ENCLOSED IS OUR PROPOSAL FOR AN ADDITIONAL EIGHT-MONTH PERIOD OF RESEARCH ON THE DEVELOPMENT OF A HYDROGEN GENERATOR (TASK ORDER NO. C).

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP78-03642A001300010057-4
• Release Decision: RIPPUB
• Original Classification: S
• Document Page Count: 21
• Document Creation Date: December 22, 2016
• Document Release Date: May 31, 2012
• Sequence Number: 57
• Publication Date: January 5, 1959
• Content Type: LETTER

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In replying please address:
January 5, 1959
Enclosed is our proposal for an additional eight-month
period of research on the development of a hydrogen generator
(Task Order No. C). It is based on recent discussions with your
technical representative.
In connection with the performance of the proposed re-
search, it is our understanding that your technical representative
will provide one balloon for use in the full-scale experiment and
120 pounds of sodium borohydride.
We are looking forward to working together on this proposed
program, and would appreciate any efforts made to expedite con-
sideration of this proposal, so as to minimize the lapse in the
continuity of the activity in connection with this research. If
you should have any questions with regard to our proposalg please
let us know. Any inquiries of a contractual nature may be directed
to at Extension 159.
Very truly yours,
In Duplicate
CONF\DENTa
CONFIDENTIAL
Vice President
L~EIC REEV 1 T! lY _.f322
OM CLASS
JUST *.. XT X- Y Nn a A T"41 A. 70-2
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CONFIDENTIAL
PROPOSAL
on
THE DEVELOPMENT OF A HYDROGEN GENERATOR
INTRODUCTION AND OBJECTIVES
On May 29, 1956, an effort under Task Order No. C was
undertaken that was directed toward the development of an experi-
mental hydrogen generator capable of generating enough hydrogen to
provide 250 lb of lift at sea level (about 3,500 cubic feet of
hydrogen) over a period of 45 to 60 minutes. Under Phase I of this
research program, a literature search was performed; an analysis
was conducted of various potentially applicable systems and a
selection was made of the most desirable system compatible with the
Sponsor's specifications for the generator of interest; a laboratory
investigation was conducted on the characteristics of the selected
hydrogen-generating reaction; and the preliminary design of an ex-
perimental full-scale generator was prepared. The system selected
involved a reaction of cobaltous chloride hexahydrate (catalyst)
with sodium borohydride. Laboratory experiments showed this re-
action to be practicable for producing the required amount of
hydrogen. The proposed design for the experimental full-scale
generator consisted of a rubberized-fabric cylinder about 8 feet in
diameter and 3 feet in height. The experimental unit was expected
to contain about 560 gallons of solution corresponding to a depth
of 1-1/2 feet; the additional height was to provide foaming space
above the solution.
CONFIDENTIAL
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. .
Subsequently, under Phase II of this research program, the
effort was directed toward the further development and evaluation of
an experimental full-scale generator based on the preliminary design
prepared under Phase I. The principal problem anticipated under
Phase II was maintaining control of the total generation time in
the course of scaling up from 1/100 scale (the size of the experi-
ments involved in the laboratory studies) to full scale (as repre-
sented by the generator of interest). The cobaltous chloride -
sodium borohydride hydrolysis is a heterogeneously catalyzed reaction.
The chemical kinetics and, therefore, the total generation time of
this reaction are strongly influenced by the distribution of the
catalyst through the system. In view of the high cost of the
chemicals involved, an experimental 1/5-scale generator was designed
and prepared, to facilitate the investigation of the effects of
catalyst distribution and rate of solution of the borohydride on the
operation of an experimental full-scale generator. Based on the re-
sults of 1/10- and 1/5-scale experiments conducted in the experi-
mental 1/5-scale unit, the design of the experimental full-scale
generator was finalized. After this unit was prepared by a commercial
fabricator, a handling technique and an operating procedure were
developed for use in a full-scale generation experiment.
A full-scale experiment was carried out under field con-
ditions on August 5, 1958; it was mutually considered to have been
quite successful. This experiment also served as a demonstration of
the one-man operation of the experimental unit, and involved balloon
handling by your technical representatives. The proceedings were
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recorded on movie film; a detailed review and summary of the results
of, and the conclusions drawn from, the proceedings were presented
in a letter dated August 21, 1958, to your technical representative.
