24th SEMI-ANNUAL SEMINAR (Fall 1964)
CALIFORNIA ASSOCIATION OF CRIMINALISTS
October 22-23, 1964
COMPARISON OF THE NALLORPHINE TEST AND URINARY ANALYSIS IN THE DETECTION OF NARCOTIC USE
Kenneth Parker, The Hine Laboratories, San Francisco (Published, in Clinical Pharmacology and Therapeutics, 5, 405, 1964)
Parker's presentation was baaed on controlled experimental single (acute) and multiple (chronic) dosages of narcotics (primarily codeine and morphine) given to human subjects and followed by nallorphine (Nalline) testing and on some 900 urines submitted by the State Parole Division from parolees who had positive or equivocal Nalline tests or other Indications of narcotic use. Some of the significant points brought out were:
- Almost always recovered Nalline from urine when 1-1/2 - 2 hours have elapsed after injection. It may or may not be recovered in earlier sample, at least partially dependent on the status of the bladder at the time of injection.
- Codeine la partially converted to morphine — also norcodeine. Always find morphine present when codeine is taken. In heavy codeine use, also find "metabolite X", which has an Rf slightly higher than codeine.
- The ratio of morphine to codeine increases as codeine is continuously administered.
- The Nalline test is not positive in acute (60 - 90 mg) codeine dosages. A subject must receive codeine every 6 hours for 3 days to get a positive Nalline test.
- With a single 15 mg dose of morphine, the pupillary test reaches its maximum response at about the fourth hour after the morphine and then rapidly decreases to negative responses in 12 hours. At no time did the Nalline test give 100% positive, or 100% positive and equivocal test combined, in the single dosage experiments,
- Morphine was always present in the urine from the 1st through the 12th hour after a single morphine dosage and was positive in 50% of tests after 36 hours. Urine morphines were 100% positive at 24 hours after completion of chronic morphine injections and 80% positive after 48 hours.
- Advantages of the Nalline test were given as:
- Detection of many narcotics usesd including heroin, morphine methadone, Demerol, but not codeine in acute dosage.
- Results immediately available.
- Regular contact between subject, parole officer and physician.
- Disadvantages of the Nalline test were given as:
- Administration of drug with frequent unpleasant side effects and possible serious effects if subject addicted rather than just a user.
- Must be administered by a physician in a fixed controlled area.
- Surprise testing is difficult. Most tests have to be done on an advanced schedule; therefore, it allows moderate narcotic use.
- Relatively insensitive with equivocal tests common, causing uncertainty.
- Congregates large numbers of narcotics parolees in one area at the time of test with known instances of arrangements made for a "post-Nalline-party."
- Does not detect acute codeine dosages.
- Chemical Test advantages were given as:
- Greater sensitivity with no false positives or doubtful results.
- Can simultaneously detect codeine, oxycodone, morphine, heroin (as morphine) and dilaudid.
- No need to inject a drug.
- Specimen can be obtained anytime by parole officer for surprise testing with no need to assemble together large numbers of parolees.
- Parolees don't have to miss up to a half-day of work to take test.
- Results can be rechecked on the same sample, or supplementary tests for methadone and Demerol can be run.
- Chemical test disadvantages were given as:
- Slight delay in results; one working day required for the analysis.
- Single test (acid hydrolysis) does not detect methadone and Demerol.
- A positive Nalline test is not, in itself, a conclusive test for narcotic use, in Parker's opinion.
- Parker is using a single solvent extraction of 20 ml urine sample, spotted with methanol-acetone (1:1), developed on 8 x 8 inch TLC plates with an ethanol: NH₄OH, dioxane: benzene (5:5:40:50) solvent system.
- Other references of interest:
- Cochin, J. and Daly, J.W.: Experimentia, 18, 294, 1962 (re: identification of analgesics in urine by TLC)
- Fujimoto, J.M., Way, E.L. and Hine, C.H.: J. Lab. & Clin. Med., 44, 627, 1954 (re: extraction method)
COMPARATIVE STUDIES ON THE METABOLISM OF INORGANIC ARSENIC
Dr. S A. Peoples, Chairman, Department of Physiological Sciences, University of California, Davis
By invitation, Dr. Peoples presented some of his work on arsenic.
