='" OnC FILE H

MEMORANDUM REPORT BRL-MR-3800

BRL

U,) ANALYSIS OF LIQUID PROPELLANTwEXPOSED TO ELASTOMERIC MATERIALS

Wr

I JO EPHINE Q. WOJC[ECHOWSKI0 SHARON L. TAYLOR

WANDA J. O SZEWSKI DTICDECEMBER 1989 ELECTE

NOV 22 1989

APIPROVID FOR PUBLIC RELEASE; DISTRIBUTION UNLIMEP~-

U.S. ARMY LABORATORY COMMAND

BALLISTIC RESEARCH LABORATORYABERDEEN PROVING GROUND, MARYLAND

89 11 17 137

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The use of trade names or manufacturers' names in this report does not constitute indorsement ofany commerical product.

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BRL-MR-3800

6a. NAME OF PERFORMING ORGANIZATION 16b OFFICE SYMBOL 7a. NAME OF MONITORING ORGANIZATION(If applicable)

US Army Ballistic Rsch Lab jSLCBR-IB6c. ADDRESS (City, State, and ZIP Code) 7b. ADDRESS (City, State, and ZIP Code)

Aberdeen Proving Ground, MND 21005-5066

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ELEMENT NO. NO. NO. CCESSION NO.

11. TITLE (Include Security Classification)

ANALYSIS OF LIQUID PROPELLANT EXPOSED TO ELASTOMERIC MATERIALS

12. PERSONAL AUTHOR(S)Wojciechowski, Josephine Q., Taylor, Sharon L, & OLszewski, Wanda J.

13a. TYPE OF REPORT 13b. TIME COVERED 14. DATE OF REPORT (Year, Month, Day) 15. PAGE COUNT

MR TFROM Sep88 TOAr8916. SUPPLEMENTARY NOTATION

Addendum to Feuer, H.O. Jr. et al. "Elastomer Compatibility with Liquid Propellant". Technical Report2476, USA Bel-voir Rsch, Dev & Engr Ctr, Ft. Belvoir, VA, 22060-5060, Dec 88

17. COSATI CODES 18 S,UBJJ1 TERM (Contnu .o reve(se if necessary rad identify by block number)FIELD [ GROUP [ SUB-GROUP *-,..4qui ropeuant llyroxylammonmum Ir trateFIL GRU U-GOP[

HAN Triethanolammonium NitrateTEAN Compatibility Elastomer.

19. ABSTRACT (Continue on reverse if necessary and identify by block number)

The Army is investigating use of LP in large and medium caliber guns. The propellant of primary interest isLGP 1846 consisting of hydroxylammonium nitrate, triethanolammonium nitrate and water. One of theconcerns with fielding a liquid propellant system is compatibility with materials used for storage, transfer andhandling. The Belvoir Research Development and Engineering Center undertook an investigation on thecompatibility of elastomers with LGP 1846. The propellant was collected after exposure to the materialsand sent to the Ballistic Research Laboratory for analysis. It was analyzed for a change in fuel and oxidizercontent. This report is a compilation of the analysis.

20. DiSTRIBUTION/AVAILABILITY OF ABSTRACT 21 ABSTRACT SECURITY CLASSIFICATION

r UNCLASSIFIED/UNLIMITED M SAME AS RPT 0 DTIC USERS Unclassified22a. NAME OF RESPONSIBLE INDIVIDUAL 22b TELEPHONE (Include Area Code) 22c, OFFICE SYMBOL

Josephine Q. Woiciechowski (301) 278-6160 SLCBR-IB-B

DD Form 1473, JUN 86 Previous editions are obsolete SECUR!TY CLASSIFICATION OF THIS PAGE

Tx:?c:OXLLYLEE? ELA- Y.

TABLE OF CONTENTS

Pane

ACKNOWLEDGMENT . . . . . . . . . . . . . . . . . . . . . . . . . . v

BACKGROUND ............ ............................ a

DISCUSSION ............... ............................ 3

RESULTS ................ .............................. 4

CONCLUSIONS ............... ............................ 5

FUTURE WORK . . . . . . . . . . . . . . . . . . . . ........ .................... 13

R.E F E REN CES................................13

DISTRIBUTION .............. ............................ 15

A,,oss. on For

IPTIS GRA&IDTIC TA8LftI4wn o uZz) C a i 1-

histribet toni

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P1st lal

iii

-%ENOALLY LEFT BLAN.K.

Acknowledgement

We gratefully acknowledge Mr. Ronald A. Sasse for

development of the method for correctly determining the level of

strong acid impurity.

VI

INT:EN::CNALLY LEFT BLANK.

vi

Background

The US Army is currently investigating the use of liquid

propellants in medium and large caliber weapon systems. The

propellants that have been chosen for the current development

program are hydroxylammonium nitrate (HAN) based propellants, LGP

1845 and LGP 1846. These two propellants have the same ingre-

dients; HAN as the oxidizer, triethanolammonium nitrate (TEAN) as

the fuel and water as a diluent. The only difference between

1845 and 1846 is 1845 has 3 % more water.