As a result of the full-scale demonstration, a review of
the film, and several recent discussions, your technical representative
has suggested that additional consideration be given to selected
areas of study in an attempt to firm up further the operation of the
unit. These areas are primarily concerned with the proper procedure
to be used in operating the experimental full-scale unit at low
temperatures, e.g., at about 35 F, and the adaptation of the pro-
cedure to operation on dry land. Also, there appears to be a need
for certain modifications and/or additions to the experimental
generator; these are directed toward minimizing the possibility of
rupture as a result of the build up of excessive internal pressure.
The program of research proposed herein and hereafter identified as
Phase III describes an investigation directed toward achieving the
above-indicated objectives.
DISCUSSION OF THE PROBLEM
Two general types of problems are anticipated with regard
to the generation of hydrogen at near-freezing temperatures: those
associated with the chemical reaction and those pertaining to the
mechanical aspects of the experimental generator. The handling of
the experimental unit on dry land and the prevention of rupture are
problems which are associated mostly with the mechanical aspects of
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the experimental unit. The two categories of problems are discussed
in some detail in the following.
The Chemical Problem
The Phase II studies were concluded with a full-scale ex-
periment and demonstration of the entire hydrogen-generation procedure.
The full-scale experiment was run at 82 F in a natural body of water.
Based on data obtained previously, approximately 8 pounds of catalyst
were used, and generation was successfully concluded in 26 minutes.
The chemical problem stems from the fact that excessively
large quantities of catalyst are required in order to achieve total
generation within 30 to 40 minutes, and possibly within 60 minutes,
at low temperatures (i.e., at temperatures below 50 F); for example,
based on the previously obtained data, it appears that at 37 F ap-
proximately 100 pounds of catalyst is required. Such a large
catalyst requirement introduces three major problems: (1) in view
of the limit of solubility of the catalyst in water, such an amount
of catalyst is more than can be dissolved in water to provide ap-
proximately 5 gallons of catalyst solution; (2) the amount of catalyst
solution needed would be too heavy to be handled by one operator as
a single "package"; and (3) the initial surge of hydrogen that oc-
curs when the catalyst solution mixes with the borohydride solution
might be uncontrollable when such a large amount of catalyst is used.
Thus, it appears that the resolution of the chemical problem
lies in decreasing the amount of catalyst required for cold-
temperature operation (i.e., temperature < 50 F) while still generating
the required amount of hydrogen within 60 minutes.
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The Mechanical Problems
The mechanical problems of cold-temperature generation are
concerned with (1) the rate of flow of the catalyst solution into
the experimental generator, and (2) the pressure that is built up
inside the experimental unit as a result of the substantially in-
stantaneous reaction which occurs when the catalyst solution first
contacts the borohydride solution.
The full-scale experiment, which was run at 32 F using a
relatively small amount of catalyst, showed that the substantially
instantaneous release or surge of hydrogen can cause noticeable
pressure inside the experimental generator. Consequently, it is
believed that the relatively large amount of catalyst which must be
used at low temperatures may well increase the internal pressure
beyond the strength capabilities of the experimental generator.
The area of the top of the experimental full-scale unit is approxi-
mately 7,500 square inches, and the manufacturer has estimated that
the unit can be expected to withstand pressures up to 1/2 psi
satisfactorily. In order to prevent the build up of higher pressures,
it appears that the flow of the catalyst solution into the experi-
mental unit should be extended over a longer period of time. It is
believed that this period of time can be reasonably reliably estimated
on the basis of small-scale generation experiments. After the entry
time was estimated, it would be necessary to investigate the size
and number of entry holes needed in order to attain the desired rate
of catalyst flow into the experimental full-scale generator.