Some arsenic is present in every animal and plant, with seafood having a propensity for storing arsenic (up to 100 ppm).
Lactating cows were fed arsenic-antimony and arsenic trioxide at different levels (up to very close to reported toxic levels) for a period of more than three weeks. Contrary to published information, Dr. Peoples noted a "blood-milk" barrier, in that no increase in milk arsenic levels were found.
Arsenic was found to be stored principally in the kidney, spleen and liver, with very low levels in fat. He now feels the principal route of excretion is the urine. In chronic feeding experiments (cows), urine levels were getting back to normal after two weeks of arsenic-free diet.
Using different animals, he showed the great differences in arsenic storage. Control rats had 15 ppm; a lethal level for any other animal. He expressed the opinion that the storage level in the various tissues of the rat is largely due to their blood content.
In suspected arsenic poisonings, the best thing to analyze is the urine. If anyone has had arsenic recently, it will be found in the urine. If not in the urine, finding it anywhere else will be a problem.
Arsenic is stored in the tissues in the pentavalent state, regardless of the form administered, and Dr. Peoples stated that they had not been able to corroborate published findings that as much as 15% of arsenic is excreted in the trivalent state. He doesn't think it to be that high.
In most animals, arsenic is not an accumulative poison and is rapidly excreted at a reasonable rate.
PHARMACEUTICAL ASPECTS OF CRIMINALISTICS
Richard Penna, School of Pharmacy, University of California, San Francisco
Two areas where the pharmacist can be of direct help to the criminalist:
(l) drug identification and (2) assist in location of early clinical studies of new drugs (which should generally include laboratory analysis).
Penna also discussed several pharmacological journals which might be of interest, particularly to those involved in toxicology and who need to keep current. These included:
- Clin-Alert, 15-25 issues/yr $15.00, Science Editor Inc., 1522 Commonwealth Bldg., Louisville, Ky. (side effects of drugs and drug toxicity)
- Current Contents, weekly $15.00/yr., Institute for Scientific Information, 325 Chestnut Street, Philadelphia, Penn. (Title pages from every journal in chemical, pharmacal, medical and live sciences appearing that week, both domestic and foreign)
- J. of Clin. Pharmacology and Therapeutics, bimonthly $17.50/yr, C.B. Mosby Co., 3207 Washington Blvd., St. Louis, Mo. (clinical aspects)
- J. of Pharmaceutical Sciences, $2/yr. for members, American Pharmaceutical Association, Washington, D.C. (primarily pertaining to the pharmaceutical industry; has predominantly articles on drug analysis in their finished dosage form; i.e., how to detect phenylporpanolamine in the presence of aspirin).
Discussed over-the-counter drugs that may be used for illicit or suicidal purposes, including; Somiex (antihistamine and scopolamine), other antihistamine sleep products, phenylpropanolamine and ephedrine products, nasal inhalers, etc. Also discussed anticipated drug combination interactions and sensitization to local anesthetics.
PRELIMINARY STUDIES OF FORCE NECESSARY TO FRACTURE THE HYOID BONE IN MANUAL STRANGULATION
Clifford C. Cromp, Los Angeles County Sheriff's Department
Using four human hyoid bones obtained from autopsies, Cromp measured the forces needed to break them, using a Soil Test Triaxial Apparatus. He measured both the deflection (inches) required and the load (pounds) at the break point. Nine to eleven pounds were required with two bones from 31 year old subjects and only six to seven pounds for two bones from 42 and 43 year old subjects. This would tend to confirm an expressed opinion that the hyoid bone is more easily fractured when more completely ossified at about middle age. A high degree of variability of the deflection results was noted, indicating the variance of flexibility with size and shape.
(Editor's note: Cromp is continuing on this project.)
LSD-25 IDENTIFICATION DATA
Paul M. Dougherty, San Mateo County Sheriff's Department (with technical assistance of James Brackett, John Williams and Fred Wynbrandt)
Dougherty handed out a seven page data sheet covering the pharmacology, physical properties, analytical methods, tablet composition (Sandoz) and references.
Two samples of tablets may be obtained from Dougherty by written request on official stationary. He may have additional copies of handouts for those who did not get them.