In order to generate a practical system for storage and

handling of liquid propellants, it is necessary to know the de-

gree of compatibility with available materials which are likely

to be used for transfer and containment of the propellants cur-

rently under consideration. The measure of compatibility in-

cludes the effect of the propellant on the materials of contain-

ment such as swelling of elastomers, corrosion and chemical re-

actions. The storage compatibility of liquid propellants is also

determined by the degradation of the propellant by decomposition,

by the solution of ballistically undesirable ions, by solution of

materials that result in undesirable changes to the physical

properties of the propellant and/or subsequent pressure rise

within the storage container.1 -5

An elastomer and plastic compatibility program was initiated

by the US Army Ballistic Research Laboratory (BRL) in 1987. The

objective of this program was to measure the compatibility of

liquid propellant with various materials of construction by

measuring rates of decomposition and reaction under controlled

conditions. The approach taken was a three step program. The

initial step was exposure of the materials to the propellant.

Step two was analysis of materials for degradation or any

changes. Steps one and two were performed by the Materials,

1

Fuels and Lubricants Laboratory at US Army Belvoir Research,

Development and Engineering Center.1 Step three, determination

of chemical changes to the propellant itself, was then to be

performed at the BRL. This report is a compilation of the pro-

pellant anaylsis.

In developing the list of materials to examine, Ft. Belvoir

searched the literature for elastomeric materials compatible with

ammonium nitrates. Candidate materials were chosen from the

following groups:

o Butyl Rubbers

o Chloroprene Rubbers

o Polysulfonated Elastomers

o Nitrile Rubbers (including Carboxylated and Highly

Saturated)o Some Urethanes and Thermoplastic Elastomers

o Some Fluoroelastomers

Also analyzed were materials from the collapsible tank and hose

industries.

In examining the results of the material study, Ft. Belvoir

determined that nitrile, nitrile/polyvinylchloride blends, poly-

chloroprenes, fluoroelastomers, halogenated butyl, and ethylene-propylene elastomers performed satisfactorily. Carboxylated

nitriles, polyurethanes, and thermoplastic elastomers either

totally failed or showed sufLicient reduct-on in properties to

label them unacceptable for use with LP.

2

Discussion

The materials tested were conditioned in the propellant for

several different time periods: 7, 14, 28, 42 and 70 days at

70 +/- 40 F. Samples of propellant were collected at the end of

each immersion time. This collection of samples was submitted to

the BRL for analysis. The original propellant, LGP 1846 Lot No.

ABY86JG2001, was also analyzed prior to exposure to any material

for comparitive purposes.

The current assay analytical technicue for LP 1846 is

aqueous titration.6 Samples were titrated on a Brinkman In-

strument Model 672 Titroprocessor and Metrohm 665 Dossimat.

Aqueous sodium hydroxide (NaOH) base was used with an approximate

0.25 molarity. Sample sizes were approximately 0.30 grams.

Fifty mL of distilled water and 2 mL of acetone were added to

each sample. The acetone reacts with HAN to form an oxime and

nitric acid and is then titrated with base. Two end points are

obtained, one for nitric acid and the other for TEAN. At least

two replicates of each sample were analyzed and eight replicates

of the control sample were analyzed. The NaOH base was prepared

and standardized several times throughout the analysis.

Analysis of several samples showed little change from the

control and it was decided that the longest exposure times

available for each sample would be analyzed first. If no change

relative to the control was evident, intermediate exposure time

samples would not be analyzed. This reduced the workload

significantly while not affecting the results.

The strong acid impurity was also determined on the control

sample. Strong acid impurities could cause decomposition of the

LP over extended periods of time. The control had 0.lq wt%

excess strong acid, an acceptable level for this investigation.

3

Sasse developed a new spiked method for measuring excess

strong acid in LP nat replaces previous BRL methods in use. It

was suggested that 1 to 4 mL of 0.25 M HNO 3 be added to 20 mL of

LP diluted with 40 mL of water. Such a small acid addition al-

lows a typical "S" slope titration curve to be developed which is

necessary to determine an end point. The sample is titrated with

0.24 M strong base. The method is accurate to below 0.01 weight

% excess acid in LP.

Results

Results of the control analysis are shown in Table 1.

Values reported are individual analyses.

Table 1. Titrimetric Analysis of LP 1846 Lot No. ABY86JG2001

Wt% HAN Wt% TEAN HAN/TEAN

61.0002 20.6333 2.9564

61.0807 20.2917 3.0101

61.0429 20.7880 2.9365

61.1214 20.5543 2.9736

61.0911 20.3975 2.9950

61.0206 20.7433 2.9417

60.9387 20.8026 2.9294

61.1557 20.6610 2.9600

Average 61.06 20.61 2.96

Standard

Deviation 0.07 0.18 0.028

4

A list of the materials surveyed is provided in Table 2 with

appropriate designations. Analytical results for these designa-

tions are listed in Table 3. The result reported in Table 3 is

the average of two to four actual titrations for each sample.