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Even with reasonable control of the initial surge of
hydrogen, it is quite possible that excessive internal pressure
might be built up as a result of blockage of the outlet tube, for
example, as a result of twisting. Consequently, a relief valve
could be used advantageously. A satisfactory valve for this purpose
would have sufficient capacity to permit the passage of a large
amount of gas at 1/2-psi maximum pressure. The accuracy of relief
valves at such a low pressure, and particularly of those with large
capacities, is questionable if it is necessary to keep the valve
simple, as is the case here. However, it appears that a suitable
valve might be prepared for the experimental generator rather simply -
by providing for the pressure to act against the weight of a part
rather than against a spring. Thus, such a valve might include a
simple lid-type part the weight of which was designed to permit the
relief of gas at about 1/2-psi maximum pressure. This type of re-
lief valve might readily be incorporated in an appropriate con-
nector (to connect the outlet of the experimental generator to the
filler tube of the balloon), the design and preparation of which
have been included in the consideration described herein, at the re-
quest of your technical representative.
The problems of handling the experimental generator in an
operation conducted on dry land can only be estimated at this time.
However, it currently appears that dry-land operation of the ex-
perimental full-scale generator is quite feasible.
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PROPOSED METHOD OF PROCEDURE
Chemical Problem
From the chemical point of view, the Phase II studies can
be summarized in terms of the relationship between amount of catalyst
and temperature, particularly at the upper part of the probable
operating-temperature range. To achieve satisfactory generation, all
other factors being fixed, it is necessary for the operator to add
the proper amount of catalyst; this is based on the temperature of
the borohydride solution. This part of the proposed program would be
directed toward establishing the relationship between amount of catalyst
and temperature at near-freezing temperatures, so as to provide for
generation within 60 minutes in low-temperature operations.
As currently contemplated, the proposed effort in connection
with the chemical problem would be directed toward reducing the amount
of catalyst required, so that it could be dissolved in water to provide
5 gallons or less of solution; and toward minimizing the surge which
occurs at the start of generation. Five gallons of saturated cobaltous
chloride hexahydrate - water solution, at about 32 F, contains approxi-
mately 40 pounds of catalyst; this is an estimate based on consideration
of the available data. Emphasis in the proposed effort would be placed
on attempting to develop a procedure for generating hydrogen in the
experimental full-scale unit using this amount or less of catalyst.
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1/10-Scale Experiments
As currently planned, two approaches would be used in
investigating the chemical problem. In the first, the amount of
catalyst would be reduced to the equivalent of 40 pounds per full-
scale generation, and generation-time data would be obtained as a
function of initial borohydride-solution temperature. If generation
times of 60 minutes or less were obtained at low temperatures (such
as 35 F), it probably would not be necessary to perform any ad-
ditional research on the chemical problem. On the other hand, as
we expect from our knowledge of this system, the low-temperature
limit in the first approach (i.e., the lowest temperature at which
a 60-minute generation time is obtained using 40 pounds of catalyst)
may occur at about 40 F or slightly higher. Then, it would be neces-
sary to attempt to increase the generation rate at the near-freezing
temperatures in another manner.
In this second approach, the borohydride concentration would
be increased by decreasing the amount of water used to prepare the
borohydride solution. (In terms of the experimental full-scale unit,
this means that less than 560 gallons of water would be used to
dissolve the borohydride.) Thus, less catalyst would be required
to perform the desired generation within 60 minutes.
Previously obtained data have shown that, at about 65 F,
reducing the catalyst concentration by a factor of two increases the
total generation time by about 50 per cent. If this relationship
holds at low temperatures, then in order to perform the generation
within 60 minutes using 40 pounds or less of catalyst, the borohydride-
solution temperature probably cannot be below about 40 F. It is
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probable, therefore, that both approaches would merit investi-
gation, in an attempt to adjust the operating procedure appropriately
for application at low temperatures.
In the proposed study of these two approaches, it is cur-
rently anticipated that ten to twelve 1/10-scale generation experi-
ments would be conducted; these would be aimed toward obtaining more
data on the catalyst-temperature relationship for cold-weather
generation. Five or six of these would be run in the approximate
temperature range of 35 to 4,5 F using the "standard" borohydride
concentration, namely, 100 pounds of borohydride per 560 gallons of
water. The amount of catalyst used would be selected in an attempt
to achieve a total generation time of 60 minutes or less. This part
of the proposed program would provide data on (1) the catalyst-
temperature relationship appropriate for cold-weather generation, and
(2) the low-temperature limit for generation within 60 minutes at
the "standard" borohydride concentration.
