PROJECT 325B SUMMARY PERIOD: 1 FEBRUARY 1972 TO 29 FEBRUARY 1972

• Document Type: CREST
• Collection: NGA Records (Formerly NIMA)
• Document Number (FOIA) /ESDN (CREST): CIA-RDP80T01137A000100010011-7
• Release Decision: RIPPUB
• Original Classification: S
• Document Page Count: 55
• Document Creation Date: December 28, 2016
• Document Release Date: March 18, 2010
• Sequence Number: 11
• Content Type: REPORT

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PERIOD: 1 February 1972 to 29 February 1972
Submitted By:
Project anager
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PROJECT 325B
SUMMARY REPORT
PERIOD: 1 February 1972 to 29 February 1972
Submitted By:
Project Manager
Copy D of 7
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Section Page
SUMMARY . . . . . . . . . . . . . . . . . . . . . . v
Chemical R and D Overview . . . . . . . . . v
Monthly Results . . . . . . . . . . . . . vii
1.0 CHEMICAL R AND D . . . . . . . . . . . . . . . 1
1.1 Leuco Dye Program . . . . . . . . . . . . 1
1.1.1 D260 . . . . . . . . . . . 1
1.1.1.1 Alternate Synthesis of
D260 - Anthrone Route , . 1
1.1.1.2 Role of D260 in Speed
Decay . . . . . . . . 3
1.1.1.3 D260 Decay Products . . . 4
1.1.2 Other Leuco Compounds . . . . . . 6
1.1.2.1 2-Methyl Leuco Crystal
Violet . . . . . . . . . 6
1.2 Carbon Tetrabromide (CBr4) . . . . . 6
1.2.1 Deterioration Studies . . . . . . 7
1.2.2 Film Additions of Suspected CBr4
Decomposition Products .?. . . . . 7
1.2.2.1 Bromine . . . . . . . 7
1.2.2.2 Tetrabromoethylene . . . 7
1.2.2.3 Hexabromoethane . . . . . . 7
1.3 N-Oxide Program . . . . . . . . . . . . . 9
1.3.1 4-Picoline-N-Oxide (4P0) . . . . . 9
1.3.2 Other N-Oxides . . . . . . . . 9
1.4 Binder Studies . . . . . . . . . . . . . 9
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TABLE OF CONTENTS (continued)
Section Page
1.5 Environmental Studies . . . . . . . . . . 9
1.5.1 Air Sampling . . . . . . . . . . . 9
1.5.2 Environmental Contamination . . . 10
1.6 Other Film Systems . . . . . . . . 10
1.7 Film Analysis of Decay Products . . . . . 10
1.8 Dye Identification . . . . . . . . . . . 11
1.9 Systems Nonuniformities . . . . . . . . . 11
2.0 ENGINEERING . . . . . . . . . . . . . . . . . 23
2.1 Calibration and Equipment Maintenance . . 23
2.2 Mechanical . . . . . . . . . . . . . . . 23
2.3 Shelf Life . . . . . . . . . . . . . . 23
2.4 Red Light Research and Development . . . 23
2.5 Environmental Conditioning . . . . . 24
3.0 PERKIN ELMER INTERFACE, QC/QA . . . . . . . . 25
3.1 Supply of Film and Equipment . . . . 25
3.1.1 Delivery of 325B Film . . . ... . 25
3.1.2 Delivery of Solvent Rinse. . . . . 26
3.1.3 Delivery of Red Light Development
Units . . . . . . . . . . . . . . . 26
3.3 Evaluation of Production, Shipping and
Contamination . . . . . . . . . . . 29
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TABLE OF CONTENTS (continued)
Page
3.4 Monitoring of Results and Anticipation of
Subsequent Plans . . . . . . . . . . . 30
3.7 QC/QA . . . . . . . . . . . . . . . . . . 31
PROBLEMS . . . . . . . . . . . . . . . . . . . . . 45
PLANS FOR NEXT REPORTING PERIOD . . . . . . . . . 45
FINANCIAL . . . . . . . . . . . . . . . . . . . . 45
1 Aging Study of Standard 5/D7 Coating Solution. 12
2 Aging Study of 5/D7 Coating Solution Minus D260 13
3 Addition of Bromine to 5/D7 . . . . . . . . . 14
4 Results of Air Sampling Program . . . . . . . 15
1 CBr4 - Deterioration Study . . . . . . . . . . 16
Figures
CHEMISTRY 1.0 SECTION:
1 Illustration of "Good" and "Bad' Films 17
2 Film 3 of Figure 1 . . . . . .. . . . . 18
3 Film 4 of Figure 1 . . . . . . . . .. . . . . . 19
4 Film 5 of Figure 1 . . . . . . ?. . . . . . 20
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TABLE OF CONTENTS (continued)
Figures Page
5 Film 6 of Figure 1 . . . . . . . . . . . . . . 21
PERKIN ELMER INTERFACE,.QC/QA 3.0 SECTION:
1 Perkin Elmer's TD-102 Densitometry . . . . . . 33
2 TD-102 Densitometry . . . .. . . . . 34
3 Project 325B's TD-102 Densitometry . . . . . 35.
4 Comparison of Three TD-102 Densitometers . 36
5 Comparison of Three TD-102 Densitometers with
Blue Filter, Ektacolor Internegative Tablet 37
6 Comparison of Three TD-102 Densitometers,
Ratio of Blue/Green Filter Densities Ektacolor
Tablet . . . . . . . . . . . . . . . . . . . . 38
7 Color Profile of 325B Film . . . . . . . . 39
8 Frequency of Good and Bad Film Days VS.
Bracketed NO2 Concentrations . . . . . . . 40
9 Frequency of Good and Bad Film Days VS.
Bracketed Oxidants Concentrations . . . . . . 41
10 Frequency of Good and Bad Film Days VS.
Bracketed X2 Concentrations . . . . . . . 42
11 Frequency of Good and Bad Film Days VS.
Bracketed HC1 Concentrations . . . . . . . 43
12 Frequency of Good and Bad Film Days VS.
Bracketed HBr Concentrations . . . . . . . . . 44
CHEMISTRY 1.0 SECTION . . . . . . . . . . . . . . . 22
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The project work for February continued; bearing on
shelf life/speed decay. The air sampling program was completed.
A complete analysis of the mass of data has not shown a correla-
tion with either "blotch" film samples or low photographic
speed samples. However, the experiments showing comparisons
between the Chemical R and D control labs and the engineering
labs show correlation between these effects and some airborne
contaminant. The pure air purging of the engineering room
produced good film samples during a three hour run. The new
isolated engineering darkroom is forecast for completion by
15 March. If good films are produced here, the engineering
work on reactivation and overcoating will be carried out during
the last two weeks of March. This effort has slipped one month.
The six HID-2 red light development units were completed.
One unit was shipped to Perkin Elmer. The last two film ship-
ments to Perkin Elmer have been delayed in.transit for periods
up to five days, in both cases the dry ice was depleted and the
films useless for red light development. It may be advisable
to ship direct to Danbury by air charter.
Considerable work was done on qualifying the Quantametric
automatic plotting densitometer as a project standard. Cross
over comparisons on the present densitometer filters and the
status "A" type on this device are being carried out. Some
problems with using the small project film samples has been
experienced. This unit is forecast to become the project
standard by the end of March.
Overview
The problem of environmental contamination, and the resultant
failure to obtain satisfactory films, continues. The contaminant
has been shown to be airborne, but it is not known whether it
is gaseous or particulate. This problem has restricted film
evaluation work to two men and one darkroom, the one which has
been environmentally controlled. The adjacent, dark room has been
sealed and shown capable of decontamination. As soon as addi-
tional Barnebey Cheney air purifiers arrive, this room should
become available for work. This is expected in the second week
in March.
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Air sampling analyses last month showed a positive correlation
.between the contamination and chemical oxidants as a
class. This month's analyses have failed to support this
initial correlation, or provide any new correlation. The air
sampling program has therefore been discontinued. The current
apporach is to secure uncontaminated work areas so that all work
can proceed.-
The contamination problem has hindered Chemical R and D's
film evaluation work, but not seriously. On the other hand,
delays in hiring the two urgently needed organic chemists has
affected nearly all aspects of the materials programs to greater
or lesser extent.
(M.S.) have just accepted the positions and begin work in early
March. Chemical R and D will, therefore, be in full progress
.by the latter part of March.
Because of the manpower shortage several work areas have
fallen behind schedule or have been postponed:
1.1 Leuco Dye Program: The model studies, particularly
the purification and testing of leuco malachite green
analogues has fallen behind schedule. The situation is
not particularly serious, however, and work is again
expected to proceed on schedule by the latter part of
March.
