SUMMARY REPORT ON TASK ORDER NO. C (PHASE III)

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP78-03642A000900040001-7
• Release Decision: RIPPUB
• Original Classification: S
• Document Page Count: 50
• Document Creation Date: December 23, 2016
• Document Release Date: September 11, 2013
• Sequence Number: 1
• Publication Date: August 31, 1959
• Content Type: REPORT

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c,"01,\IFIDENTIAL
(Phase I
Enclosed is th
n Task Order Bo. C
Oh describes the research perforsed under this
Task Order during the period January 1 through Auguet 31$ 1959.
The prototype full.,scale generator unit- with accessories,
and sieo the experimental 1/5..sea1e generator are available for
shipment. If you will provide an appropriate address ehall be.
glad to transmit then* units to you.
have Noyed working on this development and feel
_ultin prototype generator provides an effective unit
tba
for generatingthe required amount of hydrogen undor the specialised
service conditions. If you should be interested in diecuseing any
further refines nts in the design or any other aspects of thin unit
or possibly other special types of hydrogengeueratton equipment,
please do, not hesitate to call on us.
We would appreciate any comments wbI.ob you or your
*saciate might care to make with regard to the research.
Sincerely
AB $ 06
tri ate
50X1
50X1
DOC REV DATE lgeo to( t9417323....
CI.M COMP AA? CPI TYPE
L;LASS PAGES ? LUSE
dust NEXT REV /6 ACM RR 12.1
CONFID N
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t
CONFIDEN 11AL
St114/1ARY REPORT
ON
TASK ORDER NO. C
(PHASE 1)
August 31 1959
.1
?-0
S HEE CON1i11 IAL
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TABLE OF CONTENTS
Ela
INTRODUCTION
SUMMARY AND CONCLUSIONS 2
STATEMENT OF THE PROBLEM 3
MATERIALS, EQUIPMENT, AND PROCEDURES FOR HYDROGEN GENERATION 4
Materials List for Operation at 54 to 90 F With
Floating Generator 5
For Generation of Hydrogen 5
For Collection of Hydrogen. . * 6
Recommended Procedure for Operation at 54 to 90 F With
Floating Generator 7
Materials List for Operation at 32 to 54 F on Dry Land ? 12
For Generation of Hydrogen 12
For Collection of Hydrogen 13
Recommended Procedure for Operation at 32 to 54 F on
Dry Land 13
CHEMICAL ACTIVITY 18
Experimental Work 18
Results 19
Part 1: Low-Temperature Limit for Generation Under
"Standard" Conditions 19
Part 2: A Catalyst-Temperature Relationship for
Full-Scale Generation With 250 Gal of Water . . 22
Discussion 25
ENGINEERING ACTIVITY 30
Repair and Modification of the 1/5-Scale Generator . . 30
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TABLE OF 00T
NTS
cntinned
Preparation and Evaluation of Relief.olalve and
Balloon-
Connector Assembly
Design and Preparation
Evaluation. ? . ?
Study of Method of Adding Water to Generator
FUTURE WORK ? ? ? ? ? Ir ? ? ? ? ? ?? ? ? 4
APPENDIX 1. . . ? ? ** ? *** ? * ? ? * ?
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LIST OF TABLES
Lea
TABLE 1. AMOUNT OF CATALYST REQUIRED rolt HYDROGEN
GENERATION AT TEMPERATURES BETWEEN 54 AND 90 F. 4 4 10
TABLE 2. AMOUNT OF CATALYST REQUIRED FOR HYDROGEN
GENERATION AT TEMPERATURES BETWEEN 32 AND 54 F. 16
TABLE 3. RESULTS or HYDROGEN-GENERATION TESTS TO ESTABLISH
MINIMUM TEMPERATURE FOR OPERATION UNDER "STANDARD"
CONDITIONS. ? ?? ? * 6 ? ? ? ? ? ? ? . 20
TABLE 4. RESULTS OT SMALL4h$CALE EXPLORATORY GENERATION
TESTS . ? 4 ? ..23
TABLE 5. RESULTS OF HYDROGEN?GENERATION TESTS TO ESTABLISH
CONDITIONS FOR OPERATION AT LOW TEMPERATURES. s . 24
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LIST _OF PI_ tiRES
Page
FIGURE I. CATALYST REQUIREMENT FOR LARGESCALE GENERATION
OF HYDROGEN. ? 21
FIGURE 2. RELIEF*.VALVE AND BALLOON...CONNECTOR ASSEMBLY IN
POSITION ON GENERATOR. 0??.*. ***** 0 ? 34
FIGURE 3. FULL0SCALE HYDROGEN GENERATOR WITH RELIEFd.VALVE
AND BALLOON-CONNECTOR ASSEMBLY INSTALLED AND
WITH AN INTERNAL PRESSURE OF O. PSI. ? . . 0 * ? 35
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SUMMARY REPORT
ON
TASK ORDER NO. C
(PHASE III)
August 31, 1959
INTRODUCTIO
This report summarizes the research carried out under
Task Order NO. C$ during the period January 1 through August 31, 1959.
The over-all objective under Task Order No. C was to
design and develop a prototype generator which would be capable
of producing approximately 3,500 cu ft of hydrogen, at an isolated
site in a period of 60 min or less, and, at the same time, would
satisfy other specified operational requirements and conditions.
The "Summary Report on Task Order No. C (Phase II)" dated
December 31, 1958, which summarized the results of the Phase II
study, described the underlying research, design, and method of
operation of the prototype generator at temperatures between
50 and 90 F. It was concluded in the Phase II study that to
provide for the operation of the generator at temperatures between
approximately 50 and 32 If would require additional investigation.