If, as expected, the low-temperature limit is found to be
above 35 F, then five or six 1/10-scale runs would be carried out
within the same temperature range (35 to 45 F) at an increased boro-
hydride concentration. Examination of our available data indicates
that a borohydride concentration requiring about 350 gallons of water
for cold-weather full-scale generation would probably be appropriate.
This concentration would lead to a total temperature rise of about
93 F in the course of the reaction, as compared to that of about
58 F in the present system involving the "standard" borohydride con-
centration. Under cold-weather conditions, this temperature rise
would not be expected to present any problems. The results of this
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part of the proposed program would also provide information pertinent
to the catalyst-temperature relationship for cold-weather operation.
In an attempt to obtain an adequate understanding of the
surge problem, it is proposed to scale down the outlet on the ex-
perimental small-scale generator; this would facilitate observation
of any pressure build up as a result of the surge during the small-
scale generations. It is also currently planned to conduct a few
laboratory-size experiments to examine the substantially instantaneous
nature of the initial reaction between the catalyst and sodium boro-
hydride at about 35 F. The purpose of these experiments would be to
recheck the quantitative data obtained in earlier studies at higher
temperatures. These experiments would also yield measurements of
the heat of this reaction; these data would help in gaining a better
understanding of the initial temperature rise associated with the
reaction.
It is currently contemplated that, after the above-
described research was conducted, sufficient information would be
available to provide a basis for full-scale generation under low-
temperature conditions. However, it is considered worth while to run
one or two 1/10-scale experiments at an available field site before
conducting the full-scale experiment at that site. These small-
scale runs would serve to confirm the results obtained in the previously
described experiments and also to increase the reliability of the
conclusions drawn.
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Full-Scale Study
Our previous studies have shown that the small-scale runs
(i.e., the 1/10- and 1/5-scale experiments) can be used to establish
the reliability of this system with a fair degree of accuracy. How-
ever, sufficient reliability with regard to full-scale operation can
be established only on the basis of a full-scale experiment; the
many parameters which enter into the scaling-up problem cannot be
entirely accounted for except as they manifest themselves and/or
interact in the course of a full-scale generation.
It is currently planned that one full-scale experiment
would be conducted with the experimental unit on dry land, at a
temperature of 35 to 40 F. Prior to this, any modifications that were
investigated as described below and were considered mutually to be
satisfactory would have been incorporated in the experimental full-
scale unit, within the limits of the time and funds provided. The
catalyst and the borohydride concentrations used would be selected
on the basis of the results of the small-scale runs. As in our
previous full-scale effort, provisions would be made to assist your
technical representative in collecting the hydrogen in a balloon.
However, to facilitate the performance of this experiment and for
purposes of economy, it is currently planned that this run would be
conducted in a manner that would not provide a one-man demonstration
of the experimental unit; it appears expedient for us to plan to
provide a fair amount of assistance in setting up the experiment.
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Mechanical Problems
The proposed research pertaining to the anticipated
mechanical problems would involve effort directed toward investigating
several areas of interest; these include changes in the experimental
115-scale generator, design and preparation of an experimental
combined connector and relief valve, control of the catalyst flow
rate, modification of the experimental full-scale generator, and ex-
ploration of the handling characteristics of the experimental full-
scale unit when operated on dry land. The proposed effort, as
currently contemplated, in each of these areas is outlined below.
Changes in the Experimental
Scale Generator
During the effort under Phase II, the experimental small-
scale generator developed some serious leaks. Under Phase III9 these
would be repaired so as to permit additional experiments, as described
above, to be conducted. Further, in order tc scale properly the out-
let of this unit to that of the experimental large generator, some
modification effort would be performed.
Also, there is a possibility that modification of the
catalyst-ring holes may be necessary. It is not expected that ex-
cessive internal pressures would be built up in the experimental
small generator during the course of the above-described experiments.
However, if this should happen, then it is anticipated that modifi-
cation of the catalyst ring would be investigated in an attempt to
slow down the rate of catalyst entry. The general procedure that
would be followed is outlined below under "Study of the Control of
the Catalyst Flow Rate".