1.2 CBr4 - Activator Program: The program to study the
deterioration of solid CBr4 is underway and proceeding
on schedule.
1.3 N-Oxide Program: Phase I has been completed. No further
work is scheduled until the results have been thoroughly
evaluated.
1.4 Binder Studies: No work was scheduled for February. The
effort in March will be increased to compensate for
delays in the Environmental Studies scheduled to begin
in March.
1.5 Environmental Studies: It now appears that the plan
to begin purifying all materials, and to formulate and
coat film in purified atmospheres will be delayed from
March to April. This situation has arisen from delays
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in acquiring the necessary LabConco dry boxes. Supply
has been limited, and two recently acquired boxes were
defective and had to be returned. Current estimates
for securing the necessary equipment and for setup,
project the new starting date to the beginning of
April. The time originally alloted to March will be
used to increase our effort on binder studies ahead of
schedule and to catch up in other areas; such as the
leuco dye program and film analyses studies.
1.6 Other Film Systems: This work was scheduled to begin in
early March. It will be delayed to the latter half of
March when another darkroom is expected to be usable.
1.7 Film Analyses of Decay Products: Shortage of manpower
has delayed this work. Our latest research results
(Section 1.1.1.3) necessitates our proving or disproving
that 4DMAP is formed during decay. Film analysis work
will, therefore, begin during March and as soon as the
new hires begin work.
Large batches of TI41B-free D260 will begin arriving, from
Chemical Samples Company in early March.
The alternate synthesis of D260 is underway but has been
hindered due to manpower shortage.
D260 has been demonstrated to be the major culprit in rapid
speed decay. It is not known, however, if it is the sole cause
or if it is due to specific interaction(s) with one or more of
the other ingredients.
4-Dimethylamino phenol (4DMAP) has been shown to be extremely
deleterious to photores-ponse. It is a possible degradation product
of D260 hydroperoxide which is suspected of being formed during
decay.
The CBr4 deterioration studies are underway.
New supply of CBr4 (Berk Ltd.) has been found. It is manu-
factured in France and appears quite pure. Surprisingly, it has
afforded excellent films without any purification.
The N-oxide program: Phase I has been completed. Results
are being evaluated.
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1.0 CHEMICAL R and D
1.1 Leuco Dye Program
1.1.1 D260
Chemical Samples Company has promised to deliver about
700 g of D260 in early March. This material will be free of
tetramethylbenzidine (TMB) by TLC, whose detection limit is
about 50 ppm. Large scale purification of D260 will then be
undertaken. Our supply of photograde D260 remains adequate
for our on-going film studies.
A number of samples of D260 were sent to Gollob Analytical
Services for mass spectral analyses. Results of these analyses
are not yet known.
During February a fluorimeter was obtained on a trial
basis, and was used to study the purity of D260 with respect
to TMB. The results indicate that apparently as little as
200 ppb (parts per billion) TMB can be detected by this method.
This value is only approximate, however, since the level of
TMB in the control sample of D260 was known only to be less
than 50 ppm, the current limit of sensitivity by TLC. D260
which is totally free of TMB will be available from the new
synthetic route and will therefore serve as an absolute control
standard for the TMB determination.
Arapahoe Chemical (Boulder, Colorado) has agreed to prepare
5 kg of D260 by the procedure currently being used by Chemical
Samples Company, and eight thousand (8,000) dollars has been
provided for this. However, the order for this additional D260
will be postponed until the new synthetic route can be evaluated.
Should this new route prove feasible and the D260 of superior
quality (because of different or fewer impurities as discussed
in last month's report), then money will be available for securing
an adequate supply. This new route also affords the means of
preparing analogues of D260 by way of the intermediate anthrone.
1.1.1.1 Alternate Synthesis of D260 - The Anthrone Route
The details of this alternate route to D260 were shown
in last month's report. For this month's discussion, only
selected intermediates will be pictured:.
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N(CH3)2
H2
in-isopropenyl-N,N-
dimethylaniline
(Step 2)
D2.63
(Step 4)
(Step 6)
(Step 9)
The olefin, m-isopropenyl-N,N-dimethylaniline, is a common
intermediate to both the current route and the anthrone route.
The first attempt at the anthrone routes, in January and February,
resulted in crude D263 in 50% yield from the olefin. This was
reduced to 13% yield by two unfortunate recrystallizations from
ethanol. Further work led to 1.9 g of anthrone, mp 205?C,
a 2% overall yield from olefin.
The low yield has necessitated a rerun which is currently
underway. Alternatives to the ethanol recrystallization and
the chloranil oxidation will be investigated.
Optimum yields of D260 by this alternate route have been
estimated and are compared with the standard route:
Anthrone Route Standard Route
Optimum Moles Moles
m-isopropenyldimethylaniline 1.00
2-isopropenyl-4,41-bis(dimethyl-
amino) diphenylmethane
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(continued)
Intermediate
D263
anthrone
D260 carbinol
D392 (D260 dye)
crude D260
rex'd D260
Anthrone Route Standard Route
Optimum Moles Moles
0.44
0.32
0.28
0.25
0.22
0.20
The anthrone route is expected to yield less D260 than
the current method. At this time, however, this fact is not
critical especially if it settles questions concerning the effects
of TMB and other impurities. The anthrone route is being followed
according to the procedure of Aaron and Barkeri. Many improve-
ments of their procedure can be readily envisioned, should it
become necessary to ultimately prepare D260 by this route.
The last step in the Anthrone route to D260 is the reduction
of the dye to its leuco form. To confirm the feasibility of
this step, a small sample of D391 (the nitrate dye of D260)
was reduced with zinc and acetic acid. Authentic D260 was obtained.
This was a matter of concern since it was discovered that catalytic
hydrogenation (one possible means of reduction) destroys D260.
The chemical reduction, on the other hand, appears satisfactory.
1.1.1.2 Role of D260 in Speed Decay - Aging of Coating Solution
Independent series of experiments with coating solutions
of Formulas 1, 3 and 5 over the past several years show that
bulk coating solutions undergo speed decay (determined by film!
evaluation in the usual manner), and at a rate which increases
with increasing concentration of. le.uco compound2. These obser-
vations provide a strong indictment against the leuco compound
as the principal culprit in rapid speed decay.`
To test this indictment an aging-comparison was made between
5/D7 coating solution and an identical solution without D260.
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Both solutions were stored in the dark at ambient temperature.
Aliquots were periodically removed and photographically evaluated.
In the one case the appropriate amount of D260 was added just
prior to coating.
The standard coating solution was found to deteriorate
significantly within .a matter of hours as can be seen in Table 1.
In general, densities and development time decrease and fog
increases with age.
Table 2 shows the results of 52 days aging of the solution
which contained no D260. The contrast with the standard solution
is evident and striking. Within the normally experienced range
of variations, the densities and development time remained unchanged.
It is not correct, however, to say that the solution has. not
changed, or aged. An examination of speeds indicates a possible
trend toward lower speeds during the latter 30 days. This may
be real and due to some form of aging or it could be due to the
switch in samples of D260. A physical change in the solution
was noted during this latter period. The original bright yellow
solution became deep orange-brown. This observation is certainly
indicative of some chemical change possibly the formation of
bromine (see Section 1.2.2.1).
In any event results of this comparison leave no doubt
that the D260 is the principal culprit in rapid speed decay.
Whether the real cause is D260 itself or is an interaction of
D260 with one or more of the other ingredients is not known.
Additional solution experiments are planned in order to evaluate
a variety of possible interactions.
1.1.1.3 D260 Decay Products - Film Evaluation
Last month's report (Section 1.1.1.5) described the synthesis
of 4-dimethylamino,phenol (4DMAP) and referenced3 the suspicion
that the material, a possible degradation product of the D260
hydroperoxide, might be responsible for the observable properties
of speed decay. 4DMAP and related compounds were therefore
evaluated for their effect on the principal film system--5/D7.
The maximum amount of 4DMAP that can be added to the 5/D7
system without affecting its photosensitivity is about 1 pg.
Addition of 5 pg resulted in lower densities with longer develop-
ment times. Ten micrograms gave only a very slight image
(maximum density .23) after 360 seconds development. Printout
exposures gave parallel results but to less extent.
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In contrast to 4DMAP, its 3-isomer (3DMAP) had considerably
.less effect. One hundred micrograms had no apparent effect
whatsoever, and 500 ?g was necessary to observe lower densities
and longer development time.