Described herein are the results of the research carried out in
relation to the coldi.weather operation of the prototype generator.
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SUM$ART AND ONCLUSIONS
he entire research program performed under Task Order
So. 0 has established the requirements for generating 3,500 cu ft
of hydrogen in less than 60 min under field conditions where
natural water may vary in temperature between 32 and 90 F. For
temperatures between 54 and 90 r, a 560-gal pool of water con-
taining 100 lb of sodium borohydride is required* Five gallons
of catalyst solution consisting of 6 to 37 lb of cobaltous
chloride hexahydrate dissolved in water, is added the amount of
cobaltous chloride hexahydrate used depends on the initial pool
temperature and is selected from a prescribed chart listing the
weight of catalyst for various initial temperatures. For tempera-
tures of 32 to 54 F. the generation is carried out with a pool
containing 100 lb of sodium borohydride in 250 gal of water* The
catalyst requirement in this temperature range varies between
8.2 and 28 lb.
A full-scale test was performed with the prototype
generator resting on dry land and using water at a temperature of
36 r this was completed successfully in 15 min. The hydrogen
generated was collected in a balloon and had a measured lift of
223 lb (exclusive of the weight of the balloon and valving).
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STATEMENT 0 THE PROBLEM
The prototype generator developed and demonstrated in
the Phase II study used 560 gal of water and 100 lb of sodium
borohydride. The amount of cobaltous chloride hexahydrate catalyst
required to achieve a total generation time of about 40 min for
temperatures between about 50 and 90 F varied between 46 and 6 lb,
respectively.
On extrapolation of these data to near-freezing conditions,
it became apparent that excessively large quantities of catalyst
would be required. At 36 ro for example, 100 lb of catalyst would
be needed for generation in approximately 40 min. It was not
feasible to attempt to use such a large quantity of catalyst
because:
It exceeded the reported solubility of Co '6E20
in 5 gal of solution at 36 r
(2) It represented too much of a load for one man
to handle conveniently
(3) It was expected to consume a measurable quantity
of sodium borohydride and, in the process, would
release a large quantity of hydrogen too rapidly
at the start of the generation.
Therefore, in an attempt to provide for practical
generation under cold-weather operating conditions, it appeared
prudent to set 5 gal of saturated catalyst solution as a maximum
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amount of solution which could be used for fullecale generation.
This meant that, for example, at about 32 F, no more than 35 lb'
of cobaltoua chloride hexahydrate could be used.
The experimental program was subsequently directed
toward suitably generating hydrogen in a period of 60 mm or less
using no more than 35 lb of catalyst.
MATERIALS, EQUIPMENT, AND PROCEDURES
FOR HYDROGENOENERATION
Described below are the materials and equipment, and
the operating procedures for generating approximately 3,500 cu ft
of hydrogen in the Task Order No C generator under specified
conditions at an isolated site, at which there would be only a
pool of surface water sufficiently large to float the generator,
and at ambient temperatures ranging from about 32 to 90 F. Under
service conditions1 epending on the ambient temperature, the
operator would have to decide whether the generation would be
effected from a 560-gal or a 250-.gal system*
To facilitate a comparison of the two systems and as a
matter of general convenience, the materials, equipment, and
recommended operating procedures for both systems are described
below; those for the 560.- al system, for operation at temperatures
During the early stages of the Phase III study, the maximum
solubility of cobaltous chloride in 5 gal of saturated solution
at low temperatures was taken as 40 lb, based on data in the
literature. When it was subsequently realized that the appro-
priate value was approximately 35 lb, the experiments were
redesigned accordingly.
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ranging from 54 to 90 F* had been included previously in the
"Summary Report on Task Order No. C (Phase II)" dated December 31.
1958* and as presented below, reflect modifications based on the
research performed in the Phase III study. The procedure for the
560-gal system is described for application with the generator
floating on a pool of water, while that for the 250-gal system is
presented for the generator set up on dry land. However, with
only a few modifications of either procedure, the generator
could be operated as a 560-gal system on dry land, or as a 250-gal
system floating on a pool. The items of materials and equipment
are generally presented below in the sequence in which they would
be needed in order to carry out the generating procedure.
riateriale List for Operation at
4'OF With Fl?atin Generator
For Generation of Hydro en
1) Hydrogen generator
(2) Air pump* capacity about 70 cu.in. per stroke
(3) Fabric bag for weights, with drawstring, about
300-cu.-in. capacity
(4) Weights, 15 lb, as rocks or sand, probably available
at site
(5) Rope, 1/4 in., about 40-ft length
(6) Tools: knife, pliers, dipper, and funnel
(7) Adhesive tape
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.6.
(8) Solution container, 5-gal plastic wide-mouth
bottle with stopper
(9) Sodium hydroxide, 2 lb, in moisture-proof,
unbreakable, nonmetallic package
(10) Rubber gloves, shoulder length
(11) Sodium borohydride, 100 lb of crystals in five
moisture-proof, unbreakable, nonmetallic
packages
(12) Thermometer, all-metal dial type, 32 to 120 F
in 1 F increments
(13) Chart showing weight of catalyst required at
various initial temperatures of sodium borohydride
solution
(14) Cobaltous chloride hexahydrate catalyst, 46 lb
of crystals; in individual moisture-proof,
unbreakable, nonmetallic packages, 3 of 10 lb each,
2 of 5 lb each, 5 of 1 lb each, and 2 of 1/2 lb
each.
For Collection of Hxdrolien
(1) Balloon (including gas-inlet tube)
(2) Tarpaulin
(3) Sand bags
(4) Ropes
(5) Relief-valve and balloon-connector absembly.
