ASTM F359-82(1994)e1
(Practice)Standard Practice for Static Immersion Testing of Unstressed Materials in Nitrogen Tetroxide (N 2) (Withdrawn 2003)
Standard Practice for Static Immersion Testing of Unstressed Materials in Nitrogen Tetroxide (N 2) (Withdrawn 2003)
SCOPE
1.1 This practice covers the evaluation of the compatibility of nitrogen tetroxide (N 2 O 4 ) rocket engine propellant with materials which will be used in aerospace systems. The practice includes immersion procedures in the vapor phase, liquid phase, critical vapor, and vapor-liquid interface for metals, elastomers, plastics, lubricants, and other materials as applicable.
1.2 This standard should be used to measure and describe the properties of materials, products, or assemblies in response to heat and flame under controlled laboratory conditions and should not be used to describe or appraise the fire hazard or fire risk of materials, products, or assemblies under actual fire conditions. However, results of this test may be used as elements of a fire risk assessment which takes into account all of the factors which are pertinent to an assessment of the fire hazard of a particular end use.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: F 359 – 82 (Reapproved 1994)
Standard Practice for
Static Immersion Testing of Unstressed Materials in
Nitrogen Tetroxide (N O )
2 4
This standard is issued under the fixed designation F 359; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Section15 was added editorially in September 1994.
1. Scope D 638 Test Method for Tensile Properties of Plastics
D 790 Test Methods for Flexural Properties of Unreinforced
1.1 This practice covers the evaluation of the compatibility
and Reinforced Plastics and Electrical Insulating Materi-
of nitrogen tetroxide (N O ) rocket engine propellant with
2 4
als
materials which will be used in aerospace systems. The
D 883 Terminology Relating to Plastics
practice includes immersion procedures in the vapor phase,
D 1414 Test Methods for Rubber O-Rings
liquid phase, critical vapor, and vapor-liquid interface for
D 1460 Test Method for Rubber Property—Change in
metals, elastomers, plastics, lubricants, and other materials as
Length During Liquid Immersion
applicable.
D 2240 Test Method for Rubber Property—Durometer
1.2 This standard should be used to measure and describe
Hardness
the properties of materials, products, or assemblies in response
D 2510 Test Method for Adhesion of Solid Film Lubricants
to heat and flame under controlled laboratory conditions and
D 3183 Practice for Rubber—Preparation of Pieces for Test
should not be used to describe or appraise the fire hazard or
Purposes from Products
fire risk of materials, products, or assemblies under actual fire
E 8 Test Methods of Tension Testing of Metallic Materials
conditions. However, results of this test may be used as
G 1 Practice for Preparing, Cleaning, and Evaluating Cor-
elements of a fire risk assessment which takes into account all
rosion Test Specimens
of the factors which are pertinent to an assessment of the fire
2.2 ANSI Standards:
hazard of a particular end use.
ANSI MC 96.1 Temperature Measurement Thermocouples
1.3 This standard does not purport to address all of the
2.3 Military Standards:
safety concerns, if any, associated with its use. It is the
MIL-C-81302 C Cleaning Compound, Solvent, Trichlorot-
responsibility of the user of this standard to establish appro-
rifluoroethane
priate safety and health practices and determine the applica-
MIL-C-27401 C Propellant Pressurizing Agent, Nitrogen
bility of regulatory limitations prior to use.
MIL-P-26539 Propellant, Nitrogen Tetroxide.
2. Referenced Documents
3. Summary of Practice
2.1 ASTM Standards:
3.1 The practice is essentially an examination to detect and
D 380 Test Methods for Rubber Hose
measure changes in physical, chemical, and mechanical prop-
D 412 Test Methods for Vulcanized Rubber and Thermo-
3 erties of the specimens and the propellant. The changes are
plastic Rubbers and Thermoplastic Elastomers-Tension
observed visually or measured with precise tools before and
D 471 Test Method for Rubber Property—Effect of Liq-
3 after static, unstressed immersion of the material of construc-
uids
tion in N O under predetermined standard conditions of time,
2 4
D 543 Practice for Evaluating Resistance of Plastics to
4 temperature, pressure, and other selected parameters. Liquid
Chemical Reagents
phase, vapor phase, critical, and interfacial tests are included.
D 618 Practice for Conditioning Plastics and Electrical
4 3.2 Because N O is a very reactive substance, compatibil-
Insulating Materials for Testing 2 4
ity tests are generally conducted in two successive steps as
follows:
This practice is under the jurisdiction of ASTM Committee F-7 on Aerospace
and Aircraft and is the direct responsibility of Subcommittee F07.02on Propellant
Annual Book of ASTM Standards, Vol 05.01.
Technology.
Annual Book of ASTM Standards, Vol 03.01.