The addition of 3 mg phenol which is about one-thousand
times the weight of 4DMAP had no effect on either the development
or printout mode. Significantly lower densities and longer
development time were observed with 10 mg. The addition of 12 mg
N,N-dimethylaniline (DMA) also had no significant effect.
Phenol and DMA each contain one of the functional groups
present in 4DMAP and yet both are on the order of a thousand
times less effective. Thus, both the hydroxyl and dimethyl-
amino groups must be part of the same molecule and preferably
para (4DMAP) for maximum effectiveness. In support of this
conclusion is the effect of 4-methylamino-phenol (4MAP = Elon)
an analogue of. 4DMAP in which one methyl group has been simply
replaced with a hydrogen. It gave results essentially identical
to 4DMAP.
It is noteworthy that both 4DMAP and 4MAP are reducing
agents as evidenced by their effectiveness as developers for
silver halide films. Phenol and DMA are not. No data on 3DMAP
has been found but it is probably not an effective reducing
agent, and hence more like phenol and DMA. This can be supported
by the work of Tani4who has related molecular orbital calcu-
lations of certain substituted benzenes, including amino phenols,
to their effectiveness as silver halide developers, in other
words, as reducing agents. His calculations show that 4DMAP
and 4MAP should be effective developers whereas 3DMAP should not
be.
It thus appears that easily oxidized compounds are parti-
cularly detrimental to the leuco system. This conclusion is
further substantiated by earlier work in which antioxidants (com-
pounds which are themselves easily oxidized) such as Plastinox 425
and 2,6 -di-tert-butylcresol were found to also be detrimental.
In contrast to those antioxidants, 4DMAP can theoretically be
formed in situ from D260 via the hydroperoxide3. If the D260
hydroperoxide does form in the film, then it*may well be the
initial cause of rapid speed decay in which case prevention of its
formation could provide the cure. The same argument holds for
the 7/D7 system in which LCV replaces D260, since 4DMAP would
also be the result of hydroperoxide decomposition.
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An alternate approach would be a leuco compound whose hydro-
peroxide would not yield 4DMAP but rather a less detrimental arti-
fact. An example would be leuco malachite green or its D260
analogue5 , the hydroperoxides of which should give phenol.
Phenol is about a thousand times less detrimental than 4DMAP.
If all other aspects of the mechanism were the same, a thousand
fold increase in shelf-life is conceivable. This would mean.
extension of the current useful life of 30 minutes to a life of
around 21 days.
This argument is of course highly over simplified. It
assumes one cause and one mechanism for the rapid decay, and
also identical rates for hydroperoxide formation and subsequent
decomposition regardless. of the leuco compound's structure.
The argument does, however, serve to illustrate one approach
to solving the speed decay problem, and it. also serves as a
guide to planning our studies. For example, hydroperoxide forma-
tion in the film is not an established fact and direct identifi-
cation is viewed as extremely difficult. However, identification
of 4DMAP and a correlation of its increasing concentration with
increasing loss of photoresponse would be next to positive proof.
A search for 4D47AP in aging film has been planned but the current
shortage of manpower has delayed this effort. A parallel effort
in synthesizing other leuco compounds is underway but has been
hindered for the same reason.
1.1.2 Other Leuco Compounds
Last month's report (Section 1.1.2) mentioned some preliminary
studies with other leuco compounds, particularly leuco malachite
green (LMG) analogues. Little progress was made this month due
to the shortage of manpower; a situation which will have been
corrected by the middle of March. Bearing any unforeseen compli-
cations in other work areas, there should be results to report
next month.
1.1.2.1 2-Methyl Leuco Crystal Violet (D416)
The title compound has been synthesized in 70% yield by
the condensation of N,N-dimethyl-m-toluidine with Michler's
hydrol in dilute hydrochloric acid. It has not yet been evaluated.
1.2 Carbon Tetrabromide (CBr4)
A 500 g sample of CBr4 was received from Berk Limited's
Chemicals Trading Division (England). This material was manu-
factured in France and was nearly pure white as received. It
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gave excellent film results as received and sublimation did not
alter the film results. A quote on 50 and 100 kg of this material
has been requested. A request has also been made for any avail-
able analytical specifications..
1.2.1 Deterioration Studies
The purification and aging studies with BDIi and Freeman
CBr4 are underway. Chart I outlines- the program. The plan is
to comparatively evaluate the variously purified and stored
samples over an indefinite period of time. In this way it is
hoped that the cause of deterioration can be identified as
atmospheric contamination, method of purification, or the crude
material itself. Comparative mass spectra are also planned to
supplement the film evaluation.
1.2.2 Film Additions of Suspected CBr4 Decomposition Products
It was reported last month (Section 1.2.1.4) that 10 gig of
bromine (17 ppm of CBr4 on a molar basis) had no effect on
photographic properties. This evaluation was extended to
include 100 gig, 300 gig, 500 ?g, and 1 ing. The results in
Table 3 show that 100 gig is detrimental. The 1 mg level resulted
in immediate reaction with the coating solution resulting in
formation of a brown color and the precipitation,of some unknown
material. Interestingly, the behavior parallels that of aging
coating solution described in. Section 1.1.1.2, with the exception
of the precipitation.
1.2.2.2 Tetrabromoethylene
The decomposition of CBr4 to give bromine can be accompanied
by the formation of tetrabromoethylene (C2Br4). The addition of
50 mg to 5/D7 has no effect on photographic properties and no
effect on speed decay. Total replacement of CBr4 with 623 mg of
C2Br4 (maximum solubility) resulted in no photosensitivity in
either printout or development mode.
1.2.2.3 Hexabromoethane 4CZBr6)
Last month's report describes the comparison of 311 mg
C2Br6, hexabromoethane, which is near the limit of
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its solubility, with the standard-1.2 g of CBr4. The
results showed that C2Br6.is a very poor activator with essen-
tially no development capability. The comparison was misleading,
however, because the relative effects of CBr4 at the same low
level were unknown. Of particular interest was the blue printout
image afforded by C2Br6, anal whether CBr4 would also give a blue
image rather than the usual deep magenta, at the lower concentration.
Both printout and development comparisons were made between
CBr4 and C2Br6 at the 311 mg level. The results are shown below:
Development Mode
Dmax Dmin A Tr AEI Y
CBr4: 1.22 0.22 109 sec. 0.70 0.9
C2Br6: - - 960 sec. - -
CBr4:
C2Br6:
Dmax Dmin AEI 1
2.24 0.06 2.8 x 10-4 1.4
0.98 0..07 7.0 x 10-5 0.8
At this level CBr4 still, gives a deep magenta image whose
maximum density is read with the Wratten 94, blue filter. The
blue image with C2Br6 gives maximum density with the Wratten 93,
green filter. Visible spectra of the two images confirm the
fact that little if any D7-dye is formed in the image with C2Br6
while considerable D7-dye is formed with CBr4.
This fact establishes a difference in mechanisms for these
two compounds. It is not known whether D7-dye is formed by
direct reaction between D7 and hydrogen bromide or whether
another mode is operative, such as extraction of hydrogen by D7
radical cation. Whatever the mechanism, CBr4 is capable of
producing D7-dye and apparently C2Br6 is not. This fact should
be valuable in further elucidating the mechanisms of image
formation and optical development.
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 Sanitized Copy Approved for
1.3 NLOxide Program
Release 2010/03/18: CIA-RDP80TO1137A000100010011-7 25X1
1.3.1 4-Picoline-N-Oxide (4P0)
The in-house synthesis of 4P0 has been completed. The
material was purified and dried in the standard manner. It was
found to give film results identical to those obtained with
purchased and. purified 4P0. This completes the standardization
study of 4P0. The ability to synthesize acceptable material
provides insurance against future supply problems and provides
additional assurance that presence or absence of unique impurities
is no problem.
The last two N-oxides (N-36 and N-37) of the current study
have been evaluated. The results of the Phase I study are
being evaluated and will be reported in the future.
1.4 Binder Studies
Nothing to report.
1.5 Environmental Studies
1.5.1 Air Sampling
With more data, the argument incriminating oxidants, which
was presented in last month's report, becomes less persuasive
(Table 4). In the past week we have "good" film, samples 51PQ
and 53PQR, with values of 0.069 and 0.100 mg 03/M3, and "bad"
film, samples 48CH and 48RS, with values of 0.022 and 0.019 mg/M3.
This leaves us with no good correlation at present. Preliminary
data for H2Se and H2Te show no correlation either. A few addi-
tional samplings will be made, using both "good" and "bad" film
areas. There is a time lag. We have taken quite a few samples
for which the data have not yet been reported. We are currently
still sampling for oxidants, HC1, HBr, H2Se, and H2Te. Costs
for the sampling from December 17, 1971 to date are still under
the original estimate for three weeks of intensive sampling.