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?commended Procedure to
Oeaerato
(1) Select a site for operation that provides a
water.-pool depth of about 4 ft near the bank,
(2) Unpaek the hydrogen generator close to the water
edge. Unfold the generator pack in a position to
favor easy inflation, with the air valve accessible.
(3) Attach the air pump to the air valve. Inflate
the air chamber (with about 700 strokes of the
pump) until the generator stands firmly on its
supporting stays.
(4) Detach the air pump and close the air valve.
(5) Select about 15 lb of rocks or sand at the site.
Place in the fabric weight bag and tie the mouth
of the bag. The proper weight of rocks may be
estimated by comparison with an equal weight of
packaged catalyst crystals.
(6) Tip the generator and tie the weight bag to the
center of the bottom with the straps provided.
(7) Attach a rope to the generator loop so that the
floating generator does not drift. Anchor the
other end of the rope on shore.
Slide the generator into the water, and push it
away from the bank until it floats freely.
(9) Push both of the water-inlet tubes into the genera
and lay them along the inside of the generator wall.
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.8.
(10) Tilt and resettle the generator in the water
several times to dislodge any air bubbles trapped
under the bottom of the generator. Make certain
that the weight bag is hanging free from the
bottom. Recheck the position of the water-inlet
tubes along the inside wall of the generator as
necessary during the filling period of about
55 min.
(U) While the water is running Lnto the generator,
spread the tarpaulin on the ground, unpack the
balloon, and lay it out on the tarpaulin; be
careful to avoid damage to the balloon fabric.
Prepare the balloon auxiliary equipment for use
during balloon inflation. Attach the T..shaped
reliefi.valve and balloon-connector assembly to
the balloon inlet tube by slipping the free end of
the inlet tube over the open end of the connector
assembly corresponding to the bottom of the T.
Wrap adhesive tape in and around the end of the
inlet tube so as to attach the inlet tube firmly
to the connector assembly with a joint which will
not leak gas.
(12) After the generator has filled to the proper
level, with the bottom fully extended by the
attached weight, pull out both of the water.inlet
tubes and knot each to shut off the water inlets.
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(13) Put on the rubber gloves.
(14) Open the 2-1b package of sodium hydroxide flakes
and pour them into about 1 gal of water in the
plaetic container. Shake briefly to dissolve,
and pour the solution slowly through the open
gas exit into the generator pool. Induce some
mixing by tipping the generator a few times.
Add the sodium borohydride crystals to the generator
pool by opening and emptying one package at a time
into the open gas exit.
(16) Check the pool for undissolved borohydride
crystals by dipping out a small sample from the
center bottom and inspecting. Stir with the dipper
or tilt the generator to speed up the mixing and
solution, if necessary.
(17) Measure the temperature of the solution by
inserting the thermometer into the generator
through the open gas exit.
(18) Determine the weight of the catalyst required
by referring to the chart (Table 1).
(19) Make up the catalyst solution in the 5-ga1 plastic
container. first, fill the container about one.
third full of water, add some of the catalyst,
and shake to dissolve. Add more water (corresponding
to about one third the volume of the 5-ga1 container)
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TABLE 1. AMOUNT OF CATALYST REQUIRED FOR
HYDROGEN GENERATION AT TEMPERA*.
TURES BETWEEN 54 AND 90 F
Weight of Sodium Borohydridel 100 lb
Weight of Sodium Hydroxide: 2 lb
Volume of Catalyst Solution: 5 gal
(made up on basis of values
given below)
Volume of Generator Solution: 560 gaI
Generation Time: Approximately 40 in
Initial Temperature
of Solution F
Weight of
Catal st lb
90
6
88
6.5
85
7.5
82
8.5
80
9.5
78
10.5
76
11.5
74
13
72
14.5
70
16
68
17.5
66
19.5
64
21.5
62
24
60
27
58
30
56
33.5
54
37
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and the remaining catalyst, and shake again. Fill
the container to the top with more water. Insert
the container stopper, and shake or roll the con-
tainer to mix the solutions Set the container
(with the solution) upright near the generator
at the water edge.
(20) Attach the balloon to the gas exit of the generator
by inserting the open end of the relief-valve and
balloon-connector assembly into the gas-exit tube, and
taping it in position with adhesive tape so that the
joint will be reliable and will not leak gas. Arrange
the balloon inlet tube so that the balloon will start
to fill without attention while the catalyst solution
is being added to generator.
(21) Support the full container of catalyst solution
upright on the top edge of the floating generator,
remove the stopper, and pull the open end of the
tilling funnel over the neck of the container and
down around the body of the container..
(22) Tip the container and pour the catalyst solution
through the funnel into the catalyst reeervoir
on the top of the generator.
( ) Kydrogen generation will start as soon as the
catalyst solution starts to run into the gene
pool from the reservoir. quickly tie off the
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flexible spout of the tilling funnel to prevent
any loss of hydrogen.
(24) Attend the balloon during the filling operation.
No further control of hydrogen generation is
needed.
Matera1s List fcr.gperation.at
54 F_on Dry_ Land
For Generation of Hydrogen
1) Hydrogen generator
(2) Air pump, capacity about 70 Cu, in. per stroke
(3) Tools: Knife, pliers, dipper, funnel, and 2-gal
(nominal) plastic or rubber bucket
(4) Adhesive tape
(5) Solution container, 5..1;al plastic wide-mouth
bottle with stopper
(6) Sodium hydroxide, 0,9 lb, in moisture-proof, unbreakable,
nonmetallic package
(7) Rubber gloves, shoulder length
(8) Sodium borohydride, 100 lb of crystals in five
20-lb moisture-proof, unbreakable, nonmetallic
packages
(9) Thermometer, all-metal dial type, 32 to 120 F in
I F ineremen s
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(10) Chart showing weight of catalyst required at
various initial temperatures of sodium borohydride
solution
(11) Cobaltous chloride hexahydrate catalyst, 28 lb of
crystals; in individual moisture-proof, unbreakable,
nonmetallic packages, 1 of 10 lb, 2 of 5 lb each,
7 of 1 lb each, and 5 of 0.2 lb each.