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Consideration of the Experi-
mental Connector With Relief
Valve
During the previous full-scale experiment, the temporary
crude connector that was prepared in the field failed and prevented
proper filling of the balloon. Observations of the proceedings sug-
gested that a satisfactory connector should probably be rigid and
also capable of resisting the effects of moisture and of temperatures
of about 150 F. Discussions of the proposed connector with your
technical representative have resulted in a preliminary d3cision
to investigate the preparation of this item from a plastic type of
material. As currently envisioned, the proposed connector would be
fastened to the experimental-generator outlet and would provide a
horizontal opening to which the balloon feeder tube could be con-
nected.
After some consideration of the problem of relieving exces-
sive internal pressure in the experimental full-scale generator, it
appears worth while to investigate the possible usefulness of a lid
of predetermined weight as a relief valve. Thus, a vertical arm
might be incorporated in the proposed connector, and a properly
weighted lid might be placed at the top of the arm. Such an ex-
perimental connector, when attached, would look like a T placed side-
ways on the experimental generator; the balloon filler tube would be
attached to the bottom end of the vertical arm so as to provide for
passage of the gas under conditions of tolerable pressure.
The action of this type of relief valve represents one of
the oldest and simplest methods for relieving pressure. It is
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particularly suitable when the critical pressure is low. The primary
problem associated with this type of valve is the prevention of
sticking or cocking of the lid. However, it is believed that a
satisfactory experimental relief valve of this type could be pre-
pared for this application.
In addition to the proposed design effort which is generally
outlined above, it is anticipated that it would be necessary to in-
vestigate methods of preparing the experimental connector and relief
valve. At present, it appears practicable to consider a method in-
volving the preparation of a suitable form, coating of the form with
a suitable plastic, and curing the plastic in situ. If an investi-
gation of this technique does not provide satisfactory results, other
methods of preparation would be considered.
Study of the Control of the
Catalyst Flow Rate
The small-scale experiments described above are expected
to provide a basis for estimating an appropriate catalyst-entry period
of time for the experimental full-scale generator, so as to minimize
difficulties associated with the initial surge of hydrogen. After
this time interval is estimated, experiments would be conducted with
the proposed amount of fluid and different-sized holes, in an attempt
to establish a proper catalyst-solution flow rate. Most of these ex-
periments would be run in some kind of piping in which appropriate
holes were drilled. The amount of fluid flowing from the holes during
different time periods of operation would be measured. On the basis
of the results obtained, an estimate would be made of the appropriate
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size and number of holes needed in the catalyst-solution ring of the
experimental full-scale generator.
Modification of the Experi-
mental Full-Scale Generator
Subsequent to the above-outlined study of the catalyst-
solution flow rate, the experimental full-scale generator would be
modified to provide an appropriate size and number of holes in the
catalyst-solution ring. Currently, the only sizeable opening in the
experimental unit is the outlet. It is possible to manipulate the
experimental generator so that each hole in the catalyst-solution
ring would be accessible through the outlet opening; in this way, the
different holes could be covered or reduced in size systematically.
This procedure appears to be somewhat complicated; however, it is
believed that it would be much more practical than would that of
slitting the ring, adjusting the holes, and then repairing the slit.
Exploration of the Handling
Characteristics of the Experimental
Full-Scale Unit on Dry Land
Although the proposed full-scale experiment outlined above
would not constitute a demonstration of a one-man operation of the
experimental unit, it appears worth while, on the basis of previous
experience, to provide for investigating the handling characteristics
of the experimental generator in connection with dry-land operation.
The manufacturer has assured us that the experimental full-scale
generator can be placed on dry land and filled with the necessary
amount of water, without rupture occurring. This estimate has been
substantiated -,.t least in part by our operation of the experimental
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1/5-scale generator in this fashion, in connection with the previously
conducted effort under Task Order No. C. It is estimated that, under
these conditions, the forces acting on the experimental small unit
were as great as would be those on the experimental full-scale
generator; both have been prepared from the same materials and in the
same manner.
This proposed exploration would involve conducting probably
more than one run in the modified experimental full-scale unit on
dry land, without the borohydride and cobaltous chloride being used.