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 Sanitized Copy Approved for R
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1.5.2 Environmental Contamination: "Good" and "Bad" Films
Previous reports including the proposal for 1972 have
described the. phenomenon of environmental contamination. The
preceding section and last month's report have presented the
results of our air analysis program and have attempted to draw
a correlation between particular contaminant levels and the
corresponding film results. Film results have been generally
described as "good" or "bad." Figure 1 shows some examples of
what is meant by "good" (nos. 5 and 6.) and "bad" (nos. 1, 2,
3 and 4) films. It can be seen that "bad" is a matter of
degree. Although nos. 3 and 4 appear comparable to nos. 5 and
6 and would therefore appear "good." Their D-log E curves
show otherwise as can be seen by comparing Figures 2 and '3
with.4 and 5.
It is not known at this time whether the contamination is
gaseous or particulate, but there is no doubt that it is air-
borne. Figure 1 shows the films results conducted in the darkroom
which is adjacent to the environmentally controlled room. The
controlled room has continually given "good" films as evidenced
by nos. 5 and 6. Film 1 shows the results from the adjacent
uncontrolled room. After the installation of a. plastic, air-
tight ceiling the results was film 2 in which a slight improve-
ment can be imagined. The floors were then cleaned and waxed
and a Barnebey Cheney air purifier was installed. Two days
later the result was film 3: A significant improvement is obvious
but contamination is still prevalent as evidenced by the D-Log E
curve of Figure 2. After another two days the result was film
4 which is essentially identical to film 3 (see Figure 4). Door
jambs were sealed with felt padding and air purification continued.
Another three days afforded film 5 which is "good" as seen by
the D-Log E curve of Figure 4. Four days later the films were
still "good" as seen in film 6 and Figure 5. At a later date
the air-purifier was removed and within 24 hours films were again
like nos. 3 and 4.
1.6 Other Film Systems
Nothing to report.
1.7 Film Analysis of Decay Products
Nothing to report.
-10- 25X1
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 Sanitized Copy Approved for
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1.8 Dye Idcntificatidn
Nothing to report.
1.9 Systems Nonuniformities
Nothing to report.
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 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80T01137A000100010011-7
TABLE 1
AGING STUDY OF STANDARD 5/D7 COATING SOLUTION
Exp. y AEI Dmax Dmin Dnet &Tr Curve ATa
No. B B B sec. Smooth Shape
1769
48-2
1.30
1.10
2.14
.22
1.92
120
2
2
2min.
43-9
1.80
.40
2.06
.26
1.80
120
1
1
5min.
43-10
2.60
.35
2.07
.28
1.79
130
1
1
10min.
43-11
1.60
.40
1.76
.22
1.54
120
1
1
15min.
44-2
1.80
.55
2.06
.33
1.73
120
1
1
20min.
44-3
3.00
.50
2.44
.37
2.07
120
1
1
30min.
44-4
1.00
1.20
1.52
.38
1.14
110
1
0
40min.
44-5
-
-
1.70
.33
1.37
110
-
-
50min.
44-6
1.5
.50
1.50
.33
1.17
100
0
1
1 hr.
44-7
2.40
..13
1.90
.40
1.50
90
1
1
2 hr.
44-8
-
.1
1.42
.37
1.05
90
-
-
3 hrs.
44-10
1.30
.15
1.30
.36
.94
90
1
0
4 hrs.
OTa = Time lapse after addition of activator(s) to coating solution.
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 ~ o . e o
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AGING STUDY OF 5/D7 COATING SOLUTION MINUS D260
Exp. No.
Gamma
AEI
Drnax
Dmin
Dnet
?Tr
Age Com~
1769-
B
B
B
sec.
Days
45-1
1.4
1.1
2.30
.22
2.08
110
0 -
45-2
1.2
2.0
1.95
.24
1.71
130
.16
46-2
1.2
1.5
2.30
.25
2.05
120
2 -
47-1
2.0
.67
2.20
.28
1.92
120
3 -
47-4
1.4
865
2.60
.35
2.25
140
4 Some Blotch
48-1
1.4
1,6
2.36
.24
2.12
130
8 -
49-4
1.6
.32
1.50
.24
1.26
140
15 -
49-5
1,8
6.3
2.40
.37
2.03
130
15 Some Blotch
1824-
Used Another
1-2
1.5
1.2
2.31
.21
2.10
210
23 D260
5-1
1.9
461
2.24
.20
2.04
190
30 0-
9-1
1.5
.35
1.94
.24
1.70
210
37 - 25X1
13-2
2.0
.25
1.50
.16
1.34
130
44 Used Another
D260
18-5
2.8
.38
2.40
.34
2.06
130
52 Some Blotch
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 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7
Addition of Bromine to 5/D7
(Ref. 1833-33)
Br2
Dmax
Dnet
ATr
(sec.)
Comments
1.88
1.67
36
Control
100?g
1.70
1.50
25
300?g
1.34
1.00
18
500?g
1.42
1.09
24
1 mg
-
-
-
Precipitate
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 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7
Ades results reported to us through Feb. 28, 1972.
corresponding to bad film are marked with an asterisk.
r
Arsenic
Sa+rple
Nt_iber
Nl~,
n
Oxi dints,
m:.f[3
,
r _
Ta, HCl F
tr3 E C]. :d3 a Ttr _~ mi~~''a
1
0.011
0.027 0.031 0.0(71 o.OOdt
2
15
08 08 <
007
3
19
.04 90 03
04
4
10
07 1.167 10 <
0(71
5
16
08 08 07 <
007
6
07.
29 11 03
02
7
0:j ,
21 11 08
11
6
11
1.223 11 <
007
9
17
19 23 07 <
007
10
15
03 39 09
05
11
19
12
25
0.026
25
o.64o 02
-13
O6
114
17
23
12
. 09 07
15
05
03
13
12 07
16
14
26
414
0.1(6. o3
17
10
23
13
1.3 03 <
007
-8
01
46
15
0.139 07
2,9
12
17
14
0.184 09 <
007
20
07
10
18
25 06 <
007
21
07
13
22
21 08 <
007
22
12
23
10
21
20
13 0) <
007
24
12
49
08 '
0.360 09 <
'007
<
007
25
* 26
1s
31
CO,
0.128 13 <
007
* 27
12
65
?11
0.161 10 <
0(7
* ?28
12
74
114
94 ?19 <
00?
* 29
08
95
12
24 08 <
007
* 30
52
10
51 09
04
* 31
12
77
11
0.119 03 <
007
* 32
74
0.120 08
al
a 33 .
. 27
0.140 12
34
15
18
+35
- 84
14
20 <
007
36
08
58
19
63 11 <
007
37
02
12
19
0.125 10 <
007
38
07
23
16
49 08
01
39
0.186
32
84 0.110 <
Ocii
ert~ 40
22
0.099
09
0.108 0.1]7 <
01
41
14
0.154
10
0.122 0.131 <
O1
Hz Se H2Te
42
25
21
06
0.101 0.101
01 m 3 6! [3
44
< 05
21
0.035 0.060
45
37
30
0.129 0.2(71
} 46 20
47 06
,r 48cii 22
-
0.11,8 o.024
48F@ 37
0.1'39 0.136
t 48RS 19
0.099 0.113
* 49CH 43
49N 55
51CH 0.114
5u-,Q 69
(#) 52CH . 45
52F:. 43
82
("') 53CH
f?1 rot, n.]rtt)
1.1_52 0.058
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 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7
CBr4 - Deterioration Study
1. Controlled Atmosphere (%0%o N2 and.20% 02 purified)
A. Samples Currently Underway
1. BDH sublimed
a) First sample sublimed yellow
b) Second sample sublimed colorless
3. Newly acquired Berk Limited material
B. Samples Not Yet Underway
1. Freeman (twice recrystallized)
2. Freeman (twice recrystallized and sublimed)
3. Freeman (twice recrystallized and dried over
II. Laboratory Atmosphere
A. Samples Currently Underway
1. BDII sublimed
a) First sample sublimed yellow
b) Second sample sublimed colorless
2. Crude BDH
B. Samples Not Yet Underway
1. Freeman (twice recrystallized)
2. Freeman .(twice recrystallized and sublimed)
P205)
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 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80T01137A000100010011-7
ILLUSTRATION OF "GOOD" AND "BAD" FILMS
-17-
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 1 911+11 I
Sanitized
Copy Approved
for Release 2010/03/18 : CIA-RDP80T0
1.31
1.82
1.90
1.93
1.95
1.97
1.95
1.29
1.78
2.01
2.01
2.07
2.13
2.13
1
2
3
4
5
6
7
6 8
9
10
11
2.8
7:. 7
2.6
{
}
i
t
2.4
2
2
.