Per Collection of Hydrogen
(1) Balloon (including gas-inlet tube)
(2) Tarpaulin
(3) Sand bags
(4) Ropes
(5) Relief-valve and balloon-connector assembly.
Recommended Procedure for Operation
at 32 0 54 Y on Dry Laud
(1) Select 4 site for operation that provides a relatively
flat area, about 9 to 11 ft in diameter, as close as
possible to the source of water.
(2) Unpack the hydrogen generator on the flat area
as close as possible to the source of water.
Unfold the generator pack in a position to favor
easy inflation, with the air valve accessible.
(3) Attach the air pump to the air valve. Inflate the
air chamber (with about 700 strokes of the pump)
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1 the generator stande firmly on its supporting
stays.
(4) Detach the air pump and close the air valve.
(5) Knot each of the wat r inlet tubes at the bottom
of the generator so as to close them oft
(6) Using the 2-gal (nominal) bucket, pour 250 gal of
water into the generator through the open gas-exit
tube. This involves adding 125 bucketfuls of water.
(In the generator, 250 gal of water represents
pool with a depth of 8.2 in. If necessary, the
operator can coarsely check the depth of the water
in the generator by using a "dip atick" method, that
is, by inserting a tree branch or its equivalent, in
the vertical position through the generator gas exit
and estimating the length of the branch wetted by
the water. It there is any doubt in the operator's
mind as to whether be has added enough water, it would
be safest if be poured in more.) The filling operation
can be done in about 15 to 20 min.
(7) Spread the tarpaulin on the ground, unpack the
balloon, and lay it out on the tarpaulin; be care.
ful to avoid damage to the balloon fabric. Prepare
the balloon auxiliary equipment for use during balloon
inflation. Attach the Toahaped relief-valve and
balloon-connector aseembly to the balloon inlet tube
by slipping the free end of the inlet tube over the
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open end of the connector aesembly corresponding
to the bottom end of the Ti Wrap adhesive tape in
and around the end of the inlet tube so as to
attach the inlet tube firmly to the connector-
assembly with a joint which will not leak gas.
(8) Put on the rubber gloves.
(9) Open the 0.9.-1b package of sodium hydroxide flakes
and pour them into about I gal of water in the
5-gal plastic container. Shake briefly to dissolve,
and pour the solution slowly through the open
gas exit into the generator pool. Induce some
mixing by tipping the generator a few times.
(10) Add the sodium borohydride crystals to the generator
pool by opening and emptying one package at a time
into the open gas exit.
(11) Check the pool for undissolved crystals by dipping
out a small sample from the center bottom and
inspecting. Stir with the dipper or tilt the
generator to speed up the mixing and solution,if
necessary.
(12) Measure the temperature of the solution by inserting
the thermometer into the generator through the
open gas exit*
(13) Determine the weight of the catalyst required by
referring to the chart (Table 2).
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TABLE 2. AMOUNT OF CATALYST REQUIRED FOR
RYDROGEN GENERATION AT TEMPERA..
TURES BETWEEN 32 AND 54 r
Weight of Sodium Borohydride: 100 lb
Weight of Sodium Hydroxide: 0.9 lb
Volume of Catalyst Solution: 5 gal
(made up on basis of values
given below)
Volume of Generator Solution: 250 gal
Generation Time: Approximately 20 min
Initial Temperature
of Solution, F
Weight o
Catalyst lb
54
52
50
8.2
9.2
10.2
48
11.6
12.8
44
14.0
42
16.0
40
17.6
38
20.0
36
22.4
34
24.8
32
28.0
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(14) Make up the catalyst solution in the 5-gal plastic
container. First fill the container about one.
third full of water, add some of the catalyst, and
shake to dissolve. Add more water corresponding
to about one third the volume of the 5-gal container)
and the remaining catalyst, and shake again. Fill
the Container to the top with more water. Insert
the container stopper, and shake or roll the 4011w*
tamer to mix the solution. Set the container (with
the solution) upright near the generator.
(15) Attach the balloon to the gas exit of the generator
by inserting the open end of the relief-valve and
balloon-connector assembly into the gas exit
tube, and taping it in position with adhesive
tape so that the joint will be reliable and will
not leak gas. Arrange the balloon inlet tube
B0 that the balloon will start to fill without
attention while the catalyst solution is being
added to generator,
(16) Support the full container of catalyst solution
upright on the top edge of the generator,
remove the stopper, and pull the open end of the
filling funnel over the neck of the container and
down around the body of the container,
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?
-18-
(1?) Tip the container and pour the catalyst solution
through the funnel into the catalyst reservoir on
the top of the generator.
(18) Hydrogen generation will start as soon as the
catalyst solution starts to run into the generator
pool from the reservoir. quickly tie off the
flexible spout of the tilling funnel to prevent
any loss of hydrogen'
(19) Attend the balloon during the filling operation.
