X-RAY DIFFRACTION ANALYSIS OF MICRO QUANTITIES OF CHEMICAL SUBSTANCES

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP78-03166A000700010001-1
• Release Decision: RIPPUB
• Original Classification: S
• Document Page Count: 72
• Document Creation Date: December 23, 2016
• Document Release Date: April 25, 2014
• Sequence Number: 1
• Publication Date: March 18, 1964
• Content Type: REPORT

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Dear Norb:
March 18, 1964
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Project No. 05-1158
Enclosed are three (3) copies of the modified report entitled "X-Ray
Diffraction Analysis of Micro Quantities of Chemical Substances"
which was carried out under program 05-1158. Jim and I have tried
as far as possible to comply with all of your questions and to include
other information to increase the value of the report. Bill has gone
through all of his data and made the necessary deletions and has
added information to enhance the report. I had gone over the report
and made modifications a number of times which we hope will satisfy
completely your requirements.
We would appreciate having you destroy the old copy and receiving
from you an acceptance of this report so that we may clear our files
as well as destroy records connected with the program. I hope that
everything is satisfactory.
Si erely,
' 7 -
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X-RAY DIFFRACTION ANALYSIS OF MICRO QUANTITIES
OF CHEMICAL SUBSTANCES
Project No. 1158-5
March 18, 1964
APPROVED:
.1Fleirer.
Prepared by: George
Bill
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I.
III.
TABLE OF CONTENTS
STATEMENT OF THE PROBLEM
SUMMARY AND CONCLUSIONS
EXPERIMENTAL PROCEDURES
Page
1
1
6
A.
X-Ray Diffraction Technique
6
B.
X-Ray Source
8
C.
Power Supply
9
D.
X-Ray Precautions
9
E.
Camera and Collimator
10
F.
Samples
13
G.
Film and Exposure
17
H.
Measurement of Apparent Atomic Spacing
18
I.
Intensity Measurement
20
J.
Termatrex System for
Filing
and Retrieving Data
22
K.
Termatrex System for
Data
23
IV.
DATA
25
V.
ANALYSIS OF DATA
25
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Table 1
Table 2
Table 3
Table 4
LIST OF TABLES
Apparent Atomic Spacing
d/n Ranges for Termatrex Cards Containin Powder Data 50X1
Comparison of Powder Diffraction Data for Germanium 50X1
Dioxide
Tabulation of Apparent Atomic Plane Spacings and Intensity
Ratios for the Diffraction Rings from Several Powdered
Samples
73.
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LIST OF FIGURES
Figure 1 Production of Diffraction Patterns by Powdered Samples
Figure 2 Diffraction of X-rays by Atoms in a Crystal Lattice -
Bragg's Law
Figure 3 Filtered Radiation
Figure 4 Details of Diffraction Micro Camera in Position next to
the X-ray Tube
Figure 5 Effect of Sample Size on Diffraction Ring Resolution
Figure 6 Diffraction Patterns from Microgram or Less Quantities
of Sample
Figure 7 The Effect of Particle Size
Figure 8 Densitometer
Figure 9 Representative Densitometer Scan of X-Ray Diffraction
Pattern of Powdered Uric Acid
Figure 10 Diffraction Patterns from Catalogue Compounds
Figure 11 Diffraction Patterns from Catalogue Compounds
Figure 12 Diffraction Patterns from Catalogue Compounds
Figure 13 Diffraction Patterns from Catalogue Compounds
Figure 14 Diffraction Patterns from Catalogue Compounds
Figure 15 Diffraction Patterns from Catalogue Compounds
Figure 16 Diffraction Patterns from Catalogue Compounds
Figure 17 Diffraction Patterns from Dilutions of Chemicals in
Corn Starch
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I. STATEMENT OF THE PROBLEM
The objective of this program was to develop a micro x-ray diffraction
procedure capable of identifying small quantities of chemicals. The work
was divided into three areas as follows:
A. To determine the feasibility of a micro x-ray diffraction
procedure to fingerprint materials in quantities considerably less than one
B. To determine from pure chemicals the limit of detectability
by micro x-ray diffraction and prepare a standard material catalog similar
to the ASTM x-ray powder data file.
C. Obtain x-ray diffraction data from chemicals contained on
paper directly and without previous chemical treatment.
II. SUMMARY AND CONCLUSIONS
The objectives in A and B above were successfully accomplished
during the course of this program. Our attempt to obtain micro diffraction
patterns directly from traces of chemicals on paper failed.
A. Feasibility of Micro X-Ray Diffraction
The feasibility of producing powder x-ray diffraction patterns
from small quantities of materials was established by first obtaining patterns
from milligram quantities and then reducing the sample size until patterns
were obtained from microgram quantities. Initially we used brass washers,
packing the powdered samples in the holesl. These holes ranged from 0. 35
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to 1.0 mm diameter. The length of the holes was about 0. 5 mm. Thus,
the volumes of the holes ranged from about 1. 8 x 10-5 to 3. 7 x 10-4 cc;
e.,i. the sample weights (for materials of specific gravity 2) ranged from
0.036 to 0. 75 milligram. Later, sample holders were made by punching
a hole with a sharp needle in a piece of lead foil. A typical hole produced
in this way would have a diameter of about 0. 1 mm and a length of about
0.08 mm or a volume of about 5 x 10-7 cc. If packed full of powder of
specific gravity 2, the hole would contain about 0.001 milligram (one microgram).
Difficulty was experienced in keeping the sample powder in place in the hole,
but was overcome by utilizing a thin film of ethyl cellulose evaporated from
1% solution. Figure 6 shows diffraction patterns from samples of one
microgram or less. These same patterns may be found among those in
Figures 10-16, where the sample sizes are much larger (one-tenth to one
milligram). The exposure time required to produce a diffraction pattern
ranges from 15 minutes to 16 hours.
Particle size and grinding have a pronounced effect on the diffraction
pattern obtained. No. 18 in Figure 11 is a print of a diffraction pattern obtained
from 0.003 milligram of material. There was very little of this material
available, and the sample was prepared without grinding. Note the streaks
and spots in the diffraction pattern which are due to non-uniformity in the
granule size. We have no satisfactory method of grinding such a small
sample. On the other hand, where ground material is available, we have
succeeded in obtaining recognizable patterns from less than one microgram
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of sample. Indeed, one-tenth microgram of ground uric acid produced a
recognizable pattern (No. A of Figure 6). The effect of grinding upon the
quality of diffraction pattern produced is illustrated by Figure 7. Too much
as well as too little grinding can be detrimental. Diffraction pattern No. 3
in Figure 10 was made from hemin as received. When this material was
ground, the diffraction pattern from the ground material showed no rings,
only a continuous blackening over the central half of the film. As a general
' rule, the sample powder as received should be used for the first trial.
The appearance of the diffraction pattern from an unground sample will
determine the extent of grinding required to produce a pattern with uniform
rings (Figure 7). The thickness of the sample can effect the resolution
displayed by the diffraction pattern. Figure 5 compares densitometer traces
of diffraction patterns made from samples of two different sizes. The
upper trace is from a sample 0. 7 mm thick, and the lower trace is from
a sample of the same material 0. 1 mm thick. Hence, the sample thickness
for optimum resolution should be less than 0. 7 mm. In the diffraction
patterns pictured in Figures 10-16, the average sample thickness is about
0. 5 mm.
B. Determination of Limits of Detectability and Cataloging of
Diffraction Patterns
For pure compounds of the types studied the limit of detectability
was in the 0. 1 to 1.0 microgram (0. 0001 to 0. 001 milligram) range. Figure 6
shows diffraction patterns obtained from samples in this range. In addition,
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No. 18 in Figure 11 was made using only 3 micrograms of sample and
Nos. 74 and 75 in Figure 16 were made using 16 microgram samples.
Attempts at producing diffraction patterns from less than 0.1 microgram
quantities were unsuccessful for dimethylglyoxime and 8-hydroxyquinoline.
Extreme difficulty was encountered in positioning the sample in the sample
holder. Also there was considerable difficulty in mounting and retaining
these samples in place in the sample holders.
The d/n values for 75 compounds are catalogued in Table 4. The
d/n values are listed in order of decreasing intensity in the manner of the
ASTM powder x-ray diffraction data. Figures 10 through 16 contain prints
of diffraction patterns for the compounds listed in Table 4. The prints do
not exhibit all the details present in the original negatives. The d/n values
were determined by utilizing magnesium oxide as an internal standard. An
internal standard is required, as the sample to film distance in the camera
is not repeatable precisely. The main diffraction ring from magnesium
oxide lies outside the rings from most organics (Figure 7). The amount of
magnesium oxide required may be inferred by reference to Figure 17.
Note that 10% magnesium oxide added to starch shows up quite clearly,
but 1% magnesium oxide is too faint for satisfactory measurement. Since
a suitable internal standard such as magnesium oxide must be added to the
samples, at least two diffraction patterns must be made from each material.
The first pattern should be made from the material alone to insure that no
details are obscured by the presence of the internal standard. Then a second
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pattern must be made after the addition of the internal standard to the sample,
and quite often two or more trials must be made both with and without the
internal standard. For the samples listed in Table 4 an average of 5 trials
each was required to obtain diffraction patterns suitable for determining din
values. Of the 75 compounds attempted, only one failed to produce d/n data
(sample SP-1110).
As a check on our d/n measurements, we obtained the powder diffraction
pattern from germanium dioxide (hexagonal). Patterns were produced from
each of six samples ranging from 0. 3 to 0. 9 mg. each. The average values
of d/n determined from these diffraction patterns are in good agreement with
values given as standard by the National Bureau of Standards. The NBS
sample size was at lest 0.1 g.