.
2
0
;
.
H "4t
7
7
,
. -
..7 47 7
1
i
1.4
1.2
=
77
-
7
:7
=_}
! }=
---- - - -- ~~- -
-
- - -- -r: - - j .- ~ r: _ ' _}===ate
T f
It =-.-z -
77
11717TU-
'
1. .5 16 2.2 2.4. 2 I 3.
1.17 ?
Abs. Log* E
RELATIVE
LOG EXPOSURE
Saniti
zed Copy Approved for Release 2010/03/18 :CIA-RDP80T0
i -I I } I t i
1137A000100010011-7
FIGURE 2
FILM 3 of FIGURE 1
EXPOSURE STATION: No. 2
INTENSITY: 166 me
EXPOSURE TI`fE: .09 sec.
E EXPOSURE:14.9 me sec.
Log EXPOSURE: 1.17
RED LITE STATION:HID2 LAMP:
STATIONARY PLATEN: x OSCILLATING:
RED LITE DEV. TIME:40 sec.
TIME/PASS :
FILTERS USED:2030,RG654 N.D.:
RADIATED POWER:
ROOM TEMP: 70 ?
HUIVTIDITY: 41%
PLATEN TM11P:
1137A000100010011-7
 9+,
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pproved for Release 2010/03/18 :CIA-RDP80T0
1.83
1.84
11.93
1.89
1.71
1.75
2.02
1.88
1
2
3
4
5
6
7
8
9
10
11
1
as
7-'
77
1.6
1.4
fi
1
1
2
._
.
,
r -
J
-
6 f = = 1
.
= t _
t -
_
-- t =
T
t
T
i s
-
_.__. ..
.6 1. 1.5 .8 2.1 z.4 . 2./
1.17,E
Abs. Log E
RELATIVE LOG EXPOSURE
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1137A000100010011-7
EXPOSURE STATION: No, 2
INTENSITY: 166 me
EXPOSURE TIME: .09 sec.
E EXPOSURE:14.9 me sec.
Log EXPOSURE:1.17
RED LITE STATION: HID2 LAMP:
STATIONARY PLATEN:X OSCILLATING:
RED LITE DEV. TIME:34 sec.
TIME/PASS:
FILTERS USED: 2030, RG654 N. D. :
RADIATED POWER:
ROOM TEMP: 70 ?
HUMIDITY: 41%
PLATEN TEMP:
1137A000100010011-7
 ! 1 ~ I I I I I ? a
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1.4
2.8
1.2
.24
.35
.56
1.42
1.62
1.75
1.78
1.86
1.89
1.8
.24
.32
.55
1.31
1.46
1.59
.71
1.83
1.91.
1.93
1
2
3
4
5
6
7
8
9
10
11
_~.=.~
:
t
_
?_
I
t
= r
I8
-
{
-
=t I
?
1.4
17,
---- -- --- --- ---
1
0
.
+
1.
77.
_77 7
=
_ -
=f
c 1 =
r=
{ t
=
=
t ---
.z
-
2
.3
.
1. 5 1. 2.1 2
Log E 1.171'
Abs
.
RELATIVE LOG EXPOSURE
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FIGURE 4
FILM 5 of FIGURE
EXPOSLTE STATION: NQ. 2
1NTENS ITY : 166 mQ
EXPOSURE TIME: .09 sec.
E EXPOSURE: 14.9 me sec.
Log EXPOSURE: 1.17
RED LITE STATION: HID2 LAMP:
STATIONARY PLATEN:X OSCILLATING:
RED LITE DEV. TIME: 45 sec.
TIME/PASS:
FILTERS USED: 2030, RG654 N. D. :
RADIATED POWER:
ROOM TEMM4P: 70 ?
HUiti'MIDITY: 41%
PLATEN TEMP:
Y = 2.5
AEI: 5.5
1137A000100010011-7
 t ! t E ! i i " !
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.23
.26
.40
1.28
1.61
1.71
1.78
1.83
.2.3
.28
.41
1.13
1.46
1,62
1.76
1.89
1
2
3
4
5
6
7
1 8
9
10
1
1
2.8
-
-
17
t.
}
2.4
7 L.
2.0
r
'
t
1.6
7 7
1.2
1.0
-7 7.
:7L
t
I
.8
7
7= =7
77
6
-
.4
7 7-
:r
t7
~-_
0
7 3
2
4
.
.
.
. 1.2 1.5 1. 2.1 2.
Abs. Log E 1.17?
RELATIVE LOG EXPOSURE
FILM 6 of FIGURE 1
EXPOSURE STATION: No. 2
INTE,NS I TY : 166 me
EXPOSURE TIME; .09 sec.
E EXPOSURE: 14.9 me sec.
Log EXPOSURE: 1.17
RED LITE STATION: HID2 LAMP:
STATIONARY PLATEN: X OSCILLATING:
RED LITE DEV. TIME: 47 sec.
TIME/PASS:
FILTERS USED:2030,. RG 654 N.D.:
RADIATED POWER:
ROOM TE1M1P : 700
HUMIDITY: 41%
PLATEN TEMP:
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REFERENCES
2)
4)
6)
Aaron and Barker, J. Chem. Soc. 1963, 2661.
Proposal: January 1, 1972 through December 31, 1972;
Section 2.6, p.40.
Ibid, Section 3.3.1.1, p.48.
Tadaaki Tani, Photograph Sci. Eng.., 1971, 15(5), 384.
Ref. 2, Section 3.3.1.2, p. 50.
Ref. 2, Section 3.3.6.
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 Sanitized Copy Approved for Rel
2.0 ENGINEERING
ase 2010/03/18: CIA-RDP80TO1137A000100010011-7 25X1
2.1 Calibration and Equipment Maintenance
Calibration of all 325B equipment has continued on a
routine basis. All of the HID-2 red light developers recently
completed have been calibrated and tested; and for the first
time multiple 'r.ed light development units have been built
which are identical in processing characteristics within the
experimental error of the present testing equipment.
New designs for portable, exposure and coating stations
are being reviewed for portable coating and processing of the
film in remote areas in support of the environmental studies
program.
2.2 Mechanical
The HID-2 units have been completed, tested and evaluated.
The units have performed well and are presently used for all
processing of the 325B material. Work will continue evaluating
these units and improving red light technology in general.
No work has been done on shelf life because of the contamina-
tion found throughout the building with the exception
of the environmental room presently being used by the chemistry
group.
2.4 Red Light Research and Development
Work is continuing on the HID-1 and HID-2 processing units
to determine the proper filtration for optimum performance of
the 325B film. A series of interference filters has been
received which have nearly identical cut-on characteristics.
These are presently under test to determine if in fact all-
fil-ters are exactly the same when placed in all of the HID-2 units.
These filters have a 50% cut-on point of 665 nm and 655 nm.
Evaluation is not yet complete on the repeatability of these
particular filters.
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2.5 Environmental Conditioning
This is a new section having been added because of the
extreme environmental contamination problem encountered within
the building. As we reported in the last 25X1
report, some form of contaminant has essentially stopped 325B
processing outside of the one environmentally conditioned room
that the chemistry group is presently using.. Tests have been
run in other parts of the building which show this contamination
problem- A large effort is underway to (1) determine the cause
of the contaminant and (2) determine methods for countering
the contaminant. Barnebey Cheney activated charcoal units have
been placed in several laboratories with the hope they will
remove the contaminant, thus cleaning up the room and allowing
experimentation to continue. The engineering darkroom located
in the front portion of the building has had a special double
door, plastic sealing of the room ceiling, and a Barnebey
Cheney unit placed within the room area. This proved inaffectual;
only very slight improvement in film response was observed.
An experiment using 275 cubic foot of 20%0 oxygen, 80% nitrogen
(pure air) was introduced into the room and this made a signi-
ficant improvement in the film samples. This pure air mixture
was dumped directly into the hood where the coating and red
lighting was done. A marked improvement in the samples was
observed. However, upon the room standing idle for 24 hours,
the film produced showed severe blotch. This showed that the
contaminant is airborne and is not contained in a pure air
mixture; however, this method is unsuitable for this type of
room operation and another method must be found which is more
efficient and practical. An alternate darkroom is under con-
struction and consists mainly of a small environment
14' x 8' x 7' constructed in the rear section of the 25X1
building. It will be completely sealed from the surrounding
contaminated air. A Barnebey Cheney unit will be installed
along with a room air-conditioner to maintain temperature and a
double trapped door installed to reduce the airflow of contami-
nated air when entering the room. The room will be pressurized
with an activated charcoal makeup air system, which will cycle
through the Barnebey Cheney unit in a double filtration system.