Current edition approved Aug. 27, 1982. Published October 1982. Originally
Annual Book of ASTM Standards, Vol 03.02.
published as F359 – 72. Last previous edition F359 – 72 (1977). Available from the American National Standards Institute, 11 West 42nd Street,
Annual Book of ASTM Standards, Vol 09.02. 13th Floor, New York, NY 10036.
3 9
Annual Book of ASTM Standards, Vol 09.01. Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
Annual Book of ASTM Standards, Vol 08.01. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
F 359
3.2.1 First, a carefully executed exposure of the specimen to established for the operating aerospace application must be
determine if any unpredictable, spontaneous, or gross chemical used since the added impurities can drastically affect material
reaction or physical deterioration will occur. compatibility. As a minimum the N O must be analyzed in
2 4
3.2.2 Second, corrosion and compatibility measurements in accordance with the specification prior to immersion.
accordance with this practice. 6.2 Cleaning Solvents:
6.2.1 Ethyl Alcohol, ACS reagent grade.
4. Significance and Use
6.2.2 Trichlorotrifluoroethane, conforming to specification
4.1 Use limits are based on end-use requirements of the
MIL-C-81302.
N O . The quality status, revealed by tests, compared to use 6.3 Gases for Purging and Pressurizing—Gaseous nitrogen
2 4
limits affords a basis for accepting N O into a subsequent
conforming to specification MIL-P-27401.
2 4
storage or handling system. Use limits must not be the criteria 6.4 Liquid—Nitrogen tetroxide conforming to specification
for procurement acceptance where the military specification is
MIL-P-26539.
the applicable standard.
7. Properties of Nitrogen Tetroxide
5. Apparatus
7.1 Boiling Point, 21.1°C (70°F),
O
5.1 General—Apparatus that comes in contact with N
2 4 7.2 Freezing Point, −11.2°C (11.8°F),
3 3
should be made of borosilicate glass, 304 stainless steel, 6061
7.3 Density at 20°C (68°F), 1447 kg/m (1.447 g/cm ), and
aluminum, polytetrafluoroethylene plastic, or other materials
7.4 Critical Temperature, 158.2°C (316.8°F).
known to be compatible, and be free of contaminants, lubri-
cants, sealants, and extractables that might react with the N O 8. Safety Precautions
2 4
or otherwise interfere with the practice.
8.1 Toxicity—Nitrogen tetroxide is a dangerous substance.
5.2 Containers: 11
It is classified as a Class-A poison (1). The threshold limit
5.2.1 Vials.
value for nitrogen dioxide is 5 ppm (2). Breathing N O vapors
2 4
5.2.2 Corrosion Tubes.
or spilling liquid N O onto the body must be avoided. It is
2 4
5.2.3 Pressure Glass Jars, graduated in millilitres.
recommended that the user familiarize himself with the hazards
5.2.4 Stainless Steel Pressure Containers.
of N O and arrange for the necessary safety precautions prior
2 4
5.2.5 Staco Cells (optional).
to running any tests (3,4).
5.3 Temperature-Monitoring Instruments and Controls:
8.2 Flammability and Explosion Hazards—When properly
5.3.1 Constant-Temperature Bath.
stored, pure N O is a stable, nonflammable, shock-insensitive
2 4
5.3.2 Constant-Temperature Oven.
liquid. It is during handling that explosion or fire hazards might
5.3.3 Thermocouples (see 2.2).
develop. For example, accidental contact with paper, cloth,
5.4 Pressure-Monitoring Instruments and Controls.
various organic substances, solvent residues, certain chlorocar-
5.5 Measuring Devices:
bons, alcohols, and other chemicals can result in spontaneous
5.5.1 Balance, accurate to 60.0001 g.
ignition or form a shock-sensitive mixture (3,5,6,7,8,9).
5.5.2 Microscope with photographic attachment (30 power
minimum).
9. Test Specimens
5.5.3 Color Comparison Indicators for N O and speci-
2 4
9.1 General Requirements—The test materials shall be the
mens.
same chemically, physically, or metallurgically or both as the
5.6 Transfer Equipment:
material of construction to be used in the operating N O
2 4
5.6.1 Tubing.
system. Organic materials, such as plastics, greases, etc., vary
5.6.2 Valves.
considerably from batch to batch. Specification on critical
5.6.3 Disposal Vessel.
materials require performing this evaluation on every batch or
5.6.4 Cylinder Sand.
lot. The cleaning and preparation steps to be used must be
5.6.5 Flowmeters.
equivalent to those used in the system.
5.6.6 Sight Glasses.
9.2 Types of Specimens:
5.7 Safety Equipment:
9.2.1 Pure Specimens—Materials as received from vendors
5.7.1 Protective Clothing.
or prepared are cleaned and polished (metals) prior to test.
5.7.2 Fans.
9.2.2 Processed Specimens—Materials as received from
5.7.3 Shields.
vendors or prepared are processed in the same fashion as those
5.7.4 Controlled Environment.
materials used in operating systems. In effect, these samples
5.7.5 Fire-Fighting Equipment.
5.8 Dry Box for preparation of sample, test fluid, and
container.