No further control of hydrogen generation is
needed.
pitEmIcAL A TIVITT
Experiment..l Wel*
Studies were carried out in the 1/5- and full-scale
generators designed and prepared under the Phase II program. Al
of the generation experiments were performed on dry land; this
was in contrast to portions of the Phase II program in which the
full cale and some of the other tests had been run with the
generators floating on a body of water. Complete descriptions
of the two generators and methods of operation were presented in
the "Summary Report on Task Order No. C (Phase II)" dated
December 31 1958.
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OLURL I
?
Reaults.
In order to attain the goals of the Phase III study,
the experimental program was divided into two parte. The first
part was concerned with determining the lowest temperature at
which genoraton could be completed in 60 min (maximum) using
5 gal of saturated catalyst solution (approximately 35 lb of
catalyst). The second part involved establishing a new cata1yst-0
temperature relationship for a more concentrated sodium borohydride
solution, for use in generation between the lowest temperature
as determined in the above-mentioned Part 1 of the program, and
32 F.
for en r tion Under"Stand
Runs 3, 8, 9, 10, 11, and 12, listed in Table 3, are
1/10-scale tests from which the low-temperature limit of operation
under "standard" conditions (100 lb of sodium borohydride in 560 gal
? of water) was obtained. Figure I presents a plot of so e of these
data; it indicates that, under "standard" conditions, the proto-
type generator can be used to produce hydrogen in 60 min or less
? at a minimum temperature of approximately 53 F when a maximum of
35 lb of catalyst is involved. It is to be noted, in Figure 1,
that the catalyst-temperature line based on the Phase II study
intersects the extrapolated line for the data of Runs 10, 11, and
12 and the 3504b catalyst line at approximately 53 F
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TABLE 3* RESULTS or HYDROGEN*.GENERATION
TESTS TO ESTABLISH MINIMUM
TENPERATURE FOR OPERATION UNDER
"STANDARD" CONDITIONS
Run
Hos_
Reaction Solution
_
Temperature,
V
Total
Generation
Timet_min
AmSt,
lb_
Vol of
Solution'
gal
Scale
HaBH4,
10
Water,
gal_
Depth,
in.
Initial
Rise_
3
1/10
10.'0
56
9
39
57
4.0
1.0
51
8
1/10
10.0
56
9
33
58
4.0
1.0
74
9
1/10
10,0
56
9
34
58
4.0
1.0
84
10
1/10
10.0
56
9
37
60
3.0
0.5
112
11
1/10
10.0
56
9
42
59
3.2
0.5
91
12
1/10
10.0
56
9
46
59
3.3
0.5
77
* Under full?scale conditions, 560 gal of water and 100 lb of sodium
borohydride.
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aiNVilliku I
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0
,
50
40
30
20
10
9
8
7
6
5
4
3
Temperature, F
85.6 77.4 69.4 62.1 54.7 47.3
40.6
34.0
Phase
..
It Study
-0, -32-_ii
1
io /
-o..,
560 gal;
Total generation
time approximately
40 min.
/-
/
/
/
/
/
/
Phase
r
III .Study
250 gal;
Total generation
time approximately
20 min.
?
?
'V
/
Phase DI Study
Total generation
time 10-15
min.
3.20
3.30
3 40
360
370
FIGURE I. CATALYST REQUIREMENT FOR LARGE-SCALE GENERATION
OF HYDROGEN
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SLUKL I
0220
Runs 1, 2, 4, 6, and 7, shown in Table 4, were small,
bench..scale experiments which were performed in a 10-1/2.-in.-diameter
glass reactor. These smallscale tests were run to explore the
effect of catalyst distribution, depth of reactor pool, and mixing
characteristics on total generation time; and involved the same
relative borohydride concentration as the previously mentioned
1/10-scale tests.
Part g: A Catalyst.-Temperature
Relationship for Full-Scale
Generation With 250 gal of Water
After approximately 53 F was determined as the low-
temperature limit for suitable generation using 560 gal of water,
it was then necessary to establish the proper conditions for
generating hydrogen at temperatures between 53 and 32 F. Informa-
tion obtained in the Phase I study had indicated that this would
be achieved most readily by increasing the concentration of sodium
borohydride. This change would result in less water being used
in preparing the generator solution; consequently, the temperature
rise and the average temperature in the system would be greater,
and the rate of generation could be increased without using more
than 35 lb of catalyst.
Runs 14 through 17, listed in Table 5, were the 1 0-
and 1/5-scale experiments from which a catalyst-temperature
relationship was obtained for full-scale generation using 250 gal
of water. Run 13 was a 1/10 scale test based on a 400-gallon
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TABLE 4. RESULTS OF SHALL.-SCALE EXPLORATORY GENERATION TESTS
Run
no.
Reaction Solution
Temperature,
Catalyst
Total
Generation
Time, min
Remarks
g
Vol of;
Solution,
cc
Addition
Site
Na3R4,
lb*
Water,
liter*
Depth,
in.
Initial
Rise
1
0.12
2.5
1-3/4
64
34
2.97
50
Pool center
42
2
0.12
2.5
1.3/4
66
36
2.97
50
Over entire
50
14--
pool surface
4
0.35
7.5
5-1/2
68
50
8.92
150
Pool center
42
li---,,---il
5
0.35
7.5
5.1/2
64
48
8.92
150
Over entire
51
'=3
pool surface
6
0.35
7.5
5-1/2
70
50
8.92
150
Pool center
40
4510
7
0.35
7.5
5-1/2
71
51
8.92
150
Over entire
pool surface
25
Solution stirred
for 30 sec after
catalyst addition
Note: These tests were conducted in a 10-1/2-in.-diameter glass reactor.
The relative borohydride concentration was the same as that for the 1/10-scale tests listed in
Table 3.