An exterior mounted vacuum system will be used for daily
cleaning of the area. An air sampling hose will be introduced
so that air samples within the compartment can be made without
contaminating the room with sample vapors. It is anticipated
the room can be completed and tested prior to 1 April 1972.
Information received from testing within this unit should assist
in determining the contaminant, thereby making cleaning of the
air much simpler than the present gross removal system used. If
successful this should lead the way to inexpensive, multiple,
contaminant-free test rooms available to the entire project.
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3.0 PERKIN ELMER INTERFACE, QC/QA
3.1 Supply of Film and Equipment
3.1.1 Delivery of 325B Film
Shipment No.
Date Coated
Date Received
Time Lapse
1
14
Jan.
17
Jan.
2
Days
17
Hrs.
2
31
Jan.
3
Feb.
2
Days
17
Hrs.
3
14
Feb.
16
Feb.
1
Day
17
Hrs.
4
1
Mar.
7 Mar.
5
Days
17
Hrs.
Shipment 1 was delivered by station wagon and was received
in good order. It was successful and is described in the first
monthly report. It consisted of sixty 1-1/2" wide strips of
film with sufficient coating for exposure with a Kodak No. 3,
21 step tablet.
The second shipment was sent by Airborne Freight Corp.
The freight company sent it to the wrong airport causing a
two day delay in reaching its destination. The ten 7" x 7-1/2"
sheets were fogged upon arrival. A possible cause of the fog
is displacement of the air in these individual boxes by CO2
from the dry ice and/or an increase in temperature, even though
the box was still "cool" when opened (see Section 3.3).
. Shipment 3 was delivered or produced in three parts: one
by Airborne Freight Corp., one by station wagon and the third
part. by hand coating in the Perkin Elmer laboratory. The suc-
cess of delivery is judged primarily on the good printout results.
The lack of a good developed film sample prevented the test of
the film from being conclusive. Because the problem could not
be identified with certainty, all of the equipment plus two sheets
of the film were returned. Upon return a subsequent additional
control of the HID-2-004 red light development unit was found to
be operating within tolerances and the film materials used for
hand coating were found to be "probably" good. The quality .
control on the film and ingredients brought back yielded only
probable conclusions because in both cases the effects of aging
were already apparent. A possible cause of the problem'at the
P.E. facility might be air contamination, although at this point
it is not at all conclusive. Air samples were taken in their
lab each of the three days and will be analyzed for oxidants,
hydrogen-halides, tellurium and selenium Although the hand
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coatings made for this purpose appear inconclusive, the analyses
of the air samples will still be useful for establishing a
baseline at their facility and-for comparison with the pollution
profile found at our facility.
Shipment 4 was made for the sole purpose of testing and
solving storage and shipping problems. The shipment spent an
undue amount of time in transit because Airborne Freight Corp.
did not off-load it the first time it was at Bradley International
Airport, and because the receiver could not pick it up onthe
weekend when the freight company finally got it to Bradley. The
use of this film was not totally lost, apparently because some
dry ice remained and none of the film had fogged. Fogging is
the primary indication of problems, which are to be tested
this time. The number of sheets made.for Shipment 4 was only
1/3 of the normal size shipment. Of this only 2-1/2 sheets,
cut up for sample size, were sent. An equivalent shipment was
retained for comparison purposes. The sixth coating was cut
up for coating control purposes.
Perkin Elmer was made aware of the work load placed on the
325B project. The expected need`vill be approximately 15 sheets
of the film twice a month as'originally planned. All understood
that a lost shipment for whatever reason could not be made up.
The estimated cost of each.shipment including time and materials
but not overhead is about $1,000. The date of the next shipment
depends on solving the current storage shipment problem. Up
to now the shipments are still on schedule.
3.1.2 Delivery of Solvent Rinse
One and half gallons of solvent rinse was delivered
16 February with Shipment 3. They now have a total of two
gallons which should hold them until the scheduled shipment of
solvent rinse in mid April.
3.1.3 Delivery of Red Light Development Units
The HID-2-004 unit was sent air freight and received in
good order 7 March. It had originally been shipped on schedule
the second week of February by station wagon. It was not left
at Perkin Elmer because the problems with the developed samples
could not be identified at the time. The unit was returned with
film for more controls and testing. The subsequent controls
show that the problems encountered were not traceable to the
development unit. The earlier model, 4B, was also returned.
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 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80T01137A000100010011-7 25X1
3.2 Cross Calibrations
The comparison of three TD-102 densitometers, one at
Perkin Elmer and two a.t 0 , show that a major discrepancy 25X1
results when using 325B film. The ordinary black calibration
tablet supplied with each densitometer does not reveal any
discrepancy, with the visible or the color filters. The mixed
color portion of an Ektacolor internegative tablet supplied
by P. E. used as a second check, shows a discrepancy but not
of the same magnitude as revealed by the 325B tablet. With
the Ektacolor tablet, the P. E. blue filter density is only
0.01 density units above the reading when using the 325B
filter at a density of 1.43 (Figure 5). With the 325B printout
sample processed at P.E.'s lab, the density discrepancy at the
1.5 range is 0.11 density units. The Dmax read with P.E.'s
densitometer is 3.73 (Figure 1); with the same type instrument
used in another department, 3.20 (Figure 2); with the 325B
densitometer, 2.70 (Figure 3). One of the defects in making
this comparison is the fact that the 325B tablets are not uni-
form enough to rely on exact positioning of the film in all
three of the densitometers. The data plotted to this point,
therefore, is only indicative and cannot be used quantitatively.
Color ratios which could be compared quantitatively
between the three units, were plotted. The color ratio in
the case of interest is the ratio of the density through the
blue filter over the density read through the green filter of
the TD-102 densitometer. They are read by placing the reading
head of the densitometer down on one spot, and then changing
the filters after the unit has been calibrated for each filter
using the standard silver tablet. In this way the color ratio
can be derived. without worrying about replacing the densitometer
on the exact spot. The plots comparing the ratios of the three,
densitometers on the color tablet (Figure 6) as well as the
325B tablet (Figure 4), reveal unequivocally that there is
a major discrepancy in the densitometers when reading 325B material.
They also show that 325B color might vary with density. At
the higher density range, the blue/green ratio of the 325B
densitometer is the highest; the same type instrument from
another department is the lowest; and P. E.'s densitometer falls
in between. This comparison gets mixed below 1.0 densities.
Furthermore, there results in a much sharper rise and drop in
the color ratio of P. E.'s densitometer going from the eighth to
the eleventh step. This explains why P. E.'s plots of the
325B material have such a sharp shoulder at the ninth step when
reading through the blue filter.
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A plot of ratios also points out that the Ektacolor
tablet will not be a suitable standard for calibrating the
densitometers for 325B film. The comparison of the three
densitometers on a ratio plot shows them to be very close
and to follow each other across the range of the color
tablet. One must note that the color ratios of the densi-
tometers do drop as the densities become higher than the fog
levels and then rise again. This apparently is a characteristic
of the manufacturer's design of the densitometers. This
apparently is the reason why the 325B color "appears" to change
with density in Figure 4. The plot of the 325B film could be
corrected by normalizing against the plot of the Ektacolor
ratios.
The probable reason for the densitometer variabilities is
the very sharp color profile (Figure 7) of 325B film in the
blue and red regions. The convolution of the 325B color with
the color curve of the densitometer filter, lamp color, and
phototube color detectability is very sensitive to any non-
comparability of any of the densitometer components. MacBeth
Corporation does not attempt to make color densi.tometry duplicatable
between TD-102 instruments. They recommend making a nomograph
of correction values which would mean replotting of all curves
before comparing D-Log E curves generated at different facilities.
The densitometers, therefore, must be.'calibrated with sharp
filter cut-ons in the critical 325B regions.
It is advantageous to choose that filter which gives us
the highest density readings of 325B film. The implications
of the 325B color have been presented in three previous studies:
identifying maximum density wavebands with a radiometer,. checking
out a suitable light table color, and maximizing the printing
efficiency of 325B negative onto the PH 2000 duplicating film.
Based on the plot of maximum density vs. wavelength (Figure 7),
narrow band interference filters at 480 nm and 540 nm instead of
the standard Wratten filters at 455 and 540 nm will yield the
highest density and will provide the necessary color ratio for
the comparisons which have been a valuable tool.for judging
chemistry work and quality control. A 10 nm 1/2 peak bandpass
interference filter is a practical compromise between cost,
availability in quantity, maximum transmission (50%), and the.
narrowness needed to minimize the deviations of source and
detector color.