USE OF THE MONOCHROMATOR OF THE DK-2 IN REFRACTIVE INDEX AND DISPERSION COMPARISON OF GLASS FRAGMENTS
John Davis, Oakland Police Department
(Note: Abstract submitted by Davis)
In this paper Davis described and illustrated with color slides the simplicity with which the monochromator of the Beckman DK-2 Spectrophotometer can be adapted to serve as a source of illumination for a microscope, permitting rapid comparisons of refractive index of glass fragments at various wavelengths immersed in appropriate liquids. Liquids, microscopic equipment and specimen cells are the same as those described by Davis at a previous CAC seminar and reported in the Journal of Criminal Law and Criminology, Sept-Oct 1956, Vol 47 #3. Illumination, however, is now obtained from the DK-2, permitting adjustments to be made either by changing wavelengths or the composition of the liquid.
This adaptation involves construction of a microscope platform which is secured to the top of the right-hand side of the DK-2, over the cell compartment of that instrument, and held in place by a screw, after boring and threading a 1/4-20 hole in the metal plate which surrounds the DK-2 cell compartment. The platform itself is bored with a two-inch hole in a position directly in line with the microscope objective to permit light to be reflected upwards from the cell compartment to the optical system of the microscope.
Before attaching the microscope platform to the DK-2, the cell holder of the Spectrophotometer is removed, and substituted for it is a first-surface mirror mounted on an angle bracket at about 45 degrees to reflect light from the source directly upward toward the microscope. The mirror holder is centered on the pins which normally center the DK cell holder so that it may be replaced at any time in the same position. Initial angular adjustment of this mirror is quite critical and must be done by trial and error, after which it is cemented to its angle bracket. For convenience the mirror is on the "sample side" of the cell compartment.
For use, the DK is set on "Energy". Tungsten illumination is used and shutters leading to the detectors are closed. The shaft of the motor controlling the rotating mirrors is manually rotated to permit the beam of light to pass through the sample side of the cell compartment, where it may strike the substituted first-surface mirror. Wave-lengths may then be dialed in as required, in the usual manner, and slit widths manually set in accordance with intensities or band widths desired. With a 10x ocular on the microscope and a 48 mm. objective (as recommended in the earlier papers) no substage condenser is used. Illumination was demonstrated to be adequate in both intensity and area under these conditions, using slit widths of from 0.5 to 0.8 mm.
OPEN-FACED, SEMI-MICRO COLUMN CHROMATOGRAPHY — PRELIMINARY STUDY
John Davis, Oakland Police Department
(Note: Abstract submitted by Davis)
In this unscheduled paper Davis described a chromatographic method involving application of silica gel to ribbed glass plates instead of the usual flat-surfaced glass. He pointed out that by applying the gel suspension in a layer thick enough to cover the tops of the glass, drying it thoroughly, and then scraping away the excess down to the tops of the glass ribs, one obtains a series of vertical columns of silica gel, each separated by a glass barrier or rib. When utilized for "thin layer" work, such a technique results in separated components in band rather than spot form, but one in which comparisons are facilitated.
Glass being used is available both in "ground glass" finish and in the usual slick-surfaced transparent form. Of these, the ground or sandblasted type had certain advantages in that the silica gel could be more easily removed. Ribs on the glass are about 1/8 inch apart, and perhaps 1 mm. in height, permitting a large number of spots to be placed on an 8 x 8-inch plate. It was pointed out that various manufacturers produce a similar glass but the exact cross-sectional appearance of the ribs does vary in makes. That preferred for the work is one in which the ribs have a wave form rather than being constituted of a "toothed" form made of triangular-shaped ribs.
Among the advantages of this method is the ease with which, after detection of spots by appropriate spraying, the silica gel in any one column which does not represent a resolved component may be quickly scraped away with a toothpick, leaving the component area intact on the plate, after which contact photographic prints can easily be made of one or more columns on the plate, providing a graphic illustration of their positions.
Slides were shown illustrating the type of glass being used and a finished plate from one of the earlier test-runs conducted. One disadvantage to the method would be a possible failure to resolve two components as bands, which, if allowed to spread laterally to form spots, might be more distinctly separated in a given solvent-rise.