C. Diffraction from Chemicals Contained on Paper
Patterns Nos. 14, 15, and 16 in Figure 12 are from three
kinds of paper. The samples were made up of three to five disks punched
from the paper. These paper disks were retained in the sample holder in
place of a brass or lead washer. Note the intense rings which are due probably
to cellulose. The Beverly Bond and sulfite papers exhibit rings not found in
the filter paper (Table 4). Disks punched from Beverly Bond supplied to us
with a coating of dimethylglyoxime failed to produce any diffraction rings other
than those of the plain paper. Increasing the exposure produced only a general
blackening of the film. The diffraction pattern from the paper was simply too
strong to permit the pattern from any trace material to show up.
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To determine the amount of material which might be detected in the
presence of cellulose (paper), several dilutions of chemicals in corn starch
were used for making diffraction patterns. Corn starch has a simple two
ring pattern similar to paper (No. 29 of Figure-1-3). Representative diffraction
patterns from dilutions in starch are given in Figure 17. However, the fine
details present in the original negatives again are lost in the reproduction.
The diffraction rings from the ten percent concentrations of aspirin and
sulfaguanidine are faintly visible. In the one percent concentrations the
diffraction patterns of aspirin and sulfagua.nidine are lost completely in the
starch pattern. Note that the three percent concentration of uric acid produces
a faintly visible pattern. Since these starch dilution diffraction patterns imply
at least a three to ten percent concentration for detection by this method,
the attempt at detecting chemicals on paper was discontinued.
III. EXPERIMENTAL PROCEDURES
A. X-Ray Diffraction Technique
When x-rays impinge upon matter, a portion of the x-rays is
scattered by the atoms of the substance. If the atoms are arranged in an
orderly manner (crystalline substances), then the scattered rays from different
atoms will cancel and reinforce each other in a regular pattern. In the usual
diffraction experiment, the x-ray beam is collimated into a narrow pencil of
rays by pinholes in lead (Figure 1). The collimated narrow beam then traverses
the sample of crystalline material. The sample may be a single crystal, or as
pictured in Figure 1, a powder made up of tiny crystalline granules. The
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scattered or diffracted x-rays impinge upon a photographic film. For a
single crystal aligned with one of the principal axes parallel to the collimated
x-ray beam, the diffraction pattern recorded by the film will be a system of
spots or streaks distributed symmetrically about the point of intersection
of the undeviated beam with the film. For practical reasons, the direct beam
of x-rays is not allowed to strike the film. The exposure produced by the
direct beam and the fluorescent x-rays from silver, bromine, and iodine
atoms would be spread over a large fraction of the central portion of the
film. The direct beam is stopped by a lead cup or allowed to pass cleanly
through a hole punched in the film. When the sample is powdered, the
random orientation of the crystalline granules produces a series of concentric
rings on the photographic film. If the powder is uniform and of the proper
grain size, the rings will be of uniform intensity and width. If the powder
contains granules considerably larger than optimum, then there will be spots
or streaks mixed in the rings. If the powder is too fine, the rings will be
weak and diffuse or may disappear altogether. For examples of powder
diffraction patterns see Figures 10-16.
The interpretation of the diffraction pattern may be accomplished with
the aid of Figure 2. The small circles represent a series of atoms in planes
of spacing, d. The planes make an angle 0 with the incident x-rays, lines AB
and DF. It has been found experimentally, that the diffracted x-ray beam behaves
as though the x-rays are reflected from a plane mirror, but only at certain angles;
i. e. , the angle of diffraction (reflection) equals the angle of incidence. 3
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Consider then, the scattered x-ray beam defined by lines BC and
FH also making an angle 0 with the atomic planes; hence the diffracted ray
makes an angle 20 with the incident ray. Note that the ray DFH is longer
than ABC by the amount of EFG; i. e., the point H lags behing point C by
the distance EFG. The waves at points C and H, however, will be in phase
and reinforce each other if EFG is an integral number, n, of x-ray
wavelengths, X; i. e.,
nX. EFG.
Now EF FG BF sin 0, but BF tr. d, the atomic plane spacing. Thus,
nX 2d sin 0. This is the Bragg law of x-ray diffraction. 3, 4 The angle 0
may be determined from the distance, r, of the diffraction spot or ring from
the central point and D, the distance from the sample to the film (Figure 1).
In powder diffraction patterns, the diameter of the rings (2r)ds measured
readily. Distance,. D, is determined most accurately by mixing some
material of known atomic spacing, d, with the unknown.
B. X-Ray Source
The wavelength X is determined by the anode or target material
in the x-ray tube. Copper targets are widely used for x-ray diffraction
experiments. The x-radiation from a copper target is diagrammed in Figure 3. 4, 5
The characteristic copper radiations, Ka and Ki3, are superimposed on a
continuous background radiation. To avoid a multiplicity of spots or rings
arising from all the different wavelengths present in the output of the x-ray
tube, it would be desirable to limit the x-rays to the Ka. wavelength. This is
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accomplished readily for a copper target tube by placing a thin sheet of
nickel between the x-ray tube and the pinhole collimator (Figure 1). The
absorption of nickel is represented by the dashed curve of Figure 3. Therefore
the Kp and the shorter continuous wavelengths from copper are attenuated
greatly with respect to the Ka radiation. In general, a filter of one atomic
number less than the atomic number of the x-ray target material will limit
the radiation to the Ka wavelength region of the target.
C. Power Supply
In this laboratory, the source of x-rays for diffraction studies
is a General Electric Type CA-7 copper target tube. This tube is mounted
horizontally above a spectrogoniometer circle on a G. E. Type XRD-5 table.
The x-ray tube window opposite the spectrogoniometer faces a camera track.
The tube is powered by the G. E. Type XRD-5 high-voltage supply. This
supply provides up to 50 kilovolts peak at 50 milliamperes. The Type
CA-7 tube is limited to 35 kv and 16 ma. The XRD-5 power supply provides
continuous voltage adjustment and four present current adjustments.
D. X-Ray Precautions
The x-ray diffraction apparatus is. maintained and operated in
accordance with accepted practice for low-voltage x-ray generators. 6 The
diffraction unit is considered "ray proof" by the manufacturer. However,
in this laboratory a vertical shield of about 1/16 inch thick lead sheet is
placed always about the target end of the x-ray tube and the diffraction camera.
This shielding is kept in place even when adjustments to the apparatus must be
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made while the x-rays are "on." The fingers are kept as far away as possible
from the x-ray window or port. Our fluorescent screen used for location of
the x-ray beam is always handled with pliers or tongs. The beam of x-rays
from a diffraction tube is small in area but intense enough at the window to
inflict serious burns to the fingers of a careless operators A small hole was
cut in our vertical lead sheet surrounding the rear of the camera to permit
viewing the fluorescent screen (No. 7 in Figure 4) utilized in the alignment
procedure described in the following section. Whenever an exposure was in
progress a horizontal sheet of lead was placed over the apparatus.
E. Camera and Collimators
A Philips Micro Camera7 was purchased by this project.
Figure 4 shows this camera in position next to the x-ray tube. This camera
consists of an airtight cylindrical body (No. 8 in Figure 4), which may be
evacuated or filled with hydrogen or helium as required. The front of the
body is removable and secured to the rest of the body by a threaded clamping
ring (No. 9 of Figure 4). The pinhole collimator (No. 2 of Figure 4) is held
in a hole by the threaded retainer (No. 1 of Figure 4). Hence, collimators
may be changed readily. A nickel foil filter, is taped usually over the hole
in the collimator retainer. Initial work was done using a collimator, consisting
of two lead disks with 0.35 mm holes. After gaining sufficient experience
with the 0.35 mm diameter collimator, we changed to a lead glass capillary
of 0.08 mm diameter. This smaller bore collimator produces diffraction
patterns of greater resolution at the expense of increased exposure times.
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The sample support may be moved laterally to center the sample with the
ED axis of the pinholes. The film (No. 5 of Figure 4) is held by a clip to the
film support (No. 6 of Figure 4) which plugs into .a socket in the camera body.
A fluorescent screen backed by lead glass (No. 7 of Figure 4) which plugs
into a socket in the camera body is provided for precise alignment of the
collimator with the x-ray beam. The assembled camera is held in a holder
clamped to the camera track. The camera holder is adaptable for use with
diffraction apparatus made by at least three manufacturers: Philips Electronic
Instruments, General Electric X-Ray Corp., and Picker X-Ray Corp. The
camera may be removed from and replaced in the holder without disturbing
the alignment.
The alignment of the camera with the x-ray beam is a very tedious
procedure for the tiny collimators used. The collimator itself should be
removed. The retaining ring should be replaced. The camera is placed
in the support on the track. The x-rays are turned on. The track and
support then are adjusted to yield the greatest x-ray intensity through the
camera as evidenced by the spot of light on the fluorescent screen at the
rear of the camera. The camera is then removed from the support taking
care not to disturb the adjustments. The largest collimator (0.35 mm) is
installed in the camera. The camera is returned to its support. The intensity
of the spot of light produced by the x-rays in the fluorescent screen is checked.
A magnifier is very, helpful to observe the spot on the fluorescent screen.
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The camera is removed again from the support and the 0.35 mm collimator
replaced with the 80 micron collimator (marked '14"). At this point the room
should be darkened to facilitate viewing the spot of light on the screen. The
aiming of the camera should be checked carefully. The camera is ready now
for making diffraction patterns as outlined below.
The rings of the pattern should be uniform in all directions. The
orientation of the film in the camera should be marked by cutting one corner.