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5tfaitt 1
,
TABLE 5* RESULTS OF HYDROGEN-GENERATION TESTS TO ESTABLISH
CONDITIONS FOR OPERATION AT LOW TEMPERATURES
Run
No.
Reaction Solution
Temperature,
r
Catalyst,
Total
Generation
Time, min
Masts
lb
Vol of
Solution,
gal
cal('
Na8H4,
lb
Water,
gal
Depth,
in.
Initial
Rise
13
1/10
10.0
40
6.4
35
79
3.1
0.5
86
14
1/10
10.0
25
4.1
33
114
3.1
0.5
10
15
1/5
20.0
50
8.2
34
112
6.3
1.0
32
16
1/5
20.0
50
8.2
50
104
2.5
1.0
15
I?
1/5
20.0
50
842
43
113
4.0
1.0
12
18
Fu11?
100.0
250
8.2
36
121
23.0
5.0
15
14A
Small
0.6
1.5
4.0
33
98
0.19
15
14B
Small
1.2
3.0
8.0
31
102
0.37
21+
16A
Small
1.2
3.0
8.0
51
91
0.15
ein?
30
' 1* The measured lift was 223 lb (exclusive of the weight of the balloon
and valving).
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full-scale generation; Run 18 represented the full*sc le teat
which was performed to cheek the new catalyst.stemperature
relationship.
Runs 14A and 14D, and 16A were explo atory, bench-scale
experiments conducted at the same relative borohydride and catalyst
Concentrations as those in Runs 14 and 16, respectively. These
runs are discussed below.
Discussion
In the course of carrying out this program, there were
two "surge" problems which were of concern. It was possible that
the initial reaction between cobaltous chloride and sodium borod.
hydride would evolve a large, perhaps unmanageable, amount of
hydrogen when large amounts of catalyst were used. It was also
thought that an increase in the concentration of borohydride for
low-temperature oper tion would introduce a large over-all temperature
rise in the system and that this would cause an extremely rapid
increase in the generation rate during the last 30 to 40 per cent
of the reaction. The results showed, however, that, although
both of these effects occurred, the surges were not unmanageable
and were handled very easily and smoothly in a full-scale genera-
tion, as described later.
Data in the chemical literature on the solubility of
cobaltous chloride indicated that a maximum of 40 lb of catalyst
could be contained in 5 gal of catalyst solution at these low
SECREI
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Stlatts 1
?
temperatures. As a result some of the initial experiments of
the Phase III study were based on the 40.4b full-scale value.
When it was realized that this value was erroneous, all additional
experiments were designed around a maximum solubility of 35 lb
of catalyst. Runs 3, 8, and 9 (Table 3), which were designed
around the 40-1b maximum solubility, showed that with 40 lb of
catalyst (i.e., if the catalyst solution were warmed or the amount
of solution was increased to 6 gal), the 560-gal unit could be
used down to approximately 40 F for generation times of 60 min
or less.
The variation in total generation times for Runs 10, 13
and 14 (in Tables 3 and 5), corresponding to 112 in in a 560-ga1
pool, 86 min in a 400-gal pool, and 10 min in a 250-gal pool with
the same quantity of catalyst and borohydride suggests that a
specific change occurred in the reaction mechanism as the amount
of water was decreased. It was thought that the change it the
solution depth might be influencing the initial mixing and
distribution of the catalyst. The depths of the pool in these
runs were 9, 6.4, and 4,1 in. respectively (corresponding to
depths of 18 12.8, and 8.2 in., respectively, in the full-scale
generator). Runs 14A and 14B (Table 5) were performed to check
the effect of pool depth on the total generation time; as the
results show, doubling the depth of the solution did increase the
total generation time, but by less than a factor of two. Apparently,
below a certain depth mixing becomes more efficient and the
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reaction is little affected by the time required to distribute
the catalyst laterally from the point(s) of addition. Calculate
total generation times based on the rate equation developed in
the Phase I program, namely;
d(NaB114) = 1.45
dt x 1013 (CoC1
hn
rwg4 )0.39m.0,1?500/RT
""^4?
agreed very well with the experimental total generation times in
instances where the borohydride concentration was that of the
250.gal system. As a result of this depth effect, Runs 15 16,
and 17 were carried out as 1/5.-sca1e tests (in which the depth
of solution is the same as that in full-scale tests).
These results indicated that, in the course of scaling
to larger or smaller units, the pool..depth parameter is more
important than the pooli.diameter parameter. This conclusion was
borne out rather strikingly. In changing from a 10.5-hini.diameter
reactor to the prototype full..scale generator (8?ft diameter)g
the pool volume at constant depth was increased by a factor of
about 84, yet the total generation times were all in good agree-
ment with the calculated values. On the other hand, changing
the depth of the pool from 4.1 in. to 9 in. in Runs 14 and 10
(corresponding to a change of 8.2 in. to 18 in. on a full-scale
basis) increased the experimental total generation time markedly.
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?
SEC ET
?280.
The ability of the insoluble cobalt boride* to spread
out rapidly across the top of the pool was observed directly in
bench-scale experiments. While the catalyst dispersed laterally
very rapidly, approximately 1 min elapsed before the solution was
uniformly black from top to bottom in the bench-scale experiments,
and over 3 min, before the bubbling (gas evolution) appeared to
be occurring homogeneously throughout the entire solution.
Although it can be readily understood that catalyst
?distribution should be less rate-controlling in a shallow pool,
it was not clear why the effect, as noted in Runs 10, 134 and 14,
was so pronounced. However, it was not deemed sufficiently
important to the Task Order No, C program to investigate this
effect further.