SOME NEW EQUIPMENT FOB THE HANDLING AND TRANSPORTATION OF EXPLOSIVE DEVICES
D.M. Lucas, Attorney General Laboratory, Toronto, Canada
Mr. Lucas described the development and construction of a bomb handling shield device, equipment and a transportation truck. The materials for the shield cost $955, the tools $436 and the modified truck $5800.
The purpose of the shield is to allow the operator to approach safely an infernal device and either explode it at location or manipulate the device with various attachments on long poles from behind the shield and move it to where it can be safely loaded onto the transportation truck. The shield is constructed in a manner to allow collapsing to a package weighing 185 pounds and measuring 22 x 28 x 55 inches. It is made of two layers of 1/8 inch ST6 Aluminum alloy separated by a 1-3/8 inch air gap. The shield has a 90° angle front wedge-shape with an additional 15° bend about half-way back. It is attached at a 45° angle to a wooden platform on 3-1/2 inch castors with a sliding extension at the rear. A 3/8 x 3 x 8 inch lucite window is provided in the front, 17 inches above the base. Two holes, 22 inches above the base and 6 inches from the sides, allow the insertion and manipulation of poles.
Various manipulating devices were shown and described. These included a fishing pole modified to drop a noose around a package and pull the noose tight and two sections of 6-foot 1-inch I.D. 65ST6 aluminum pipe (tubing and fiberglass too flexible). These form a 12-foot pole to which is attached a "Fit-On Pole Head" made by Kearney Hi-line Tools and which allows the rapid attachment of different heads. The heads are fitted with "Fit-On Insulator Tongs" which allow the heads to be opened and closed by rotating the pole with one hand, thus grasping infernal device packages, The heads were of different types and designs to pick up various sizes and shapes.
The specially modified truck for transportation has a flat bed of 3/4 inch steel and a 14 x 6 x 2 foot box made of 10 gauge steel. At the front of the box is a 6 x 8 foot deflection plate of 1/2 inch steel extending from the top of the cab to the truck bed between which are storage compartments. The heart of the truck is a drum 48 inches high and 42 inches in diameter, made of 3/4 inch cold rolled steel with a dish-shaped bottom of 1 inch boiler head steel. The drum sits directly over the rear axles, contains 6 to 8 inches of sand and is surrounded by sand and sandbags. Explosives are placed in the drum with a net on the end of a boom attached to the truck and operated from the opposite side of the truck. It positions itself automatically over the center of the drum.
Mr. Lucas pointed out that, in Ontario, arrangements have also been made with the Department of Highways to have available an ordinary 3-ton dump truck along with sand and sandbags. A cavity in the sand about 3 to 4 feet in diameter and 8 to 10 feet deep (surrounded with sandbags) will successfully contain the explosion of 6 sticks of 40% dynamite with no damage to the truck.
THE IDENTIFICATION OF HEROIN IN THE PRESENCE OF MONOACETYLMORPHINE
John I. Thornton (and Duayne Dillon), Contra Costa County Sheriff's Department
Monoacetylmorphine (MAM) may be present in heroin from either incomplete acetylation of morphine or from the hydrolysis of heroin after manufacture. Of the two isomers, only 0 MAM is at all stable.
The authors found that large quantities of MAM do not preclude the obtaining of characteristic heroin crystals with Fulton's mercuric iodide reagent and that MAM itself gives no characteristic crystals with this reagent. MAM will interfere in getting typical heroin U.V. data.
Thornton reported that rapid separation of heroin and MAM in evidence samples is accomplished by TLC previously described by them (See Seminar Abstracts for October, 1963).
It was the opinion of the authors that of the iodine-iodide reagents, the superior one for MAM is one in which the iodine-lodinde ratio is 1:1 (1% each in aqueous solution). With this, MAM gives needles and dendrites clearly distinguishable from heroin, morphine and codeine.
Thornton passed out a 3 page ditto handout covering the background information, experimental data and references.
FIRST YEAR PROGRESS REPORT ON SINGLE VEHICLE ACCIDENT STUDY
Allen Gilmore, Criminal Investigation and Identification Division, Calif. Dept. of Justice
Gilmore presented some of the background leading up to the special study which is being done in cooperation with the California Highway Patrol, Coroner's Association and the State Department of Public Health. The study includes 22 factors involving the driver, 9 factors regarding the vehicle, 6 factors of environment and 5 factors in regard to the accident (given that it is a single-car accident in which the driver was killed or died within 15 minutes) as well as blood analysis for alcohol, carbon monoxide and drugs.