If the resulting pattern is non-uniform in intensity, the tilt of the camera
with respect to the x-ray beam can be ascertained by inspection. The
aiming of the camera should be altered as indicated. Further exposures
should be made until uniformity of pattern is achieved. The collimators
should last indefinitely. Those with pinholes in lead may be cleaned with
suitable solvent (acetone). Care must be taken not to enlarge the lead
pinholes with wire or other hard material. The space between the lead
disks is much larger in diameter than the pinholes to provide a trap for
debris. This debris is removed effectively from the x-ray beam. The lead
glass capillary pinholes supplied by Philips with the camera are cleaned with
a fine wire (tungsten: 0. 001 - 0. 003 inch diameter). Solvents such as acetone
must not be used, since the glass capillary appears to be retained in the
brass body with household cement (Duca). The lead glass capillary can be
contaminated easily or stopped up. Particles adhering to the edge of the
capillary next to the sample can produce diffraction patterns also. The sample
end of the capillary is examined best with an ordinary microscope at 20-100 power.
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F. Samples
To insert a sample, the camera is removed from the holder and
opened at the locking ring. The powdered samples are packed in small
washers (No. 4 of Figure 4). These washers are made of brassl or lead
and are 1/4" in diameter. The brass washers are about 1. 5 mm thick and
have holes ranging from 0. 35 to 1.0 mm diameter. The holes are funnel
shaped on one side to facilitate filling. No difficulty was encountered
in filling the holes in the brass washers. The washer was placed with the
funnel end of the hole upward on a hard flat surface, preferably a glass plate.
A small spatula was used to place some powder over the hole. A rod of the
same diameter as the hole or slightly smaller was used to push the powder
into the hole, and pack it down. The cleaned shank end of a drill of the
proper diameter is suitable for this purpose. Powder was packed into the
hole until it filled to the start of the funnel. Hand pressure only was used
to pack the material in the hole. The lead washers are about 0.07 mm thick.
Holes are punched in the lead with a sharp needle and have diameters of 0. 1 mm
Or less. Such holes (0.1 mm diameter by 0.07 mm long) will hold about one
microgram (0.001 milligram) of material. Usually powders may be packed
in the brass washers without a binder. Since the intensity of the diffracted
x-rays depends on the quantity of sample, the brass washers usually are
used when sufficient sample is available. Note that a compound containing lead
or other good absorber may require many hours of exposure when packed in
a brass washer. The lead washers are used to hold microgram samples.
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Several
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Several compounds have been studied using the very small samples
(about 0.001 milligram) and are listed in Figure 6. After filling, the
sample-holding washer was positioned in the camera with the aid of a
microscope. The entire front of the camera was placed on the stage of a
microscope with the sample holder up. The camera front was positioned
so that the collimator was centered in the cross hairs of the microscope
ocular. The filled sample washer was put in place, and the holder was
moved with respect to the camera front to align the sample with the cross
hairs to be sure the sample was on the axis of the pinhole collimator. The
brass washers may be cleaned and reused.
The use of lead sample washers is difficult to describe. The lead
washers were punched from lead foil 0.003 inches thick (the backing from
Rinn dental x-ray film) with an ordinary paper punch (1/4 inch diameter).
Several disks were stacked together in a 1/4 inch hole drilled in a metal
plate (about 1/8 inch thick). A brass sample washer was placed in the hole
on top of the lead disks. Using the hole in the brass washer as a guide, a
sharp needle was stuck through the stack of disks. The point of the needle
was allowed just to penetrate the bottom disk. Since the needle tip was
tapered, the holes in the lead disks were graduated in size. The proper
size hole then could be selected to fit the amount of sample. The lead
washer was placed under either a stereo or regular microscope. A drop
of ethyl cellulose solution which just covered the entire washer was placed
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on the washer. The ethyl cellulose was dissolved in ethylene dichloride to
give about one percent solution. Both the ethyl cellulose and ethylene
dichloride were technical grade. When the ethylene dichloride had evaporated,
a thin film of ethyl cellulose was left across the hole. As the last bit of
ethylene dichloride evaporated, the film was examined with 40X to 100X
magnification to make sure the film was continuous across the hole. The
sample powder was placed then on the just dried ethyl cellulose film.
Working under the microscope, the sample was transfered using a needle.
After filling with sample, the lead washers were handled in the same manner
as the brass ones. The lead washers were discarded after use.
The thickening of the sample in a brass washer can become too
great. Figure 5 shows the rather interesting comparison of two different
diffraction patterns for diformylbenzidine. The actual comparison is of
the densitometer scans of the films. Curve A is a portion of the scan of
a pattern made from a large sample. Note the blunted appearance of the
two peaks. Curve B is a portion of the scan of a pattern made from a much
smaller sample. Note that the left peak is resolved actually into two peaks;
while the right peak is much sharper than in Curve A. The crucial dimension
of the sample is the thickness, for Curve A is 0. 7 mm thick and for Curve
B is only 0. 1 mm thick. In other words, the sample thickness for Curve B
is on the order of the size of the x-ray beam (0. 08 mm diameter).
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In the same manner, the diffraction patterns reproduced in Figure 7
illustrate the effect of particle size. No. 1 in the first row of Figure 7 was
made with the powdered sample as received. Notice the streaks and spots.
The second photograph represents the effect of grinding the sample in a
small agate 40 mm diameter mortar and pestle. The rings are fairly
uniform now but still exhibit a granular appearance. The last picture in
the first row exhibits very uniform rings as a result of continued grinding.
At this stage magnesium oxide (for use as an internal standard) was added
and ground together with the sample (No. 4 of Figure 7). The final print
shows the improvement produced by still more grinding of the sample plus
magnesium oxide mixture. Very uniform rings make the scanning with the
microdensitometer much easier. Furthermore, the diameters of the rings
can be measured more precisely when these rings are uniform. After use,
the agate mortar and pestle may be cleaned with nitric or chromic acid.
The size of a sample and amount of grinding necessary must be
determined by trial and error. Often three trials are required. In most
cases the first trial should utilize the sample powder as is. If sufficient
material is on hand, a brass washer should be used as the holder. Subsequent
trials may require much grinding and also require a very small sample held
in a pinhole in a lead foil washer. However, the first trial is made almost
always with a large sample without grinding.
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rc3
Lri
I
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Loly y 1 l/1
G. Film and Exposure
The camera is carried into a darkroom for film loading. The
size of film required is about 35 by 40 mm. - We have used industrial x-ray
film (Ilford Type G and Eastman Kodak Type KK) and dental film (Rinn DC-1).
The dental films are cut already to size. A hole is punched in the film with
a punch supplied with the camera. The film is clipped to the film support
No. 6 of Figure 4) with the hole in the film centered on the hole in the support.
The support is plugged in place and the front secured by the clamp ring (No. 9
of Figure 4). The camera is ready now for placement in the holder next to
the x-ray tube.
Exposure may require as little as 15 minutes when the 0.35 mm
collimator is in place, or as long as 16 hours with the 0.08 mm collimator.
Films are developed in G. E. Supermix x-ray developer for 2-4 minutes,
rinsed briefly in plain water, and fixed for 10 minutes in G. E. Supermix
x-ray fixer and hardener. Following a 10 minute wash, the films are dipped
in photo detergent and dried in air at room temperature. Representative
diffraction patterns are shown by Figures 10-16. The weight of and exposure
time for each sample are listed. Over 600 negatives have been made during
the development of this method. This large number of trials has been necessary
for the determination of the optimum exposure time, sample size, film type,
and even for the proper alignment of the x-ray collimator. As stated before,
2 to 5 exposures are required usually to determine the optimum conditions
for producing a satisfactory diffraction pattern from a new compound.
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r
L?opy r 01
H. Measurement of Apparent Atomic Spacing
Since we usually do not know either the order, n, or the atomic
spacing, d, for a diffraction ring, the diffraction rings from a particular
material are simply catalogued in terms of d/n, an apparent atomic spacing.
Rewriting the Bragg equation (from Section III - A)
d _ X
n2 sin 0
But tan 20 r/D (Figure 1)
Hence
20 arctan ?
D
X
'2 sin arctan (r/D)
2
Since the values of d/n are determined repeatedly for many
diffraction patterns, it is convenient to calculate d/n for the range of r/D
values possible in a particular camera. From an accurate plot, one can
then find d/n very readily.
Table 1 lists the d/n values for diffraction angles (20) from
4? to 45?. This table is computed for the average copper Ka radiation
(1. 5418 Angstrom units). Now d/n values can be determined readily simply
by measuring the diameters of the diffraction rings on the film. The sample-
to-film distance (approximately 15 mm) can be determined by measurement
or from the diameter of a ring produced by an internal standard included with
the sample. Magnesium oxide is a good internal standard since it produces a
ring of large diameter which lies outside nearly all rings produced by the organics.
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E
CI
This magnesium oxide ring has a d/n value of 2.10, or an r/D value of 0.935.
Hence, the sample-to-film distance, D, equals the radius, r, of this large
magnesium oxide ring divided by 0.935. The lead washers used for microgram
samples also produce a large diameter ring which may be used as an internal
standard (No. 77 of Figure 16). This lead ring has a d/n value of Z. 47.
As an internal standard, magnesium oxide has the drawback of being less
transparent to the x-rays used (Copper Ka) than the organics being studied.
The absorption of x-rays is proportional to the atomic number. Since lithium
has a lower atomic number than magnesium, lithium carbonate was tried as
an internal standard. Unfortunately lithium carbonate produces rings which
fall in the same region as the organics (No. 64 in Figure 15).
The diameters of the diffraction rings can be measured directly
on the film with a ruler. However, we have found that this measurement can
be accomplished more precisely by using a magnified image of the rings. In
one method the diameters of the rings are measured on the densitometer
tracings (see following section). These traces present a magnified image
of the spacing of the rings along a diameter, and indicate the relative densities
of the rings as well. As an alternative the ring spacings are measured on a
projection comparator. The film is clamped between glass plates on a carriage
driven by a graduated lead screw. A magnified image of the film is projected
on a screen. The lead screw is turned by hand until the ring falls on a fiducial
mark on the screen. The position of the carriage can be read to 0.01 mm.