The average and standard deviation of all 100 numbers in Table 3

is given.

Conclusions

Over 90 % of the values listed in Table 3 are within two

standard deviations for both weight % HAN and weight % TEAN.

Therefore, there is no statistical basis for claiming chemical

reactions of HAN and TEAN. This is not to say that the pro-

pellant was not affected as some of the samples showed evidence

of change by color and precipitation. Indepth analysis is

required on the LP samples of the best material sample

candidates.

Future Work

Examination of the most promising material candidates is

planned at temperature extremes. Indepth propellant analysis

will be made at that time to include gas products.

5

Table 2. Material Designators

A. Highly Saturated Nitrile Rubber

LP-l NBR-2

B. Nitrile Rubber

LP-2 N-BR-8LP-3 NBR-9LP-4 1203-F60-R2, RADIANLP-5 VT-380 (NBR/PVC), RADIANLP-6 BJLT MI-40, UNIROYALLP-7 OZO-HA-0221 (70% NBR/30% PVC), UNIROYAL

C. Carboxylated Nitrile Rubber

LP-8 XNBR-2LP-9 XN BR-3LP-10 XNBR-6

D. Polychioroprene Rubber

LP-11 CR-iLP-12 CR-2

E. Fluoroelastomers

LP-13 VITON-1LP-14 VITON-2LP-15 REEVES S/4646, (GUM)LP-16 FLURAN F-5500-A NORTON IND. PLASTICS

F. Ethylene-Propylene Rubber

LP-17 REEVES 4601 (GUM)

LP-18 REEVES 4594 (GUM)

Table 2. (cont) Material Designators

G. Thermoplastic Elastomers

LP-19 THP-1, ALCRYN R1201 B-70ALP-20 THP-3, ALCRYN R1101 B70LP-21 THP-4, MONSANTO GEOLASTLP-22 THP-5, MOBAY TEXIN 3550RLP-23 THP-6, MOBAY TEXIN 480 ARLP-24 THP-7, GAFLEXLP-25 THP-8, SANTOPRENE, 201-55LP-26 THP-9, SANTOPRENE, 101-64LP-27 THP-10, SANTOPRENE, 101-73LP-28 CD-9250, DISOGRINLP-29 NORPRENE, NORTON IND. PLASTICS

H. Polyurethanes

LP-30 PU-1, TSE INDUSTRIES, MILLATHANE HT-TIOLP-31 PU-2, TSE INDUSTRIES, MILLATHANE HT-R5LP-32 TSE-E-34-94, TSE INDUSTRIES, MILLATHANE

I. Synthetic Rubber

LP-33 3130 TREADLP-34 KRATON 1650, ILC DOVERLP-35 ATL-644-30, AERO TEC LABORATORIES, INC.LP-36 GOODYEAR COLLAPSIBLE TANKS GUM

J. Halogenated Butyl

LP-37 PE 100A027, ILC DOVER INC.

K. Miscellaneous

LP-38 SANTOPRENE aged 7 days at room temp.LP-39 REEVES S/4616 aged 7 days at room temp.

7

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12

References

1. H.O. Feuer, Jr., G. Rodriguez, and A.R. Teets, "ElastomerCompatibility with Liquid Propellant", Technical Report 2476, USABelvoir Research, Development and Engineering Center, FortBelvoir, VA, December 1988.

2. M.M. Decker, E. Freedman, N. Klein, C.S. Leveritt, and J.Q.Wojciechowski, USA Ballistic Research Laboratory, AberdeenProving Ground, MD, and 0. Briles and L. Joesten, SundstrandCorporation, "Compatibility Assessment of HAN-Based Liquid Pro-pellants", CPIA Pub. 470, pp 119-125, Proc. 1987 JANNAF Propel-lant Characterization Subcommittee Meeting, Laurel, MD, October1987.

3. K.A. Lavin, "Material Compatibility Testing Results", LetterReport from GE Company, Ballston Spa, NY, June 1987.

4. R. Hansen, E. Backof, and H.J. de Greiff, "Process forAssessing the Stability of HAN-Based Liquid Propellants", 1stInterim Report on Contract DAJA45-86-C-0056, Fraunhofer-InstitutFuer Trieb-und Explosivstoffe, Pfinztal-Berghausen, FRG, February1987.

5. O.M. Briles and L.S. Joesten, "Experimental Analysi- ofHydroxylammonium Nitrate (HAI) on Sample Materidis", Final Reporton Contract DAAD05-86-C-0168, Sundstrand Corporation, Rockford,IL, August 1987.

6. M.M. Decker, E. Freedman, N. Klein, C.S. Leveritt, and J.Q.Wojciechowski, "Titrimetric Analysis of HAN-Based LiquidPropellants", BRL-TR-2907, USA Ballistic Research Laboratory,Aberdeen Proving Ground, MD, March 1988.

13

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