Findings based on the partial analysis of the first 5 months have shown that carbon monoxide was not a problem except in perhaps one or two isolated cases.
Of 344 cases, 76.7% had alcohol, with most of them above .06%. In the 15-20 age group, 51.3% had alcohol. In the 27-31 age group, 92.31% had alcohol.
About 15% of the drivers are having heart attacks; all are above age 60. Only during the last six months has the drug study been rather extensive. About 10% are showing drug involvement. The most common class of drugs is barbiturates, and nearly always with alcohol.
The project will go another year, without the carbon monoxide, and will also include a pilot study on mechanical failure involvement in the 5 counties surrounding Sacramento.
SOME FORENSIC CONSIDERATIONS OF SHOTGUN WADS
Paul M. Dougherty, San Mateo County Sheriff's Office
Dougherty collected some 60 different wadding samples from various manufacturers. Some can be identified not only as to gauge, but also as to manufacturer and whether they are for handloads or for factory loads only.
Doughtery had displays of the waddings, but had no compilation of data at the time.
NEUTRON ACTIVATION ANALYSIS CHARACTERIZATION OF PAPER SAMPLES
Mrs. Dorothy Settle, General Atomics Division, San Diego
Mrs. Settle reported on neutron activation analysis of various rag content paper samples and 100% sulfite papers from different manufacturers, using techniques for both short and long lived isotopes. She found the same elements present in all samples. Results were too variable between different samples of the same type of paper to characterize. The results did indicate that activation analysis may not be of value in characterization of the type of paper, but it may be of value in helping to establish that a given sheet is from a particular batch of paper if examined by comparative quantitative analysis.
PRESENTATION OF NEUTRON ACTIVATION ANALYSIS DATA IN COURT: THE SAN MATEO PAINT CASE
Donald E. Bryan, General Atomics Division, San Diego
Discussed a burglary case in which the suspect was picked up at the scene, but not in the act. A lug wrench recovered at the scene bore blue paint and brown paint. Microscopic examination of the paint smears on the lug wrench showed them to be similar to brown paint from the jimmied door and blue paint from the suspect's automobile.
Transfer and standard paints were examined by activation analysis. Five elements in the same relative concentrations were found in the blue paint and 7 elements and concentrations in the brown paints. A 99.98% probability that the blue paints were identical and a 99.99% probability that the brown paints were identical, were given in testimony. These figures were based on:
- Analysis of 10 other blue automobile paints; some, if not all, could be differentiated by microscopic comparison of color. Five were from the same manufacturer. The 10 were shown to be different by activation analysis.
- If two paints of similar color showed the same single element within 30% concentration, a figure of 1 chance in 5 that they did not come from the same source was chosen (a probability of .8 of being from the same source).
- If n number of elements are found in the same concentrations (within 30%), then the probability of them being from different sources is (1/5)ⁿ.
- With the blue paint there was (1/5)⁵ probability that, if the 5 elements agreed qualitatively and quantitatively, they would be from different origins — or 99.98% probability that they are the same.
Bryan stated that they did not want to give probability figures, but did so on the insistence of the District Attorney's Office. They felt the figures were conservative and that the values were more valid than some people thought.
An extensive discussion followed this presentation, which centered largely on the question of whether elemental content of paint is an independent variable the sufficiency of 10 paints being used to establish the probability figures and pointing out the need of a much more extensive activation analysis survey of paints.
ACTIVATION ANALYSIS OF THE OSWALD PARAFFIN CASTS
Donald E. Bryan, General Atomics Division, San Diego
Previously, Dr. Guinn reported that if the diphenylamine test had not been performed and if the rifle had been fired three times, it was quite possible that the fact that the person had fired the weapon could be determined by activation analysis for Ba and Sb on the person's hands and face. Also, even though the diphenylamine test has been run and the Ba essentially removed, the Sb would remain. (See previous abstracts - May, 1964).