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CI
Two operators were able independently to make measurements of diffraction
ring diameters which were in agreement to within 1/2%. A short lead screw
at right angles to the measuring screw enables the diffraction pattern to be
set precisely so that the measurements of diameters are made along a diameter.
The d/n values for various compounds are tabulated in Table 4.
I. Intensity Measurement
Several factors determine the relative intensity of the diffraction
rings. Among these are the atomic number of the atoms involved, the
population of the planes producing the ring, and the number of possible
orientations of the crystal producing the same planar spacing. Furthermore,
other considerations being equal, the larger the diameter of a ring, the lower
the intensity, since the same quantity of x-rays is made to cover a larger
area. The intensity of the diffraction rings is determined with a densitometer.
Figure 8 is a schematic diagram of the densitometer. Light
from the concentrated filament lamp is collected by the condensing lens.
The lower microscope objective focuses the region of the condensing lens
onto the film emulsion. The glass jaw slit serves to limit the size of the
scanning spot while still providing background illumination for focusing the
system. The diffraction rings are usually so broad and diffuse compared
to the sharp, narrow line produced by the glass slit, that no benefit comes
from using this slit with the powder diffraction patterns. Usually, it is
removed for scanning powder patterns. The upper microscope objective
focuses the film emulsion on a metal jaw slit before the photo tube.
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u o p y 1 oI
The film is clamped between glass plates to hold it flat and in focus over the
entire length of scan. The amount of light reaching the photo tube is reduced
by the density or blackening of the particular area of the emulsion interposed
between the light source and phototube. The microscope objectives reduce
the size of the area scanned to microscopic proportions. Indeed, if the slit
is set fine enough, individual clumps or granules of the emulsion are
recognized in the output of the phototube. Usually the slit is set wide enough
that the granularity of the emulsion does not contribute to the signal.
Therefore the phototube current is reduced in proportion to the blackening
of the various rings. The blackening is taken as a measure of the intensity
of a diffraction ring. The phototube output is recorded on a continuous chart,
pen and ink recorder. The diffraction pattern is moved by a lead screw
driven by a synchronous motor. The chart paper moves at a much faster
rate. Hence, the diameters of the various rings are magnified by the ratio
of chart travel to film travel per unit time.
Figure 9 is a tracing of the densitometer scan of the diffraction
pattern from uric acid, No. 24 of Figure 11. The dark ring of the diffraction
pattern produces the peaks at about 7 mm from the center of the scan. A
hole is punched in the middle of the film to allow the direct beam of x-rays
to bypass the emulsion, preventing blotting out of the central portion of the
diffraction pattern. This hole is responsible for the two sharp peaks at the
center of the densitometer scan. This pattern does not have a magnesium
oxide ring since the ring lies outside the scanned area presented here. Relative
intensities as determined by the densitometer are listed in Table 4, along with
the apparent atomic spacings.
- 1 -
r?-?
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p y
J. Termatrex System for Filing and Retrieving Data
(Th The Termatrex system utilizes a square array of 10,000 hole
positions in a deck of thin plastic cards. The hole positions are assigned to
the items to be described, e. g., chemical compounds. Each card represents
one particular characteristic that several items have in common, e.g. ,
molecular weight. Hence, the hole positions for all compounds of one
molecular weight would be drilled out. Similarly, cards may be drilled
for other characteristics such as melting point, color, etc. One deck of
cards is required for every 10,000 items to be described. The deck will
consist of as many cards as are necessary to break down the data. The
operation of the system can best be explained in terms of an actual set of
cards, the Termatrex decks for searching the ASTM x-ray powder data.
There are about 150 cards divided into three decks. Deck A consists of
50 cards covering the d/n values from 1. 5 to 10.0 A. U. The range of
d/n values on one card varies from about 0. 1 A. U. for the low end to
1. 5 A. U. at the upper end. Deck B consists of 47 cards covering the same
d/n values, but the ranges in Deck B are displaced about one-half range
with respect to Deck A. Deck C consists of 52 cards covering the chemical
elements. Major elements such as aluminum, iron, oxygen, etc. , are
represented by individual cards. Less frequently occurring elements, such
as the rare earths, radioactive elements, noble metals, etc., are grouped
together on cards. There are also cards listing the minerals, hydrates, and
alloys. Oxygen and hydrogen are punched into colored transparent cards as
well as opaque cards.
-22-
11-t
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'17 p y I Ui. `-?
To use the system, one selects from either Deck A or Deck B
the cards which cover the d/n values obtained from the x-ray powder
diffraction pattern of an unknown substance. The selected cards are stacked
together on top of an illuminated viewing box. The cards must be in precise
register with the viewing box and with each other. Where a hole position is
drilled out in all cards on the viewer, light will, come through, of course.
If no holes light up, then the cards or cards covering the weakest diffracting
ring or rings can be removed. If too many holes are lighted, then pairs of
cards should be selected from both Decks A and B so that each pair covers
a narrower range of d/n. values. The viewing box is equipped with a coordinate
system for indexing the 10,000 positions. The "y" is read first and the "x"
second, both as two digits; e. g., 0000 would be the upper left starting position.
Termatrex has been set up so that the y axis is read first always. There is
an index supplied with the decks which lists the Termatrex coordinates,
substances, and ASTM file number. There are 5700 entries. Hence, the
holes in the Termatrex cards suggest ASTM file data which may be the same
substance as the unknown. If the chemical elements in the unknown have been
identified, then appropriate cards from Deck C may be added to the stack on
the viewer.
K. Termatrex System for Data
The Termatrex viewing box purchased on this program is equipped
to drill the Termatrex cards as well as search them. The Termatrex people
suggested we utilize the same cards as are used for the ASTM data. Hence,
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50X1
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we acquired blank decks A, B, and C, as described above. These decks are
obviously custom marked for the ASTM data. Our values tend to be higher
than those in the ASTM file (1. 5 - 10.0). We have few values less than 2. 5,
and we have many values between 5 and 6 where the ASTM data "thin out.
It was decided that our file should cover the range from 2. 5 to 12.0 rather
than from 1. 5 to 10.0 as for the ASTM data. Table 2 lists the Termatrex
card numbers and the corresponding d/n ranges. There were no cards
marked for the chemical elements, since most of our data concerned organics.
As an example of the method of drilling the Termatrex cards,
consider anthracene, the first entry in Table 4. Note that for anthracene we
have obtained one intense ring, and six rings of intensity considerably less
than the first ring. The data for the two weakest rings are dropped, leaving
five rings. In general, only five or six rings from one pattern are of sufficient
intensity to be considered. Indeed, the original ASTM file card sets contain
only three cards for each compound. The three strongest d/n values are used
to index the three cards. One card is printed for each of the three strongest
values. Using the Termatrex cards, we may select as many d/n values for
one compound as are useful. For anthracene, the following cards would be
drilled at the same coordinate: from Deck A of Table 2, green/57, orange/90,
green/90, green/15, and black/40; from Deck B of Table 2, green/50, orange/95,
green/80, green/10, and black/44. None of the blank Termatrex cards were
drilled.
-24-
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LLIuopy
V. DATA
Figure 6 shows x-ray diffraction patterns for several compounds
obtained from microgram (0.001 milligram) quantities of sample. The
microgram samples were prepared from ground material. One sample,
216-F1, produced a usable pattern from 0.003 mg of unground material.
A print of the diffraction pattern from this sample is given as No. 18 in
Figure 11.
Table 3 compares data obtained at with that published by the 50X1
Bureau of Standards2 on the compound germanium dioxide (hexagonal).
Table 4 catalogues the data obtained on about 75 materials during the course
of the program. The data in the table are tabulated for each entry using
the ASTM system. The apparent atomic spacings (d/n) are listed in order
of decreasing intensity. The data in Table 4 have been revised for this
report. In many cases the values listed are not the same as those listed
in previous reports. Some compounds were re-run several times to
obtain good patterns. Figures 10-16 are contact prints of diffraction
patterns. Figure 17 shows the diffraction patterns for several dilutions
of chemicals in corn starch.
VI. ANALYSIS OF DATA
Table 3 compares our data for a particular compound with the data
published as standard by the National Bureau of Standards. The NBS data
are obtained by a diffractometer and radiation counter from rather large samples.
-.25-
gEDEE7
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LL):: A 1L-, y ti -?
Our data are obtained photographically using very small samples, one milligram
or less. The compound chosen was germanium dioxide (hexagonal). This
compound was selected since it has no state of hydration and crystallizes in
only two systems, hexagonal and tetragonal. The tetragonal converts to the
more common hexagonal form upon heating. Note that our data agree within
1% with the NBS data except for our 4.27 and 1. 99 values. The 4.27 ring is
rather small in diameter. The larger d/n values actually are measured less
precisely than the small d/n values. For the 1. 99 value, the NBS data list
a very weak intensity. The general agreement of the two sets of data.
demonstrate that our "postage stamp" films present valid x-ray powder
diffraction patterns.
The most striking feature of the diffraction patterns printed in
Figures 10-16 is that no two are alike. At first glance, Nos. 14, 15, and
16 in Figure 11 appear the same. However, in the printing process some
detail is lost. These three patterns are made from different kinds of
paper. In Table 4 the differences are quite apparent. The cellulose rings
are present in each case plus other rings probably due to fillers or residues
from the manufacturing process. Even the pattern from dialysis tubing,
No. 17, contains most of the cellulose rings.