On the basis of Runs 14 through 17 (Table 5), a
catalyst-temperature plot was prepared for the 250-gal unit,
This plot, the dotted line in Figure 11 was related to cold-weather
generation with a total generation time of approximately 10 to
15 min. It was then thought that this total generation time might
possibly be too rapid. Calculations were subsequently made to
determine the effect of decreasing the amount of catalyst used
by 20 per cent. The results of these calculations were as follows*
This is the active catalyst compound which is formed as soon as
the catalyst solution is added to the borohydride solution, as
described in the "Summary Report on Task Order No. 0 (Phase II)"
dated December 311 1958.
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os29*
System: 100 lb of NaBli 4
250 gal of water
33 F initial temperature
Amount of Total Generation
S:q9.21.ELLat Time.,mi
31 16
25
20
Thus, the calculations indicated that a 20 per cent decrease in
catalyst concentration would slow down the reaction, but not too
drastically. On the basis of these calculations, the catalyst-
temperature relation, shown as the solid line on the right side
of Figure 1$ was obtained.
The results of the full-scale test showed that the
catalyst-temperature relatio ship for the 250-gal unit resulted
in a smooth generation of 3,500 cu ft of hydrogen in approximately
15 min. The initial surge was quite evident as soon as all of the
catalyst solution was added; but, at no time did it appear even
close to "getting out of hand". The "tail end" surge was also
evident, but to an even lesser extent than the initial surge.
The full-scale test also showed that, under service conditions,
the operator would have no problem in determining when the
generation reaction is complete. The end of the generation is
apparent from the cessation of both the sound of the reaction
within the unit and of the motion of the balloon gas-inlet
tube.
SURE'
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-30?
As a result of the studies carried out under the Phases
11$ and III programs, it is evident that hydrogen generators can
be designed and constructed to produce hydrogen under a wide
variety of conditions. The chemistry of the sodium borohydride
hydrolysis is now sufficiently well understood; consequently,
only a relatively small amount of calculation and experimentation
should be necessary for the development of other hydrogen generators.
ENOTNNWNG ACTIVITY,.
The engineering activity under the Phase III program
dealt with the mechanical aspects of the hydrogen generator, and
included the repair and modification of the 1/5.-scale generator,
and the design, preparation, and evaluation of a relief-valve and
balloon-connector assembly for the full-scale unit.
Repair and ,lodifics.tion of the l/5Scaie,0enerator
In preparation for the 1/10- and -scale hydrogen-
generation tests in the 1/5-scale generator, the unit was nspocted
and repaired to eliminate gas and water leaks. Also, since
several wooden stays which supported the wall of the generator
were warped badly or broken, new stays were installed.
To provide for the study of the hydrogen...generation
surge problem in the 1/5-scale generator, the gas-exit tube was
scaled accurately to that of the full-size unit; as a result of
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T)Ltilit
?
31
the corresponding decrease in the diameter of the exit tube, the
rate of gas flow from the small generator would be reduced and
the internal pressure produced by the hydrogen generated by the
reaction would be similar to that in the full..scale unit. The
modification was made by installing an adapter prepared from two
sizes of brass tubing. Fittings were provided on the scaled
adapter to permit attaching thermocouple leads and a connection
to a manometer. In subsequent generation tests, surge in the
1/5-scale generator was noticeable, but, as confirmed by internal..
pressure measurements, the generator was at no time in danger of
rupture in these tests.
Preparation and Evaluation of Relief-Valve
and Balloon-Connector Assembly
Design and Preparation
In view of the experience gained in the previous full-
scale experiment, it appeared that there might be a need for a
relief valve which would be located in the system at a place
between the generator and the balloon; and also for a connector
of some type, to provide for the flow of the generated hydrogen
from the generator to the balloon gas-inlet tube (and subsequently
into the balloon).
Nonmetallic, low-pressure, large-volume-flow relief
valves were not commercially available, so several designs of
relief valves were evolved and evaluated. Since it was necessary
HUEY
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StiGHL I
a
4.32
also to provide a connector between the generator exit tube and
the balloon inlet tube, an effort was made to design the relief
valve as a part of the connector*
The full-scale generator had been designed to withstand
an internal pressure of approximately 0.5 psi; consequently, the
relief valve was designed to operate at approximately 0.45 psi.
An experimental relief-valve assembly was fabricated with a brass-
tube housing, a brass ring valve seat, and a brass free-floating
weighted-lid valve. To check out this experimental assembly, air
under a 70-psi air-line pressure was let into a closed system
incorporating this unit. The valve opened at a pressure of
approximately 0.45 psi and, in general, operated satisfactorily.
However, the size of the weight needed (on the lid of the valve)
and the necessity of maintaining the valve in a near-vertical
position on the fairly flexible generator led to distinct problems.
In an effort to reduce the size of the weight on the
valve and to improve its reliability, the weight in the experimen a
valve (lid) was replaced by a spring; also, a free-floating
lightweight lid was incorporated in the spring-loaded relief
valve. The operation of this valve in the test housing was quite
satisfactory. The valve was operable and reliable regardless
of the mounting position.
The compactness of this experimental valve made it
possible to incorporate the valve assembly into the design of the
balloon connector. The balloon connector was a T-shaped rigid
plastic unit made from short lengths of 5-tn.,-diameter Plexiglas
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SEMI
tubing. One open end was to be inserted in the full-scale..gene atm*
gas-exit tube, and the balloon inlet tube was to be attached to
the second open end; the relief valve was located in the third
open end of the T-shaped unit. The relief-valve and balloon..
connector assembly, in position in the generator, is shown in
Figure 2. Drawings of the assembly are included in Appendix 1.