This report does not identify completely the reason why
the samples processed at their facility yield such high densities.
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In spite of the difference in densitometers, the samples
processed at P. E. had a significant increase in density
above what is normally attained at The real density 25X1
increase appears to be caused ty the fact that their printouts
are done with an EK-101 sensitometer with a 2850?K color
temperature. Compared to the daylight exposure of 5500?K, their
exposures of 200 seconds to 1700 meter candles allows signi-
ficant development as well as production of latent image.
Without the Pitt 2043 heat absorbing glass, the exposure and
development occurs above room temperature. Temperature signi-
ficantly affects printout results (reported in June, 1970,
325 Progress Report). By removing the color correction CG 5900
and Pitt 2043 filters from one of the sensitometers, the 25X1
same increase in densities was produced at Because 25X1
of the end use of the film, the printouts as well as the exposures
for the developed film, must be done with the correction filters
in place to produce 5500?K color temperature as well as a mini-
mum amount of YR. The daylight correction, therefore, must
extend out into the infrared region, also. The two filters
were taken along with Shipment 3 and the above effect was demon-
strated at P.E. Their exposures will now be done with those
filters.
3.3 Evaluation of Production, Shipping and Contamination
Two problems have come up within the last month; the
air carrier has performed very poorly two out of three times.
The first time he sent it to the wrong airport; the last time
it went from Boston to Chicago before it was correctly off-
loaded at Bradley International Airport. Future mistakes
will be circumvented by sending the film either by charter plane
to Danbury Airport or by using American Airlines priority parcel
service to LaGuardia Airport. The reliability of shipment is
especially important because of the costs of the film shipment,
which is approximately $1000, and of the delay in project per-
formance at P. E. Although the time involved in hand coating
limits the amount of film that can be shipped, the primary cost
is still the synthesis, purification and quality control of the
materials.
The other problem that has appeared in February is the fogging
of film in storage. Ten percent of Shipment 1, all of Shipment 2
and the 30% of Shipment 3 that was left at P. E. fogged to about
1.0 density. On the other hand the last samples used from
Shipment 1 after four weeks of storage were not fogged and still were
up to speed. Shipment 4 was set out to test this and find a
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secure way of sending the film. Unsealed shallow boxes were
used for the first two shipments; shallow boxes are necessary
because the film is still wet when it is placed in storage
and then frozen within two minutes of coating. The third
shipment included putting the boxes in unsealed polyethylene
bags, which in turn were placed inside unsealed black light-
tight bags. A fourth shipment included packaging that dupli-
cated the first three shipments, plus an additional sample
sealed in an air-tight metal tube. The di lacement of air as
a cause of fogging has been observed at when argon or 25X1
CO2 was purposely used to displace the air. Time and tempera-
ture were also observed to bear upon the problem. One sheet
that was retained was allowed to have its surrounding air
displaced by CO2 and then warmed to approximately 40?F around
the edges only. Because the outside edge was fogged and the
center was still useful for sensitometric evaluation, the
test indicated that the lack of the oxygen inhibitor plus
a "warm" temperature was needed to cause fogging. Shipment 5
will be sent under the conditions demonstrated by the results
of Shipment 4.
That the air at the P.E. facility may be contaminating
our film is not being overlooked. The three sets of air samples
taken the 16, 17, and 18 of February will. be used to hopefully
shed some light on the subject. The problem involved in
evaluating this data is formable (see Sections 3.7 and 1.5).
3.4 Monitoring of Results and Anticipation of Subsequent Plans
The first shelf life study at P. E. was begun with Shipment 1.
The data and conclusions will be reported in the monthly report
from P. E. It was in regard to this that the Corning Glass 5900
and Pitt 2043 filters were supplied with Shipment 3. Because of
the demonstrated difference that the source color has on the
film, the shelf life study up to now will have to be repeated
using the 5500?K source. The results of 2850?K and the future
results of 5500?K will be coordinated with the shelf life study
going on concurrently at In particularly, one point 25X1
to be evaluated is the importance of establishing a starting
point of the decay curve since the film P.E. uses might already
be aged.
The possibility of using their environmental chambers for
test and evaluation of storage and sensitometry of our film
under a variety of conditions was brought up. In the laboratory
adjoining P.E.'s 325B lab is a vacuum chamber that has been
instrumented for photographic evaluation of film under camera
vehicle environments. A test plan based on the use of this
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equipment is being established. Past and concurrent work at
using glove boxes will be coordinated with their test 25X1
plan. P. E.'s vacuum chamber is equipped to go to deep vacuums
as well as duplicate actual camera environments. It has the
advantage of being fully instrumented with controls and moni-
toring probes. Throughputs are available for working on the
film in a photographical and mechanical way under the variety
of environmental conditions. To start with, it will be useful
for evaluation of storage problems. The program can then
advance to environmental conditions during exposure and develop-
ment. Previous offgassing data was generated with this equipment.
3.7 QC/QA
The supply of chemicals and materials for standard formula
5/D7 has been keeping comfortably ahead of usage rate, in
spite of one accidental loss of,a quantity of D260. The quality
of materials found acceptable by the coaters has decreased
somewhat. The materials.that yielded a Dmax of only 2.0 and
a a' above 3, has been accepted for chemistry work. This
has been acceptable for much of the screening work in the
chemistry section. The reason for accepting these materials
is the same as the reason for not filtering each coated sample
and for not adding silicone in each case; i.e., the "cosmetic"
defects do not hinder the reading of the necessary data. The
supply of materials from ChemSampCo has been increasing, especially
since the identification of TMB as an impurity. The new D260
synthesis route being worked on at is expected to yield 25X1
higher and more consistently high quality D260.
Sensitometry within our facility has remained consistent
over the last several years and is being maintained at a high
quality. Sensitometers andthe development units are routinely
checked. Comparisons of our data with data that might be
generated outside the facility runs into the problem explained
in Section 3.2. The use of our MacBeth TD-102 densitometer,
Gamma meter, and averaging technique has been such as to maintain
consistency within the 325B project.
A major problem for maintaining the engineering R and D?
schedule has been environmental contamination. Additional
Barnebey Cheney charcoal filtering units for air filtration
have been ordered. Three of the four cabinet units have been
delivered. Difficulties in securing delivery from Barnebey
Cheney has delayed upgrading additional coating rooms. Each
unit contains six panels with a total of 42 lbs. of activated
charcoal, type CH, and delivers 400 cfm of filtered air. That
has been sufficient for the one room which is approximately
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2200 cubic feet in volume. A small adjoining lab of approximately
2000 cubic feet should be ready for daily use the second week
of March. Difficulty has been experienced with the engineering
darkroom of 2600 cubic feet. A fourth Barnebey Cheney cabinet
unit should be delivered by the end of March. At that time at
least three, possibly four, rooms should be in full operation.
Experience has shown that the 42 lbs. of charcoal is good
for at least one month of continuous operation. Apparently
larger amounts of charcoal/cfm will be necessary for the larger
labs with particularly severe contamination problems. Type CH
charcoal, according to the Barnebe.y Cheney Company, is particu-
larly suitable for filtering out sulphur dioxide, hydrogen
chloride, chlorine gas and other acid gases. As with any
activated charcoal the effect of filtration is very broad with
.respect to the type of contaminants removed. The impregnant
only optimizes the efficiency with regard to certain contami-
nants. Ozone for instance continues to be converted to 02
in spite of the impregnant. Although a fiber glass filter is
provided ahead of the activated charcoal, it is not effective
against particulates to the extent desired. The RFQ that was
put together for clean chemistry rooms and submitted to a list
of suppliers revealed that "economical" off-the-shelf units
all had precise control with regard to temperature and relative
humidity. Our primary need is filtration and purification of
the air. The temperature and relative humidity need-to be main-
tainedat a reasonable 72 +2?F and 40 to 50% relative humidity.
As the rooms are upgraded, the use of "hats and booties" and
other procedures typical of a machine coating facility will
be instituted.
The identification of the air contaminant producing film
problems from the extensive gas samples has not proved fruitful.
The most recent results received from the analytical lab seem
to go against the earlier observation that oxidants are the
possible sources of "bad" film (see Section 1.5). Because of
the large number of samples taken, the evaluation of the data
lends itself to frequency diagrams (Figures 8 through 12). The
data is presented in Table 4, Section 1.5. Although there is
considerable overlap of the data, the frequency diagram will
distinguish two separate signals if there is a correlation between
"good" and "bad" film samples. On this basis a higher level of
oxidants show a correlation with bad samples, which was somewhat
obvious from the run down of the data on Table 4. In addition
the frequency diagram shows a positive correlation with a
slightly higher concentration of HBr, which was not so obvious
on Table 4. The levels of the contaminants found are low enough
that general air pollution in the Cleveland area cannot be
overlooked!