In Figure 12, patterns Nos. 31, 32, and 33 appear the same. Again
the data in Table 4 give significant differences among these patterns. Two
large rings are entirely absent in the reproduction of No. 32. Pattern No. 47
-26-
F'
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jkg Y /
in Figure 13 comes close to reproducing most of the rings present in the
negative. At least 15 rings may be counted on the negative, and most of
these are reproduced here.
Most of the negatives selected for reproduction were made from
sizable quantities of sample, i. e. , about one-tenth to one milligram.
However, No. 18 in Figure 11 is a print of a diffraction pattern made
using a sample of the order of 0. 003 milligram. There was very little
of this material available to us. Note the streaks and spots. These are
due to non-uniformity- in the granule size. We have no satisfactory method
of grinding such a small sample to uniform grain size. Where ground
material is available, we have succeeded in obtaining recognizable patterns
from less than 0. 001 milligram. Indeed, 0.0001 milligram of ground uric
acid produced a recognizable pattern (Figure 6).
LLD -27-
D,
, 1 r
F,
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I Ui `-?
OEO.RET
r/D
TABLE 1. APPARENT ATOMIC SPACING*
d/n r/D
d/n
0.075
O. 080
O. 085
O. 090
O. 095
O. 100
O. 105
O. 110
20. 612
19. 321
18. 194
17. 181
16. 284
15. 477
14. 746
14. 080
0.310
O. 320
O. 330
0. 340
0. 350
0. 360
0. 370
0. 380
5. 148
4. 999
4.858
4.726
4.601
4.485
4.374
4.269
O. 115
13. 475
O. 390
4. 170
O. 120
12. 915
O. 400
4. 077
O. 125
12. 352
0. 420
3. 904
O. 130
11.935
0. 440
3. 746
O. 135
11.502
0. 460
3. 604
0. 140
11. 092
O. 480
3. 474
O. 145
10. 716
0. 500
3. 356
O. 150
10. 366
0. 520
3. 246
O. 155
10. 036
0. 540
3. 146
O. 160
9. 729
0. 560
3. 054
O. 165
9. 438
0. 580
2. 968
O. 170
9. 168
0. 600
2. 888
O. 175
8.910
0.620
2. 814
O. 180
8. 670
0. 640
2. 745
O. 185
8. 441
0.660
2. 681
O. 190
8. 225
0.680
2. 620
O. 195
8. 007
0. 700
2. 564
0. 200
7. 823
0. 720
2.511
0.210
7. 462
0. 740
2.462
0. 220
7. 134
0. 760
2.415
0. 230
6. 834
0. 780
2.371
O. 240
6. 562
0. 800
2. 329
O. 250
6. 309
0. 850
2. 234
O. 260
6. 078
0. 900
2. 152
0. 270
5. 863
0. 950
2. 079
O. 280
5.666
1.000
2.014
0. 290
5.481
O. 300
5.308
*Apparent atomic spacing (d/n) for values of the tangent (r/D)
of the diffraction angle (20) from 4? to 45?. Radiation:
Copper Ka - 1.5418 Angstrom units.
arcR, ?Er.
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TABLE 2. d/n RANGES
CON TAININ
2014/04/25 : CIA-RDP78-03166A000700010001-1
0) ...dopy
FOR TERMATREX CARDS
I U.1.
POWDER DATA
DECK A
Card No.
d/n Range
Card No.
d/n Range
Yellow/22
Less than 2.500
Green/25
4. 200 - 4.299
53
2.500 - 2.569
II 35
4.300 - 4.399
It 58
2. 570 - 2. 639
I 45
4.400 - 4.499
66
2. 640 - 2. 709
It 57
4.500 - 4.649
72
2.710 - 2.779
11 72
4.650 - 4.799
80
2. 780 - 2. 849
11 90
4.800 - 4.999
11 87
2.850 - 2.919
94
2. 920 - 2.999
Purple/10
5.000 - 5.199
" 32
5. 200 - 5. 399
Black/02
3.000 - 3.059
It 50
5-400 - 5.599
it 10
3.060 - 3.139
11 71
5.600 - 5.799
II 17
3.140 - 3.209
92
5. 800 - 5. 999
II 24
3.210 - 3.279
it 32
3.280 - 3.359
Yellow/60
6.000 - 6.299
11 40
3.360 - 3.430
Orange/65
6.300 - 6.699
it 48
3.440 - 3.519
Sand/68
6. 700 - 6. 999
11 56
3.520 - 3.599
Orange/70
7.000 - 7.399
it 64
3.600 - 3.679
" 76
7. 400 - 7. 899
It 72
3.680 - 3.759
11 80
7.900 - 8.499
80
3.760 - 3.839
11 90
8.500 - 9.499
It 88
3.840 3.919
11 99
9.500 -10.499
u 96
3.920 3.999
Sand/10 10. 500 -11. 999
Green/05 4. 000 - 4. 099 White/20 12. 0 & Greater
" 15 4. 100 - 4. 199
DECK B
Card No.
d/n Range
Card No.
din Range
Yellow/51
" 54
II 62
11 69
11
75
tt 85
ii 92
11
99
2.460 - 2.529
2.530 - 2.599
2. 600 - 2. 669
2. 670 - 2;739
2. 740 - 2. 809
2. 810 - 2.879
2. 880 - 2. 949
2. 950 - 3. 019
Green/10
" 20
11 30
it 40
II 50
11 65
ii 80
11
99
4.050 - 4.149
4.150 - 4.249
4. 250 - 2. 349
4.350 - 4.449
4. 450 - 4. 569
4.570 - 4.719
4.720 - 4.899
4. 900 - 5.099
74.
'51
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- copy J of 4
TABLE 2. d/n RANGES FOR TERMATREX CARDS
CONTAINING POWDER DATA (Cont'd)
Card No. d/n Range
Black/06 3. 020 - 3. 099
3. 100 - 3. 169
3.170 - 3.239
3.240 - 3.319
3.320 - 3.399
3.400 - 3.479
3. 480 - 3. 559
3.560 - 3.639
3.640 - 3.719
3.720 - 3.799
3.800 - 3.879
3.880 - 3.959
3. 960 4. 049
11
14
II
21
It
28
11
36
H
44
II
52
1,
60
11
68
II
76
n
84
If
92
It
99
DECK B (Cont'd)
Card No. d/n Range
Purple/ 18
II 39
It 57
81
Purple/60
5. 100 - 5.299
5.300 - 5.499
5.500 - 5.699
5.
700
- 5.
899
5.
900
- 6.
149
"
64
6.150
- 6.499
If
67
6.500
- 6 849
69
6.850
- 7.199
Orange/75
7.200
- 7.599
78
7. 600
- 8. 199
85
8.200
- 8.999
It
95
9. 000
- 9. 999
Sand/05
10. 000
-11.199
r
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50X1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
0 y "-?
TABLE 3. COMPARISON OF OWDER DIFFRACTION DATA
FOR GERMANIUM DIOXIDE (HEXAGONAL) WITH NBS DATA
Data NBS Data
d/n
I/10
d/n
I/I0
10.83
97
6.82
44
4.61
12
4.27
72
4.32
21
4.00
10
3.78
28
3.41
100
3.429
100
3.00
24
2.73
56
2.496
11
2.36
30
2.366
22
2.27
16
2.283
13
2.16
26
2.159
18
1.99
15
2.018
02
1.88
34
1.884
08
1.870
14
Note: data taken from six samples ranging from
0.3 to 0.9 mg. The NBS data are taken on 0.1 g or
larger samples. 2
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50X1
50X1
50X1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES
The upper row of figures in each case is apparent spacing (d/n). The lower
row of figures is the intensity ratio, I/I0, taking the most intense ring as I.