Evaluation
The relief-valve and balloon-connector assembly was
installed in the full-scale generator, approximately 560 gal of
water were added, the balloon connector opening of the assembly
was closed and sealed, and the unit was pressurized internally at
approximately 0.45 psi. The relief valve opened and fluttered
to allow air to escape, and the internal pressure of 0.45 psi was
maintained. The amplitude of movement of the valve as the air
escaped was a function of the volume of air flowing through the
valve. The full-scale generator ballooned considerably at an
internal pressure of 0.45 psi as shown in Figure 3; however,
the unit, containing 560 gal of water, was found to be quite
stable while resting on dry land.
It was estimated that, during the hydrogen.generation
reaction in the full-scale unit, the hydrogen might at times be
evolved at a rate as fast as about 1,500 cu ft per min. Calcula?
tions indicated that with a 6-in.-diameter balloon inlet tube,
50 ft long, and with a 0.5..poi pressure drop in the tube, the
flow capacity of the system incorporating the relief valve
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alnifiL El
nu RE 4. RELIEY04ALVE AND BALLOONE.
IN POSITION ON GENERATOR
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0
TOR ASSEMBI?T
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.350
FIGURE 3, FULL.SCALE RIDROGEN GENERA= WITN RELIEF*VALVE
AND BALLOON.,CONNECTOR ASSEMSLT INSTALLED AND
WITH AN INTERNAL PRESSURE OF 04?45 PSI
SBRE
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-36-
could accommodate, theoretically, the flow of hydrogen at a
rate of 41000 Cu ft per min.
In preparation for this evaluation, the relief-valve
and balloon-connector assembly had been inserted into the generator
exit tube and initially sealed in place with plastic electrical
tape. However, at low temperatures, this tape becomes brittle
and its usefulness is impaired. As a result, adhesive tape was
used for this purpose in the full-scale test and was found to
be quite satisfactory.
In regard to the problem of attaching and sealing the
relief-valve and balloon-connector assembly to the generator
exit tube and also to the balloon inlet tube, the use of metal
clamp bands was considered to be objectionable because these
would permit the operator to readily apply enough pressure so as
to break the plastic connector. Also, the use of metal in the
generator kit was to be kept to a minimum, in order to decrease
radar detectability. It was felt that plastic clamp bands lacked
the necessary strength and reliability, especially for use in the
connection to the generator exit tube where the material consisted
of several thicknesses and was difficult to seal. 0-rings used
as clamps were inadequate. The combination of a wide natural-
rubber band plus an 0-ring clamp was found to be relatively
effective. A webbed-fabric draw-up band used with the rubber
band was considered to be a more desirable combination. The
rubber band would make the seal; the webbed-fabric band would
? ?? provide for holding the connector in place so as to prevent it
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from being being dislodged from the generator, and also for maintaining
the connection between the balloon inlet tube and the plastic
connector. However, the elastic bands probably would deteriorate
in storage.
Therefore, it appears that adhesive tape should be
provided in the kit because taping the joints with this material
provides a reliable seal and method of attachment. Also, adhesive
tape is satisfactory when using the generator in cold weather, at
which temperatures other types of tape become brittle and ineffective.
Stud of Method of Add' Water to Generator
During consideration of the various problems of filling
the generator with water, it became evident that, at times, it
might be necessary to put the water in manually. Thus, if the
generator were sitting in water which was too shallow or on dry
land, a device such as a bucket would have to be used to obtain
the desired volume of water in the generator.
With these needs in mind, a cursory experiment was run
to determine how much water could be bucketed by one man in a
continuous effort and how fatigued he might become under these
conditions. A 2-gal (nominal) bucket was used and the experimenter
stood in water which came to a level just above his knees. The
bucket was of light plastic material and had a hand grip on the
bottom; this grip proved to be very helpful. By bucketing water
from one side of a narrow surface, which was about 18 in. above
SECRET
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Declassified in Part- Sanitized Copy Approved forRelease2013/09/11 : CIA-RDP78-03642A000900040001-7
StlAti
the water, to the other side, the experimenter simulated tilling
the generator manually*
Under these conditions, it was possible to bucket
600 gal of water in just over 1, mini The experimenter was a
person who is an average type of office worker (sedentary worker);
while he was tired at the conclusion of the experiment, the effort
did not cause significant discomfort.
ruTURE WORK
The use of the prototype generator on land and in water
has been demonstrated, and the present design of generator has
proven to be quite satisfactory. However, as suggested by your
technical representative, the full-scale generator might be
improved by eliminating the metal wall supports or stays, in
order to decrease further the over-all weight and the radar
detectability. Also, when the unit is used in water, the weight
its supported by the fabric bottom, which assumes a cone shape and
thus pulls in the peripheral wall. If the wall was prepared
entirely from the air-mat section, the metal stays could be
eliminated, and the unit would assume a more satisfactory shape
in the water because it would float on the surface and the wall
would be fully supported. Also, following field evaluation of the
full-scale generator, there would probably be other design changes
to be considered.
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attAt I
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? In addition, a water-filling device of some type would
be helpful in decreasing the time and/or effort involved in
filling the unit with either 250 or 560 gal of water. This device
should be capable of appropriately filling the generator either
on dry land or in the water.
This study (Phases I I, and III) has enabled us to
develop an understanding of more of the chemistry of the hydrolysis
of sodium borohydride than had been previously known. If it
should become necessary or advantageous to generate 3,500 Cu ft
or even larger quantities of hydrogen from a physically smaller
unit, this could now be achieved with a minimum of development
effort.
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APPENDIX, 1
DRAWINGS OF RELIEF-VALVE ARD
BALLOON.000NNECTOR ASSEMBLT
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