The Dallas P.D. did perform the diphenylamine test. Oak Ridge (Tenn.) ran activation analysis on scrapings from the inside surface of the casts and later on the outside surface as a control. There was slightly less Ba and more Sb on the outside surface than on the inside. The results had to be considered inconclusive. The reasons for this occurence may have been due to contaminated paraffin (General Atomics has not, however, found Sb in standard paraffin) or casts that were improperly collected and handled for activation analysis.
NATURAL EXTRACTIVE FROM BLOOD
James W. Brackett, San Mateo County Coroner's Office
This paper dealt primarily with the identification or characterization of the naturally occurring extractives (primarily from the neutral fraction) obtained by extracting blood (without buffering) with chloroform (1:12), which extracts the phenolic acids with pK's of 10 to 10 and all lipid matter. The solvent equivalent of 2 ml of blood is dried down, taken up in ether, spotted and chromatographed (with cyclohexane-absolute alcohol?). The chromatograms are examined by U.V. and with a series of reagents, including N-chloramine test (see below). Spots were tentatively identified as lecithin, triglycerides and cholesterol ester, Rf .72-98, fluorescent; cholesterol, Rf .7; phospholipids, Rf .5, fluorescent; urea and creatinine, Rf .05 and bilirubin, Rf .00.
Of interest was a test reported by Brackett (that he called the N-chloramine test) in which the material is chlorinated on the plate. The excess chlorinating reagent is destroyed by spraying with a dilute solution of phenol in water and then over-sprayed with KI and starch solution to detect those substances that will N-chlorinate. He reported success with this test for substances such as amino acids, Doriden, Miltown, etc.
EXPERIMENTS ON FATIGUE OF DRIVERS
Allan Gilmore, Criminal Investigation and Identification Division, California Department of Justice
The study was done with the National Safety Council and a Nevada sports car club. One group of four drivers was tested during the day and four others at night after working all day. The drivers drove one course for twelve hours and were tested on another about every 3 hours.
The test driving course required only a few minutes and consisted of driving a winding path around pylons and through staggered gates in a descending alley to where there were about 4 inches of clearance; then into a garage, back out and retrace the course. The subjects were also given a series of visual tests including a flicker test (time required to read a statement flashed on a screen) and a glare recovery test (in a room with a headlight flashed on the screen) and the time required to read a lighted number just above the headlight).
Neither group showed any fatigue impairment by the tests, although, while in the sustained driving situation, they became irritable and sleepy, but not on the test course. Under emergency conditions, there can be an unusual emotional strain causing an expenditure of considerable energy without fatigue. This is important where an officer stops a drunk. The man may claim he was tired, not drunk. This doesn't bear out; he should be able to pull himself together even though he may be fatigued.
(Editor's Note; Nice try, CII. Things don't always work out in the way that is expected. The results are still worth reporting and discussing.)
- CLINKERS FROM HAY FIRES
Burd passed around a clinker recovered from a hay fire. Similar ones analyzed in the past were found to contain common earth elements present in plant materials. When large amounts of hay burn with very slow combustion on the inside, few, to many, clinkers are formed. Inexperienced arson investigators often think a fuse is involved.
- BRITISH 303 INCENDIARY MILITARY AMMUNITION
Cartridges were passed around. At first thought to be tracer ammo, they were identified as being incendiary, containing white phosphorous. This ammo had been involved in a forest fire in the Fresno area.
- BRITISH 303 TRACER MILITARY AMMUNITION
A San Bernardino area forest fire was established as having been caused by tracer ammunition. A Forest Service investigator answered an advertisement for British 303 military copper jacketed ammunition and received two boxes containing all tracer ammunition. The only warning label on the box read, "Keep out of reach of children". The source was VIC'S FOR GUNS 2413 D, Galveston, Texas.
- (FLASH PAPER)
Flash paper sold as a novelty and used as bookmaker markers. Practically pure nitrocellulose and easily and rapidly disposed of by burning. The bookies were charged with possession of explosives with felonious intent.
- (WATER SOLUBLE PAPER)
Also used by bookies. The paper thrown into water immediately turns to pulp. Apparently egg albumin sizing suspects also had dye in the water to prevent ink identification.
- RESEARCH REACTOR AT U.C., BERKELEY
A Triga III reactor will be available for use by the University, as well as by private industry and governmental laboratories. Technical details of availability not known at this time.