Anthracene
4. 54
1.00
9. 08
0.42
4. 83
0.35
4. 14
0.32
3.43
0.29
3. 53
0.20
3. 02
O. 19
Ethyl Cellulose
10.50
7.95
4.41
1.00
0.98
0.79
Hemin
8.98
5.32
4.23
3.71
1. 00
0. 92
0. 82
0. 75
Disodium EDTA
Calcium
10.33
8. 19
17.90
5.77
5. 12
1. 00
0. 88
0. 87
0. 77
0. 75
Carbanthrene
Violet
12. 23
7. 97
3. 86
1.00
0.99
0.60
Dis odium EDTA
Zinc
6. 33
8. 98
5.00
12. 51
4.30
3.69
3.24
1. 00
0. 95
0.90
0. 88
0. 80
0. 75
0. 70
Disodium EDTA
4.98
3.44
3. 10
4.27
7.91
1. 00
0. 96
0. 93
0. 92
0. 83
Disodium EDTA
Magnesium
6.28
5. 16
4.38
11.56
3.74
3.52
1.00
O. 69
0.62
0. 60
0.60
0.60
Magnesium Oxide
4.64
2.10
6.51
2.43
2.32
1.85
1.94
1.00
0. 83
0. 82
0. 45
0. 34
0.22
0. 15
8-Hydroxyquinoline
6. 16
3. 75
3. 46
3. 17
9. 62
4. 55
1.00
0.89
0.84
0.81
0.81
Tetrasodium EDTA
12. 30
7. 44
5. 53
3. 70
4. 76
3. 28
1.00
0.61
0.59
0.53
0.51
0.39
Isopropyl Jade
Green
13. 88
8. 65
4. 48
5. 94
3. 51
3. 04
2. 53
1. 00
0. 99
0. 92
0. 91
0. 87
0.66
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25 : CIA-RDP78-03166A000700010001-1
I.+ \ I upy I vi
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Cont'd)
Paper 3. 76 4.02 5.49 3.01 2.48 2.26 6.88
(Beverly Bond) 1.00 0.94 0.80 0.49 0.49 0.45
Whatrnan No. 2
3. 78 4. 17 5. 50 2. 53
3. 07
2. 27
2. 11
Filter Paper
1. 00 0. 76 0. 76 0.45
0.40
Sulfite Paper
3. 87 4. 24 5. 38 6.61
2. 51
3. 64
2. 25
1. 00 O. 85 O. 85 O. 64
O. 50
O. 41
0. 28
Dialysis Tubing
4. 19 8. 56 3.09 2. 52
2. 18
1. 00 0. 85 0.48 0. 32
0.23
216 F-1
4.65 14. 59 5. 73 3. 95
7. 05
3. 29
1.00 0.88 0.65 0.65
0.43
0.35
Sudan III CI 248
6. 55 3. 34 12. 88 4. 85
7. 46
3. 54
4. 33
1. 00 0. 78 0.69 0.62
0.61
0.60
0. 57
5.62 4.03 10.97 3.10
0. 56 0. 56 0. 52 0.48
Mylar
8.41 5.34 3.49 2.68
1.00 0.63 0.29 0.21
Uric Acid
3.08 3. 17 3. 86 2. 47
2. 53
5.62
6. 56
1.00 0.83 0.68 0.66
0.53
0.43
0.40
4.89 5.21 4.47 2.86 2.61 2.28 2.23
0.40 O. 34 O. 30 0.28 O. 28 0.28 0.28
2. 80 2. 72 2. 05 3. 38 10.46
0.23
O. 21
0.21
O. 17
O. 13
Sulfadiazine
5. 32
6. 78
4. 27
4.09
11.60
3. 79
3.36
1. 00
0. 96
O. 95
0. 86
O. 77
0. 55
Sulfapyridine
5.57
3.68
7.37
4.42
11.10
2.98
2.87
1. 00
0. 81
O. 74
0.66
O. 55
O. 30
O. 27
Versene
3.04
4. 21
3.38
4. 94
3. 89
7. 80
6. 16
1. 00
0. 96
0. 96
0. 92
0. 90
0. 88
--
Corn Starch
5.65
7.68
4.94
3.77
1.00
0.92
0.84
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Contrd)
Formvar
Triphenylphosphate
Talca
4. 74
1.00
8. 09
1.00
8.25
1.00
8. 77
0.80
5. 40
0.96
5.65
0.90
3. 96
0.92
Talcb
9. 10
4. 86
2. 77
1. 00
0. 92
0. 80
Talcc
8.72
5.61
1.00
0.90
Talcd
8. 66
5. 34
1.00
0.79
Dimethylglyoxime
5.77
5.06
3.60
1.00
0.97
0.70
Pyrazalone
4. 32 4. 63 6. 68 3. 75
0.91 0.90 0. 77
2. 59
0. 72
3.29 3.43 2.56 6.34
0. 55 0.49 0.34 0.27
2.91 10.93 2.33 2.42 2.14
O. 18 O. 15 O. 14 O. 13 O. 10
4.11 4.51 3.49 3.61 3.35 7.72 3,17
1.00 0. 72 O. 55 0. 48 0. 37 0. 36 0. 30
6. 52 4. 83 6. 95 9.06 5. 97 5.22
0.27 0.27 O. 21 O. 18 O. 15 O. 15
5.53 2.63
0.12
Paraffin 4.09 3.66 16.34 11.42 7.92 2.94 2.47
1. 00 0. 97 0, 78 0. 63 0.63 0. 22 0. 19
Diacetyl Benzidine 4. 74 7. 39 4. 45 3. 73 4. 00 6. 24 10. 19
1.00 0. 87 0. 55 0. 45 0.40 0. 35 O. 30
5.68 3.33 2.71
0.25 0.20,.--
Aspirin
9.11 11.34 4.51 5.64 2.62 3.28 3.41 4.25
1.00 0.85 0.82 0.51 0.42 0.40 0.38 0.37
3.12 3.91 4.96 2.90 2.44 2.18
O. 36 O. 35 O. 34 0.20 O. 17 O. 14
a - Penaten - German b - Nivea - German
c - Creta Gallica - French d - PhanThom - Vietnam
rl
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
opy 1- 01 `-*
EE5RET
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Contrd)
Sulfaguanidine
6.23 4.33 4.05 5.28 3.63
1. 00 0. 94 0. 74 0. 58 0.49
2.84 2.60 2.47
0.15 0.12 0.11
2-Naphthoic Acid 5. 60 3. 26 3. 43 15. 46 5. 08
1.00 0. 52 0.35 0. 30 0.22
3.90 4. 52 4.24 3.08 7.
0.16 0.10 0.09 0.03
Lead Foil 2. 84 2. 47
1.00 0.60
Diformylbenzidine 4. 46 3. 49 3. 93 2. 79 2. 98
1.00 0. 74 O. 34 O. 32 O. 18
Diphenylthiour ea 4.47 3. 91 12.45 5. 41 8.03
1.00 0.45 0.43 0. 35 0.30
2.89 3.38
0.11 0.10
Aminopyrine
Sulfanilamide
Citric Acid
9.68 6. 65 4.30 5. 30 3. 76
1.00 0.96 0.86 0.66 0.57
3.46 3.08 3. 20 2. 83
0.29 0.23 0.20 O. 11
3.90 4.85 3.11 3.27 6.17
1.00 O. 83 O. 78 O. 65 O. 57
3.05
11.87
0.
38
0.
27
3.
60
4.
79
0.
20
0.
17
81
2.27
8.
13
13.
07
O. 13
O. 06
3. 14
3.67
0. 22
0. 14
7. 80
6.08
0.43
0.36
4.10
3.42
O. 56
0. 52
8.41 3.66 4. 27 6.65 2. 50 2. 75
0.46 0.44 0.43 0. 39 0. 33 0. 22
2. 93 5.29 2. 81 2. 65 2. 24
0.20 0.19 0.17 0.15 0.11
5.08 3.56 6.?40 4.70 3.91 5.58 2.98
1. 00 0.66 0.62 0. 59 0.48 0. 39 O. 35
2. 57 4. 25 3. 23 2. 79
0.30 0.25 0.24 0.20
Sodium Chloride 5. 31 8. 93 3. 02 2. 74
1.00 0.53 0.49 0,38
RJ 7,DRIET-7
-- Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
L-Li]
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Contid)
13-Naphthol
4. 50 3. 99 3. 53 7.63 3.31 3. 15 15. 16
1.00 0. 91 0. 73 0. 72 0.67 0. 30 0.20
2. 91
O. 19
5. 79 5.04 2.44 2. 79 2.69 2. 30
O. 18 O. 17 O. 15 O. 10 0.09 0.05
Octylthiourea
17. 58 3.
40
4. 18
3. 69
9. 50
7. 37
4. 60
1.00 0.
86
0. 79
0. 64
0. 52
0. 43
0. 41
5.98
0.16
Hydroquinone
15.71 9.
75
3.27
7.68
3.51
4. 14
3.62
1.00 0.
73
0.62
0. 57
0. 52
0. 48
0.47
4.40 2. 55 3. 83 3. 13 3. 00 2. 89
0.44 0.43 0.42 0.34 0.27 0.22
4. 80 2. 73 2. 20 5. 74
0.21
0.20
0.20
0.19
Amylase
3. 70 2. 77
2. 21
3. 06
2. 53
3. 16
2.64
1.00 0.97
0.87
0.63
0. 58
0.55
0.47
4.07
O. 39
o.-Nitrobenzene
11.85 14.21
3.33
3.14
2.85
3.51
2.66
arsonic acid lead
1.00 0. 86
0.53
0. 52
0.48
0.47
0.42
salt
7. 33 3.
62 4.
81 2.
80 5.
45 2.
50
Antipyrine
Thiourea
O. 39 O. 38 O. 36 0.36 O. 34 O. 33
4.26 5.85
0.32 031
3. 53_ 5. 28 4.49 3.28 6.63 5. 92 3.68
1.00 O. 72 0.66 O. 65 0.63 O. 60 O. 55
7.51 4.11. 2.98 3.88 2.88 3.12
0. 54 0.42 0. 37 0.34 0. 33 0. 26
2. 64 2.21 2. 73 2.26
O. 18 O. 16 O. 14 0. 12
3.49, 3.53 4.30 3.08 4.45 3.81 2.78
1.00 0.92 0.86 0.81 0.67 0.58 0.47
2.27 2.35 2.18
0.31 0.28 0.25
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
VI "-?
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Coned)
Nickel Acetyl-
8.34
10. 37
9. 05
7. 09
4.28
3. 45
4.63
acetonate
1. 00
0. 87
O. 78
O. 65
O. 63
O. 63
0. 62
3.
81
5.
39
4.
76
3. 66
3.
37
3.
02
0.
57
0.
50
0.
48
0.43
0.
34
0.
