERNITY METHODS AND NOMENCLATURE
Lowell W. Bradford, Santa Clara County District Attorney's Office
California legislation and court decisions were briefly reviewed. The volume of cases handled and percentage of exclusions for Santa Clara County were given. The cost of sera used per test was given as $2.00 to $6.00.
Sources of typing sera were listed as:
| Certified Blood Donor Service 14616 Hillside Avenue Jamaica 35, New York |
American Hospital Supply Co. 1210 Leon Place Evanston, Illinois |
| Ortho Pharmaceutical Supply Raritan, New Jersey |
Hyland Laboratories 14501 Colorado Blvd. Los Angeles, Calif. |
References on the law, theory, and techniques were also given.
Identification and test record cards of the type designed and used by the Santa Clara County District Attorney's Office were distributed. The frequency distribution for each of the blood groups was given for Santa Clara County together with the distribution given by Wiener.
A description of pit-falls to be avoided in making accurate tests and drawing valid conclusions followed. It was recommended that Heparin be used in the syringe with which blood is drawn from a child. Re-check of any exclusion or unusual blood type was also recommended. The age of the blood sample is very important. The fresher the better. Care must be exercised in making "N" exclusions. By testing more than one child it may be possible to determine the genotype of the mother. No child under the age of 3 months should be tested. Du variant test should be made whenever "d" negative and other big factors are positive. Mother exclusions should be considered technique error until properly re-checked.
ODD AND UNUSUAL METHODS OF' IDENTIFICATION IN FIREARMS CASES
Charles M. Wilson, Wisconsin State Crime Laboratory
It was emphasized that no detail is too small to be considered in a firearms case. A thorough examination of the weapon together with photographs and a recovery of any residues in the barrel should be made. Positions of cartridge cases, flares, mechanical defects, or the position of moving parts of automatic weapons can be of utmost significance.
X-ray photographs of a bullet in the body which could not be recovered were responsible for making an important identification when a substitution was later made in the body.
Defects in lettering on cartridge cases can be a valuable identification. Extractor marks on unfired ammunition have led to the proof of the existence of or the recovery of a second weapon which was critical to the case.
It was recommended as a general philosophy in investigating a case that all evidence be recovered. It can always be released later if it is of no value.
THE PRESENT STATUS OF CHEMICAL TESTS FOR INTOXICATION
Ray Pinker, Los Angeles Police Department and Robert Stettler, Orange County Sheriff's Office
An earlier study, A Critical Evaluation of the Intoximeter, presented by Ray Pinker at the 10th Semi-Annual Seminar of the C.A.A., October 18 & 19, 1957 showed that duplicate Intoximeters agreed better with each other than they did with blood alcohol values for the same subjects. Since that time several modifications were made in the instrument and the approved technique of sampling by Dr. Forrester. In order to evaluate these modifications, another test program was instituted.
INTOXIMETER STUDY
| Correlation of actual blood alcohol values | Correlation of Intoximeter alcohol values with Lab A blood values | ||||
| Divergence from Lab A |
Frequency Lab B |
Frequency Lab C |
Frequency Lab A |
Frequency Lab B |
Frequency Lab C |
| Blood 0.00 |
3 | 5 | 4 | 4 | 5 |
| 0.01 | 7 | 6 | 3 | 4 | 5 |
| 0.02 | 4 | 2 | 5 | 7 | 2 |
| 0.03 | (all bloods not tested) | 5 | 6 | 6 | 4 |
| 0.04 | (all bloods not tested) | 3 | 1 | 2 | |
| 0.05 | 1 | 1 | 1 | 0.06 | 1 | 0 | 0 |
| 0.07 | 0 | 0 | 1 | ||
| μ | 0.011 | 0.014 | 0.023 | 0.020 | 0.020 |
| Range | -.01 to +.02 = .03 | -.05 to +.01 = .04 | -.06 to +.03 = .09 | -.03 to +.05 = .08 | -.07 to +.04 = .11 |
Comparison of three Intoximeter units taken from the same subject at the same time and analyzed by three different laboratories. Samples were taken from twenty-five subjects arrested for 502 CVC. Laboratory A Intoximeter results were used as reference values.
| Divergence from Lab A Intoximeters |
Frequency Lab B |
Frequency Lab C |
| 0.00 | 4 | 5 |
| 0.01 | 8 | 7 |
| 0.02 | 4 | 1 |
| 0.03 | 3 | 1 |
| 0.04 | 0 | 2 |
| 0.05 | 1 | 2 |
| 0.06 | 1 | 0 |
| μ | 0.017 | 0.017 |
| Range | +.03 to -.06 = .09 | +.04 to -.05 = .09 |
STUDY OF FIVE BREATH INSTRUMENTS
A report was made at a controlled study of four volunteer subjects who were given known quantities of alcohol and then tested with all available breath devices. Blood samples were drawn from each of the subjects at hourly intervals. A portion of each blood sample was extracted and run immediately in the Gas Chromatograph. Subsequently two determinations of the blood alcohol value were made using the method of Kozelka-Hine and a third was made using an aspiration method by three of the laboratories represented. The breath instruments studied were: the "Alcometer," the "Breathalyzer," the "Drunkometer," the "Intoximeter," and the "Gas Chromatograph." The results of all testing was presented in the form of separate graphs for each subject plotting time as the abscissa and the alcohol values found by each method along the ordinate.
It was observed that the Kozelka-Hine and Gas Chromatograph determinations of the blood showed good correlation for each of the subjects. Of the breath instruments the "Breathalyzer" showed the best correlation with the blood alcohol values.
BREATHALYZER
A short series using new catalyzed dichromate tubes in the Breathalyzer vs. blood alcohol determinations by the method of Kozelka-Hine on subjects arrested for 502 CVC.
| Blood Alcohol Kozelka-Hine |
Breathalyzer (Catalyzed Tubes) |
Deviation |
| .254 | .255 | +.001 |
| .217 | .210 | -.007 |
| .272 | .240 | -.032 |
| .243 | .215 | -.028 |
| .246 | .240 | -.006 |
GENERAL
It was stated that New York is experimenting with the Breathalyzer. Some physicians are refusing to draw blood samples because they cannot be assured of protection against civil suit.
The Intoximeter has been abandoned in San Diego except to determine that alcohol is present in the suspected driver.
The Los Angeles County Sheriff's Office reported that the use of Intoximeters is left to the discretion of the station officers.
It was reported that the Breathalyzer is used in Switzerland. If the subject does not indicate that he will accept the Breathalyzer finding, a blood sample is drawn.