A cursory investigation would be made of a suitable method of filling
the experimental full-scale unit with an appropriate amount of water
(for the borohydride solution). No provision has been made herein
for effort directed toward modifying the experimental full-scale
generator in an attempt to alter its filling characteristics. It is
expected that, in the course of the proposed effort, some feel for
the difficulties involved, if any, would be obtained, and that a
resolution of such difficulties would be fairly straightforward.
Of particular importance in the proposed "dry" runs would
be the checking of the time interval required for the flow of an
appropriate amount of simulated catalyst solution through the catalyst
ring. If the rate of entry is not satisfactory, it would be neces-
sary to modify the holes in the ring accordingly. Some need for
modification of this sort is to be expected since the area of the
holes in the flexible ring material is difficult to estimate, and to
provide for.
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Another aspect which would be investigated would be the
problem of attaining the necessary amount of low-temperature water
during the time of the year when the ambient air temperatures might
be relatively warm. It is estimated that the full-scale experiment
would be run at a time when the ambient temperatures would be con-
siderably above 40 F. It is currently contemplated that the full-
scale run would be conducted at a borohydride-solution temperature
of 35 to 40 F. Consequently, it would be necessary to provide a
relatively large amount of low-temperature water.
At the present time, we believe that the water could be
cooled readily by using an auxiliary water tank and ice. A suitable
tank, costing approximately $150, would consist of a 12-foot-diameter
plastic liner supported by a wire fence. (The diameter of the ex-
perimental full-scale generator is 8 feet.) The proposed procedure
would involve filling the tank with ice water, and then placing the
experimental generator in the tank and filling it with ice water.
It appears that it would be readily possible to maintain the
experimental-generator water at low temperature while the necessary
associated equipment was being set up. When the experiment was to
be started, the water in the tank could be released, and the experi-
mental generator would be left standing in the dry tank. The support-
ing fence of the water tank could then be removed, and the generation
process could be carried on. If this method was found to be un-
satisfactory, others would be investigated.
On the basis of recent discussions, it is our understanding
that one balloon for use in the full-scale experiment and an additional
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120 pounds of sodium borohydride would be furnished by your technical
representative. We currently have on hand approximately 120 pounds
of borohydride. The above-indicated additional amount is based on
the requirements of the currently planned schedule of experiments;
this includes approximately fourteen 1/10-scale experiments (about
10 pounds per experiment) and one full-scale experiment (about
100 pounds per experiment). It is expected that your technical
representatives would be present during the full-scale experiment.
After the conclusion of the full-scale experiment, the ex-
perimental generator(s) would be provided to your technical
representative for further evaluation.
REPORTS AND LIAISON
Your technical representative would be kept informed of
the progress of the research program by informal monthly letter re-
ports. These reports would be supplemented by meetings with your
technical representative. At the conclusion of the proposed research
period, a summary report would be prepared that would include a
description of the experiments conducted and the results obtained.
Also, the operating procedure for the experimental full-
scale generator that was prepared under Supplement No. 4 to Task
Order No. C would be revised to reflect any appropriate changes re-
sulting from the effort proposed herein.
Declassified in Part - Sanitized Copy Approved for Release 2012/05/31 : CIA-RDP78-03642AO01300010057-4
 Declassified in Part - Sanitized Copy Approved for Release 2012/05/31 : CIA-RDP78-03642A001300010057-4
~ v -
DURATION AND ESTIMATED COSTS
It is proposed that the contract provide for an additional
eight-month period of research, with an estimated additional appropri-
ation of $15,317, including the additional fixed fee. A general
breakdown of the estimated appropriation increase is attached.
THE CONTRACT
The proposed contract would be a period-basis research
agreement, consistent with our current contractual arrangements and
providing only for a fixed period of research leading toward the ob-
jectives outlined above.
Declassified in Part - Sanitized Copy Approved for Release 2012/05/31 : CIA-RDP78-03642A001300010057-4
 Declassified in Part - Sanitized Copy Approved for Release 2012/05/31 : CIA-RDP78-03642AO01300010057-4
Declassified in Part - Sanitized Copy Approved for Release 2012/05/31 : CIA-RDP78-03642AO01300010057-4