34
2. 79
2. 72
2. 38
2. 43
0.31
0.23
O. 18
O. 17
Dry Stab elite
16.28
4.65
6.41
(Paper Resin)
1.00
0.57
0.28
Lithium Carbonate
3. 31
2.25
2. 32
4. 14
1.91
2.. 82
2.47
1.00
0.75
0.71
0.67
0.60
0.50
0.46
1.94 2.43 3-.01 2.10 1.85 2.63
0.46 0-.44 0.38 0.35 0.33 0.31
1-. 99 3. 64 2. 56 3. 79
0.31 0.27 0.25 0.21
0I635 Sudan III Red
5.69 7. 20 8. 14 6. 46 5.01
3,34
2.68
1.00 0. 84 0. 83 0. 81 0. 56
0.47
0.43
2.80 3.12 2.43 2.25
0.40 0.34 0.22 0. 13
0I636 Tartrazine
8.01 10.07 8.78 15.68 6.97
5.40
4.30
1. 00 0. 85 0. 74 0. 64 0. 49 0. 41 0. 40
2.24 2.82 3.95 3.81 4.75 3.22
0. 40 O. 39 O. 37 O. 37 0. 36 O. 36
3.34 2.67 2.58 1.99
O. 35 O. 34 0. 30 0. 24
16 Cinnamic Acid 3.82 9.06 7. 18 7.89 3.08 2. 79 4.75
1.00 0. 83 O. 83 0. 75 O. 69 O. 63 O. 60
3.42 3. 51 4. 18 5.98 3.26 2. 42
0.52 0.48 0.44 0.40 0.40 0.35
2.62 2.32 -
0.23 0.17
14 diformylbenzidine 3. 59 2. 80 4. 53 3. 97 3. 08 3. 28
1.00 0.64 0. 55 0. 41 0.26 0. 16
?- r
- Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
IJ JI k_Jupy z-1
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Cont'd)
SP-1102
SP-1103
10.26 718 8.95 7.93 6.12 4.29 5.41
1. 00 0. 92 0. 88 0. 86 0.62 0. 59 0.53
2. 94 4.00 3.82 4,77 3.66 3.25
0.47 0.44 0.44 0.42 0.42 0.38
3.40 3.06 2.39 2.21
0. 36 0.27 0. 12 0. 12
5. 09 9. 88 3. 51 3. 26 6. 39 4. 32 5. 56
1. 00 0. 91 0. 80 0.64 0.61 0. 61 0. 50
SP-1105
4.08 3.83 2.98 4.76 2.86 3.11
0.41 0.41 0.41 O. 39 O. 36 O. 34
2.45 2.70 2.61 2.31 2.26 2.09
0.27 0.18.,0. 14 0.14 O. 14 O. 11
11.70 14.48 4.53 3.38 3.67 3.82 4.20
1. 00 0. 76 0.42 0. 34 O. 33 0. 32 0.29
5. 74 3. 14 4. 96 2.91 2. 78 2.64 2. 47
0.27 0.26 0.22 0.22 O. 18 O. 18 O. 11
SP-1107
12. 19 6.82 6. 18
5.27
4.06
3. 18
1. 00 0. 76 0.67
0. 60
0. 50
0. 38
SP-1108
9. 97 6. 26 4. 94
5. 64
2. 76
1. 00 0.61 0. 57
0.41
0.23
SP-1110
No Sharp Rings
SP-1111
2. 47 3. 07 5.21
2. 53
6.60
3. 88
5. 73
1.00 O. 68 0.67
O. 64
0.61
O. 61
O. 55
SP-1112
4.45 4.91 2.56 3. 18 2.71 2.28
0.48 0.45 0.42 0.41 0.39 0.35
3. 38 2. 95 2. 82 2. 23 2. 05
0. 32 O. 32 0. 27 0.21 0.21
4.91 3.48 6.18 5.37 7.11 4.37 3.83
1.00 0.91 0.52 0.51 0.47 0.46 0.44
3. 14 2.60 3.29 2.22 2.09 1. 88
0.32 0.23 O. 19 O. 16 O. 16 O. 11
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
( 2,
FL,
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Cont' d)
SP-1113
3.61
3.96
4.53
2.81
1.00
0.62
0.59
0.49
SP-1114
3.58
3.29
1.00
0.79
SP-1115
12.91
3.59
4.51
3.95
1.00
0.27
0.22
0.20
SP-1116
8. 12
4. 93
3.20
4.40
1.00
0.80
0.57
0.50
SP-1117
SP-1118
SP-1119
3,09
0.38
2.59 2.53 2.44
O. 11 O. 11 0.09
2.66 2. 59 3. 54
0.48 0.43 0.35
2.70 2.48 2.31 2.27
0.30 0.22 0.15 0.15
11.99 13.01 15.01 7.95 18.21 10.08 8.81
1.00 0.79 0.76 0.61 0.57 O. 51 0.45
4.40 7.26 2, 26 3. 96 4. 86 2. 70 2.60
0.44 0.39 0. 28 0.27 O. 26 0.24 O. 24
5. 54 5. 88 3. 76 6. 55 3. 55 2, 99 2. 35
O. 23 0.22 0. 21 O. 18 O. 16 O. 16 O. 16
3.37 3.11 4.13 3.29 2.09 1.96
O. 15 O. 15 O. 12 O. 11 0.07 0.06
7. 91 10, 08 8. 80 6. 16 6. 75 5. 22 4, 78
1. 00 0. 93 0. 84 0.67 0. 57 0.47 0.47
4.37 3.90 2.86 3.61 3.45 2.91 2. 74
0.45 0.38 0.34 0.31 0.31 0.31 0.31
3. 14 3. 26 2. 59 2. 53 2.25
O. 29 0.28 O. 24 O. 16 O. 16
8.84 4.35 7.64 6. 15 6.75 5.02 5. 55
1. 00 0. 85 0. 83 0. 77 0.68 0. 57 0. 55
4. 78 3. 91 2. 93 2. 74 3. 73 3.45
0.53 0.49 0.45 0.45 0.42 0.42
3.04 3.23 2.63 2.54
0.42 O. 38 0. 36 O. 36
7, 7
- Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
y
L
TABLE 4. TABULATION OF APPARENT ATOMIC PLANE SPACINGS
AND INTENSITY RATIOS FOR THE DIFFRACTION RINGS FROM
SEVERAL POWDERED SAMPLES (Conti d)
SP-1120
11.91 7.95 10.15 8.87 7.20 4.39 5.98
1.00 0.62 061 O. 58 0.44 0.43 0.28
5.
51
4.
85
3. 95
3.
77
2.
70
2. 70
2.60
0.
27
0.
24
O. 23
0.
23
0.
23
0.23
O. 19
3. 56
3. 37
3. 29
3. 11
2. 98
2.43
2. 36
O. 16
O. 13
O. 13
9. 13
O. 12
O. 12
O. 11
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
ijitApes11/.
z
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
0 0 0 0
0
0
FIGURE 2. DIFFRACTION OF X-RAYS BY ATOMS IN
A CRYSTAL LATTICE - BRAGG'S LAW
Nickel
Absorption
.???????
K cc
_Copper
Radiation
I
1.0 1.5
Wavelength in Angstrom Units
2. 0
FIGURE 3. FILTERED RADIATION. CHARACTERISTIC COPPER
RADIATION AND NICKEL ABSORPTION. RELATIVE INTENSITY
AND ABSORPTION VERSUS WAVELENGTH.
(Note: Intensity and absorption are not to scale.)
?.
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WasusO
Cathode
x-rays
Copper
Anode
x-rays
$hutter (Closed)
7?
0
(D
0
Shutter (Open)
71747127
_1.
2.
3.
4.
5.
6.
7.
8.
9.
(1)
cc,
(D
-0
.Retainer
Pinhole collimator (/)
Sample support
Sample washer
Film
0
Film support
Fluorescent screen
and lead glass -a
-a
Camera body
Clamping ring - (D
(D
0";? (7)
ts4 Q)
s
46.1?
'47##
1017'
N:.\\ AS"
G. E. Type CA-7 X-ray Tube Philips Micro Camera No. 52055
Go
FIGURE 4. DETAILS OF DIFFRACTION MICRO CAMERA IN POSITION
NEXT TO THE X-RAY TUBE
1?,;r:r; 0
cyi
0
-0
co
0.)
0
0
0
0
0
0
0
0
0
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SECR
'NY
FIGURE 5. EFFECT OF SAMPLE SIZE ON DIFFRACTION RING
RESOLUTION. Densitometer scans of Powder Patterns
from diformylbenzidine. A - sample size - lmm. dia.
by 0. 7 mm. thick. B - sample size - 0. 2 mm. dia. by
0. 1 mm. thick.
SECRET
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In 1E:4'
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
y I J. -X
?fl
No.
FIGURE 6. DIFFRACTION PATTERNS FROM MICROGRAM
OR LESS QUANTITIES OF SAMPLE
Compound Weight(milligrams) Exposure Time (hours)
A
Uric Acid
0.0001
5
B
Magnesium Oxide
0.0003
6
C
Dimethylglyoxime
0.001
7
D
2-Naphthoic Acid
0.0002
15
E
Anthracene
0.001
4
F
Pyrazalone
0.0003
16
G
Diacetyl Benzidine
0.0005
8
H
Sudan III CI 248
0.0003
16
Note: All patterns produced on Ilford Film.
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.:L
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
FIGURE 7. THE EFFECT OF PARTICLE SIZE
1. Unground
2. After Grinding
3. After Further Grinding
4. Magnesium Oxide Added
5. Further Grinding with MgO Added
Note: All diffraction patterns made from SP-1111. Average sample weight
one mg. All exposures 7 hours on Eastman KK film.
(JD
1
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73 7 Cs'
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Photo Tube
10 -Powe r
Microscope
Objectives
Fraory
Slit
Recorder
Material to be Scanned
'*--Sandwiched between
Glass Slides
Glass Jaw Slit
Condensing Lens
Straight Filament Lamp
FIGURE 8. DENSITOMETER
SEC Fig
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
itrArrir
"1J/it!
.2
10
20
rik
30
E-1
4a'
(N.;
G)
40
50?i
70 ?
90 ?
Hole
-10
-5 0 +5
+10
Distance from Center of Diffraction Pattern in Millimeters
FIGURE 9. REPRESENTATIVE DENSITOMETER SCAN
OF X-RAY DIFFRACTION PATTERN
OF POWDERED URIC ACID
(The numbers by the peaks are the d/n values)
t';:olor
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
FIGURE 10. 10. DIFFRACTION PATTERNS FROM
CATALOGUE COMPOUNDS
Sample
Weight(mg. )
Exposure Time
Film*
1.