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. 10
1. _
Y,
.10
.21
.52 11.021
2.34
3.13
.56
3.22
.10
C
/
~
.10
.21
.50
1.01
2.30
2.93
,2.96
2,* 4
1
2
3
4
5
6
7
8
9
10
11
I
I
1
1
i
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:
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8
.8
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.
1.2
1.0
_J r
1.7
I
NE
.2 - -
-
e.
6 1.L 2.5 I. 2.1 2.4 2.7 3
Abs. Log E 4.53'
RELATIVE LOG EXPOSURE
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FIGURE 1
P. E.'s TD 102 DENSITOMETRY
FORMULA 5/D7
Exp. and Fix: P. E. 18 Jan'
Densitometry: P. E. 18 Jan
25X11
Shipment 1
Box 23
Sample No. 4
EXPOSURE STATION: P.E.'s EK 1
INTENSITY: 1700 mo Filters
EXPOSURE TIME: 200 sec.
E EXPOSURE: me sec.
Lo; EXPOSURE: 4.53
RED LITE STATION: No RLD
STATIONARY PLATEN: OSCILLATING:
RED LITE DEV. TIME: sec.
TIME/PASS:
FILTERS USED:
RADIATED POWER:
ROOM TEMP:
HUMIDITY:
PLATEN TEIvIP:
.Blue Green
1 - 5.2 4.6
AEI: 2.0x10-4 2.1x10-4
01137A000100010011-7
 -CGHRE 2 ?
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3309
2.76
Z, 77
-
-i
`
}
t
t
-
_.. _ ..
_ .. - -
--- ?.-
_..1 .-- _.. ... ~.
1
7
7.
77
Lm=~-
7--
7
_4
__ .
T
iZ:
l
t
}
M
cgL
-
r-
L
5
TD 102 DENSITOMETR'5X1
FORMULA 5/D7'
Coated:
Exp. and Fix:
Densitometry:
14 25X1
18 Jan.
-25X17
Shipment 1
Box 23
Sample 4
EXPOSURE STATION: EK 101
INTENST`r.': 1700 me No Fi
EXPOSURE TIME: 200 sec.
E EXPOSURE: me sec.
Log EXPOSURE: 4.53
RED LITE STATION: No RLD.
STATIONARY PLATEN: OSCILLATING:
RED LITE DEV. TIME: sec.
TIME/PASS:
FILTERS USED:
RADIATED POWER:
ROOM TEMP :
HUMIDITY:
PLATEN TEMP:
Blue Green
7 = 4.0 3.9
AEI: 2.7x10-4 2.9x10'4
RELATIVE LOG EXPOSURE
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 RELATIVE LOG EXPOSURE
Abs. Log E 4.53 '!'
FIGURE 3
325B's TD 102 DENSITOMETRY
FORMULA 5/D7
Coated: 14 25X1
Exp. and Fix: P. E. 18 aan.
Dens itome try: 325X1>.
25X1
Shipment 1
Box 23
Sample No. 4
EXPOSURE STATION: P.E. EK 1
INTENSITY: 1700 me No F
EXPOSURE TIME: 200 sec.
.E EXPOSURE: me sec.
Log EXPOSURE: 4,53
RED LITE STATIONNQ RLD LAMP:
STATIONARY PLATEN: OSCILLATING;
RED LITE DEV. TIME: sec.
TIME/PASS:
FILTERS USED
RADIATED POWER:
ROOM TEMP:
HUMIDITY:
PLATEN TEMP:
-Blue . Green
1 4.60
AEI: 2.3x10-4 3.7x104
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1i -I-' I
1WAC
.10
(aptewd
x
1 I [ 1 t
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.26 1 .54
2.06
:a_ Z
7
Z.
.7 7-
2-
-7
7
-
777
a 7.
i~ -
I
77
-
77
F.
-777
-7=
i
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=1
i =
-4;
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=
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-77
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7= T
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7= 77
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FIGURE 4 .
COMPARISON OF 3 TD 102 DENSITOMETERS
_.__ ..~ BLUE FILTER DENSITIES
GREEN FILTER DENSITIES
P325B 2850?K, PRINTOUT AT P. E.
E-4
H
z
1.40
1.30
W H
1.20
Z
w
1.10
t7
1.00
a
M
0 0.90
0
Ei 0.80
0 Perkin Elmer's TD-102
x TD-102
A Project 325B's TD-102
Step 3 4 5 6 7 8 9 10 11
Average 0.12 .24 .53 1.06 2.26 3.21 3.12 2.97
Blue
Density
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-777T77
-
7
~
I
1
-LELi
1
4
'
t
mo
-
1) P.E.'s Densitometer
21 I n-nc i ------
COMPARISON OF 3 DENSITOMETERS
With Blue Filter,
Ektacolor Internegative Tablet
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1
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FIGURE 6
COMPARISON OF 3 TD-102 DENSITOMETERS
RATIO OF BLUE/GREEN FILTER DENSITIES
EKTACOLOR TABLET
o Perkin Elmer's TD-102
X
TD-102
A Project 325B's TD-102
0.90 t \~ s
I I
Step 3 5 6 7 8 9 10 11
Average 0.16 0.21 .26 .35 .49 .70 .97 1.23 1.40
Blue
Density
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V'S
0.1
-2
3.6
1
18
19
1.0
1.1
1.2
.9
1.1
1.2
1.3
1d
1 ,25X1
700 750"
No. 1674-24-19 325A 5/D7
edLum,Low Density Segments
21 Apr. 197
DATE_
COLOR PROFILE OF 325B FILM
-1 at
II HIGH, MEDIUM, and LOW DENSITIES I
~
SCAN SPEED FAST_ OPERATOR F, W . S.
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NO2
Total Population
23 + 10 = 33
FIGURE 8
FREQUENCY OF GOOD AND BAD FILM DAYS
VS.
BRACKETED NO2 CONCENTRATIONS
0
0
oI
0 to.3 6
21
AVERAGE
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24 27
ppm
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OXIDANTS
Total Population
13 + 22 = 35
.... 0 ao
0
19
Good
a
70
FIGURE 9
FREQUENCY OF GOOD AND BAD FILM DAYS
VS.
BRACKETED OXIDANTS CONCENTRATIONS
0
80 90 100 110 120 130 140 150 160 170 180 190 200 ?g/M3
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 FIGURE 10
FREQUENCY OF GOOD AND BAD FILM DAYS
VS.
BRACKETED X2 CONCENTRATIONS
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AVE. 17.5 14.6
u-T
0
0 2 4 6
1 16 1 20 22 24 26 28 30 32 34 36 38 40 42 44 ?g/M3
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 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7 -- .
Total'Population
20 + 13 = 33
Oqo
11
w 5
Total Population FREQUENCY OF GOOD AND BAD FILM DAYS
16 + 13 = 29 VS.
FIGURE 11
o ._ _
10 20 30 40 T50
AVERAGE Good
25X1
O r 0 i . 1 . i i Q I I (1~_I 1 g 1~-i ri
60 70 80 90 100 110 120 130 140 150 160 170 180 190 200
0 0
o -~
0
0 0
80120 160 200 240 280
ad T Good
RAGE
0
320 360 400 440 480 520 580 600 640 680 720 760 800 840 880 920 960 1000 1040 1080 1120 1160 120Q 12.4
Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7
 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7
HBr
Total Population
FIGURE 12
FREQUENCY OF GOOD AND BAD FILM DAYS
VS.
BRACKETED HBr CONCENTRATIONS
o
V~~
(J o
9 10 11 12 13
T
Bad
oo~
49 Br-/M3
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 Sanitized Copy Approved for Relea
1) As of February 28, written authorization to proceed not
received.
2) Determining the exact air contaminants that produce film
blotch. '
3) Delivery of laboratory chambers for baseline speed decay
measurements. Two of three chambers received were defective.
4) Shipment of film sample to Perkin Elmer.
5) Slippage of schedule on engineering experiments on reacti-
vation and overcoating.
Press to secure three usable laboratory chambers.
Attempt engineering reactivation and overcoating work.
3) Continue chemical R and. D work according to schedule
possible with one laboratory chamber.
Project is within labor and materials forecasts.
-45-
25X1
Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7
 Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7
Sanitized Copy Approved for Release 2010/03/18: CIA-RDP80TO1137A000100010011-7