Reagent Chemicals, American Chemical Society Specifications, American
5.9 First Aid Equipment.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
6. Reagents and Materials
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
6.1 The N O used in this practice must be of the same
2 4
MD.
quality and type (NTO or MON-1) as used in the final
The boldface numbers in parentheses refer to the list of reference at the end of
application. Nitrogen tetroxide conforming to the use limits this practice.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
F 359
will have the same history and surface finish as those to be provided in Test Method D 1460. The method does not permit
encountered in service. determination of the changes in mechanical properties.
9.3 Dimensions of Specimens—The size and shape of speci-
10.1.6 Clean specimens to remove contaminants. The clean-
mens may vary with the purpose of the test, the nature of the
ing agent used must not permanently affect the specimen nor
materials to be tested, and testing apparatus to be used. The
leave a residue. The cleaning and preparation steps to be used
size may also be limited by the necessity of preserving a proper
must be equivalent to those used in the system.
ratio between the area of the specimen and the quantity of
10.2 Plastic Specimens:
N O when the latter must be limited. However, when possible,
2 4 10.2.1 Prepare test strips for mass and dimension changes
the size of the specimens should conform to the requirements
measuring 76.00 by 25.00 by 3.20 6 0.20 mm (2.99 by 0.98 by
of Section 10.
0.13 6 0.008 in.) in accordance with Test Method D 543. The
9.4 Number of Specimens—A sufficient number of samples
method of cutting shall be such as to ensure that opposite ends
shall be prepared from a single lot of material to run at least
are parallel. Specimens for tensile strength and other physical
three tests for each set of conditions to be evaluated.
tests must conform to dimensions in accordance with the
9.5 Handling—Precautions must be taken to prevent han-
mechanical property method that applies (see Section 11). For
dling that results in contamination of the specimen with
components of peculiar conformation, procure sheet material
fingerprints or other soils.
of the exact same plastic from the vendor for preparation of test
specimens.
10. Preparation of Test Specimens
10.2.2 Clean the specimens to remove contaminants, mois-
10.1 Elastomer Specimens—:
ture, burrs, flashing, etc. The cleaning agent used shall not
10.1.1 Prepare the test specimens in accordance with their
permanently affect the plastic nor leave a residue. The cleaning
source and the tests to be performed.
and preparation steps to be used must be equivalent to those
10.1.2 Specimens for change in mass or volume shall be
used in the system. Make all edges smooth by cutting,
rectangular, having dimensions of 50.80 by 25.40 by 2.03 6
machining, or by finishing with No. 0 or finer sandpaper, or
0.13 mm (2 by 1 by 0.086 0.005 in.) as described in Test
emery cloth prior to cleaning.
Method D 471.
10.2.3 Condition the specimens for at least 40 h in accor-
NOTE 1—Specimens from commercial articles shall be the thickness of
dance with Procedure A of Practice D 618, unless otherwise
the material as received when it is less than 2.03 mm; otherwise, buff them
prescribed in the particular material specifications.
to a thickness of 2.03 6 0.13 mm, as described in Practice D 3183. Data
10.3 Metal Specimens:
obtained on specimens having different original thicknesses are not
10.3.1 Prepare the specimens in accordance with Recom-
comparable.
mended Practice G 1, unless otherwise specified. Specimens
10.1.3 Cut specimens for change in tensile strength, elon-
for loss of mass (rate of corrosion) shall be 50.00 by 20.00 by
gation, and durometer hardness from flat vulcanized sheets
2.00 6 0.10 mm (1.97 by 0.79 by 0.08 6 0.004 in.) in size
2.03 6 0.13 mm (0.08 6 0.005 in.) thick using die C of Test
unless otherwise specified. Size the specimens for change of
Methods D 412. For each test condition, six specimens are
tensile strength and elongation to fit the test method (see
required, including three for the controls. Subject these control
Section 11).
specimens to the same temperature for the same time as the test
10.3.2 Preparation of Specimens:
specimens, but without N O .
2 4
10.3.2.1 For laboratory corrosion tests that simulate expo-
NOTE 2—Special techniques for the tensile strength of completed hose
sure to service environments, a commercial surface closely
are available in Test Methods D 380, which contains specific instructions
resembling the one that would be used in service yields the
for conducting immersion testing of specimens cut from the hose in
most significant results.
Sections 23 through 27 therein. These specimens differ from 10.1.2 in that
10.3.2.2 Thoroughly clean the specimens and remove con-
they must not be more than 1.6 mm (0.062 in.) thick for the change in
volume test. taminants which might react with N O . The final cleaning
2 4
agent shall be essentially free of residue. Water based cleaners
10.1.4 Use specimens consisting of O-rings as received,
must be followed by an alcohol dip after thoro
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