Anthracene
0.4
15 min.
Il
Z.
Ethyl Cellulose
1
15 min.
R
3.
Hemin
1
30 min.
R
4.
Disodium EDTA Calcium
1
1 hr.
R
5.
Carbanthrene Violet
1
15 min.
II
6.
Xylenol Orange
0.17
4 hr.
Il
7.
Disodium EDTA Zinc
1
4 hr.
R
8.
Disodium EDTA
1
15 min.
R
9.
Disodium EDTA Magnesium
1
30 min.
R
10.
Magnesium Oxide
1
15 min.
II
11.
8-Hydroxyquinoline
1
15 min.
R
12.
Tetrasodium EDTA
1
15 min.
R
*II - Ilford Type G, R - Rinn Type DC-1
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
I `-"..
FIGURE 11. DIFFRACTION PATTERNS FROM
CATALOGUE COMPOUNDS
13.
14.
15.
16.
Sample
Weight (mg.)
Exposure Time
Film*
Isopropyl Jade Green
Paper (Beverly Bond)
Whatman No. 2
Filter Paper
Sulfite Paper
1
0.7 (5 layers)
1 (4 layers)
0.8 (6 layers)
30 min.
30 min.
30 min.
30 min.
R
R
R
17.
Dialysis Tubing
(Cellulose)
0.01 (1 layer)
30 min.
18.
216 F-1
0.003
4 hr.
Il
19.
Sudan III CI 248
0.1
1 hr.
Il
20.
Mylar
0.05
15 min.
Il
21.
Dry Stabelite
(Paper Resin)
1
1 hr.
Il
22.
Sulfanilamide
0.2
4 hr.
Il
23.
Octylthiourea
0.5
2 hr.
Il
24.
Uric Acid
1
2 hr.
Il
*II - Ilford Type G, R - Rinn Type DC-1
FJT
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved fcaRr117.1e171775 : CIA-RDP78-03166A000700010001-1
L.opy oi 4-?
FIGURE 12. DIFFRACTION PAT TERNS 'FROM
CATALOGUE COMPOUNDS
Sample
Weight (mg.)
Exposure Time
Film*
25.
Sulfadiazine
1
30 min.
R
26.
Sulfapyridine
1
30 min.
R
27.
Versene
1
30 min.
R
28.
Formvar Film**
0.0001 (est.)
15 min.
Il
29.
Corn Starch
1
30 min.
R
30,
Triphenyl Phosphate
1
30 min.
R
31.
Talca
1
30 min.
Il
32.
Talcb
1
30 min.
Il
33.
Talcc
1
30 min.
Il
34.
Talcd
1
30 min.
Il
35.
Dimethylglyoxim.e
0.2
2 hr.
Ii
36.
Dimethylglyoxime
(showing lead rings)
0.02
7 hr.
*II - Ilford Type G, R Rinn Type DC-1, K - Eastman Type KK
**Evaporated from 10% Soln. in ethylene dichloride
a - Penaten - German
b - Nivea - German
c - Greta Gallica - French
d - Phan Thom - Vietnam
07,
T_T!
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
;.;
'
? Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
'-'
,
FIGURE 13. DIFFRACTION PATTERNS FROM
CATALOGUE COMPOUNDS
37.
38.
Sample
Weight (mg.)
Exposure Time
Film*
Paraffin Wax
Diacetylbenzidine
1
0. 6
30 min.
1 hr.
Il
Il
39.
Aspirin
0.5
6 hr.
K
40.
Sulfaguanidine
0.02
7 hr.
K
41.
Antipyrine
0.02
7 hr.
K
42.
Hydroquinone
1
5 hr.
K
43.
Citric Acid
0. 6
4 hr.
Il
44.
Diforrnylbenzidine
(showing lead rings)
0.02
7 hr.
K
45.
Diformylbenzidine
0.6
4 hr.
Il
46.
p-Naphthol
1
2 hr.
Il
47.
2-Naphthoic Acid
0.003
15 hr.
Il
48.
Aminopyrine
0.2
2 hr.
II
*II - Ilford Type G, K - Eastman Type KK
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
P F r
'? Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
LYI
FIGURE 14. DIFFRACTION PATTERNS FROM
fl
CATALOGUE COMPOUNDS
Sample Weight (mg.)
Exposure Time
Film*
49.
SP-1107 ec, c-A4-)I" ' Y /4-9
0.02
3 1/2 hr.
K
50.
SP-1116.C44-1A--o.,,a4...;
0.02
5 hr.
K .
51.
SP-1114
0.02
7 hr.
K
52.
SP-1104
0.02
7 hr.
K
53.
SP-1110 ri'l
0.02
7 hr.
K
54.
Mica
0.07
15 min.
Il
55.
Tin (foil)
0.2
1 hr.**
Il
56.
Aluminum (foil)
0. 07
15 min.**
II
57.
Sodium Chloride
(powdered)
1
4 hr.
58.
Sodium Chloride
0.005
15 min.
Il
(single grain)
59.
o-Nitrobenzenearsonic
Acid Lead Salt (unground)
0. 01
8 hr.
60.
o-Nitrobenzenearsonic
Acid Lead Salt (ground)
0.01
7 1/2 hr.
*II - Ilford Type G, K - Eastman Type KK
**Without nickel filter over collimator
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
?
? Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
W.L
`6DLLLL
r
FIGURE 15. DIFFRACTION PATTERNS FROM
CATALOGUE COMPOUNDS
Sample Weight (mg.) Exposure Time
Film*
61.
Pyrazalone
0.1
1 hr.
Il
62.
Thiourea
0.6
16 hr.
K
63.
Sudan III Red CI 635
0.02
7 hr.
K
64.
Lithium Carbonate
0.01
8 hr.
K
65.
Lithium Carbonate
plus sulfaguanidine
0.02
7 hr.
K
66.
Tartrazine CI 636
0.02
7 hr.
K
67.
Cinnamic Acid
0.02
7 hr.
K
68.
SP-1108 rig /7)
0.02
14 hr.
K
69.
SP-1113 N- ,,R
0.02
7 hr.
K
70.
SP-1l05 SP-1105
0.02
7 hr.
71.
SP-1115
0.02
6 hr.
K
72.
SP-1106
0.02
8 hr.
K
*II - Ilford Type G, K - Eastman Type KK
F.7
[L, (3
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
A .
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
r? Y ?L
'
FIGURE 16. DIFFRACTION PATTERNS FROM
CATALOGUE COMPOUNDS
73.
Sample
Weight (mg.)
Exposure Time
Film*
Magnesium Oxide
plus Germanium Dioxide
0.03
8 hr.
74.
Magnesium Oxide
plus Amylase
0.02
8 hr.
75.
Nickel Acetylacetonate
0.013
3 1/2 hr.
76.
Diphenylthiourea
1
4 hr.
Ii
77.
Magnesium Oxide
plus Lead
0.02
7 hr.
78.
SP-1103 fr,z/G1A4A-.
0.02
7 hr.
K
79.
SP-1102 Yke-w.:4.-v-
0.02
7 hr.
K
80.
SP-1112 FAAP
0.02
6 hr.
K
81.
SP-1118 PA0 (rt-r-HLO
0.02
6 hr.
K
82.
SP-1117 P A P (Le)
0.02
6 hr.
K
83.
?PAN
SP-1119
0.02
6 hr.
K
84.
PAO 6 (14 4
SP-1120
0.02
8 hr.
K
*II - Ilford Type G, K - Eastman Type KK
-
--- Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
\%
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
--
uopy rz
LT
L_
FIGURE 17. DIFFRACTION PATTERNS FROM DILUTIONS
fl OF CHEMICALS IN CORN STARCH
A. 50% Aspirin, 50% Magnesium Oxide
B. 25% Aspirin, 25% Magnesium Oxide, 50% Starch
C. 10% Aspirin, 10% Magnesium Oxide, 80% Starch
D. 1% Aspirin, 1% Magnesium Oxide, 98% Starch
E. 50% Uric Acid, 50% Starch
F. 25% Uric Acid, 25% Magnesium Oxide, 50% Starch
G. 10% Uric Acid, 10% Magnesium Oxide, 80% Starch
H. 3% Uric Acid, 97% Starch
J. 25% Sulfaguanidine, 25% Magnesium Oxide, 50% Starch
K. 10% Sulfaguanidine, 10% Magnesium Oxide, 80% Starch
L. 1% Sulfaguanidine, 1% Magnesium Oxide, 98% Starch
Note: Average sample weight was 1.3 mg. All exposures on Rinn DC-1
film for 30 minutes except E - 15 minutes and H - 1 hour.
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
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Declassified in Part - Sanitized Copy Approved for Release 2014/04/25: CIA-RDP78-03166A000700010001-1
y j%/I '"t
REFERENCES
1. Gross, S. T. and Oberst, F. W., J. Lab. Clin. Med., 32,
94(1947).
2. Swanson, H. E. and Tatge, E., Standard X-Ray Diffraction
Powder Patterns, N. B. S. Circular 539, Vol. I, 1953, P. 51.
3. Clark, G. L., Applied X-rays, McGraw-Hill (New York, 1955),
pp. 95-102.
4. Azaroff, L. V., Norelco Reporter, VI, Nos. 4-5, pp. 76-79.
5. Handbook of Chemistry and Physics, Chemical Rubber Publishing
Co., (Cleveland, 1953) pp. 2399 and 2406.
6. Medical X-ray Protection Up to Three Million Volts, N. B. S.
Handbook No. 76, Supt. of Documents (Washington, D. C., 1961),
p. 20.
7. Bergmann, M. E., Norelco Reporter, VI, Nos. 4-5, pp. 96-100.
1-=
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