ASTM D301-95(1999)
(Test Method)Standard Test Methods for Soluble Cellulose Nitrate
Standard Test Methods for Soluble Cellulose Nitrate
SCOPE
1.1 These test methods cover the material known as soluble cellulose nitrate (also known as soluble nitrocellulose), which is shipped wet in conformance with regulations of the Interstate Commerce Commission.
1.2 The test methods appear in the following sections: SectionsAsh5-7Drying Samples4Nitrogen8-10Stability11-13Toluene Dilution22-24Viscosity14-18
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. For specific hazard statements, see Notes 2 - 5.
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Federation of Societies for
Designation: D 301 – 95 (Reapproved 1999) Paint Technology Standard No. Cs-2-58
Standard Test Methods for
Soluble Cellulose Nitrate
This standard is issued under the fixed designation D 301; 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.
1. Scope the barrels, two samples of approximately 1 pt (0.5 dm ) each
shall be taken from two well-separated points at least 1 ft (0.3
1.1 These test methods cover the material known as soluble
m) beneath the surface of the material in the barrel. These
cellulose nitrate (also known as soluble nitrocellulose), which
samples shall then be composited to represent each lot or batch
is shipped wet in conformance with regulations of the Interstate
in the shipment.
Commerce Commission.
3.2 The samples shall meet the following requirements:
1.2 The test methods appear in the following sections:
3.2.1 Appearance—The cellulose nitrate shall not be discol-
Sections
ored and shall be free of lumps and foreign matter, such as
Ash 5-7
charred particles.
Drying Samples 4
3.2.2 Ash—Ash content shall not exceed 0.30 %, calculated
Nitrogen 8-10
on the basis of dry-weight soluble cellulose nitrate.
Stability 11-13
Toluene Dilution 22-24
3.2.3 Nitrogen—The percent nitrogen, calculated on the
Viscosity 14-18
basis of dry-weight soluble cellulose nitrate, shall be within the
1.3 This standard does not purport to address all of the
limits agreed upon by the purchaser and the manufacturer for
safety concerns, if any, associated with its use. It is the
the particular type of soluble cellulose nitrate.
responsibility of the user of this standard to establish appro-
3.2.4 Stability—The stability as determined by the 134.5 C
priate safety and health practices and determine the applica-
test shall be not less than 25 min.
bility of regulatory limitations prior to use. For specific hazard
3.2.5 Viscosity—The viscosity shall be within the limits
statements, see Notes 2-5.
agreed upon by the purchaser and the manufacturer for the
particular type of soluble cellulose nitrate.
2. Referenced Documents
3.2.6 Solubility and Appearance of the Solution—The solu-
2.1 ASTM Standards:
bility and appearance of the sample shall be equal to the
D 302 Specification for Ethyl Acetate (85 to 88 Percent
reference standard for the particular type of soluble cellulose
Grade)
nitrate.
D 303 Specification for n-Butyl Acetate (90 to 92 %
3.2.7 Film Test—The film test of the sample shall be equal
Grade)
to that of the reference standard for the particular type of
D 362 Specification for Industrial Grade Toluene
soluble cellulose nitrate.
D 1343 Test Method for Viscosity of Cellulose Derivatives
3.2.8 Toluene Dilution Test—The toluene dilution value of
by Ball-Drop Method
the sample shall be equivalent to that of the reference standard
D 4795 Test Method for Nitrogen Content of Soluble
for the particular type of soluble cellulose nitrate.
Nitrocellulose—Alternative Method
DRYING SAMPLES
E 1 Specification for ASTM Thermometers
4. Procedure
3. Sampling
4.1 Soluble cellulose nitrate is a flammable material, the
3.1 Samples shall be taken from not less than 10 % (at least
degree of flammability varying with the extent and nature of
two barrels) of each lot or batch in the shipment. In sampling
the wetting medium. Cellulose nitrate is always wet with water
or alcohol in commercial handling, shipping, and storage, in
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
which condition it presents no unusual hazard. Dry cellulose
and Related Coatings, Materials, and Applications, and are the direct responsibility
nitrate, if ignited by fire, spark, or static electricity, burns very
of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
rapidly. Samples of dry cellulose nitrate must not be stored at
Current edition approved Sept. 15, 1995. Published November 1995. Originally
published as D 301 – 29. Last previous edition D 301 – 89.
any time. Dry only that portion required for immediate test.
Discontinued, see 1986 Annual Book of ASTM Standards, Vol 06.03.
Wet the excess material and the samples left after testing with
Annual Book of ASTM Standards, Vol 06.03.
4 water and dispose of by burning on a safe burning ground.
Annual Book of ASTM Standards, Vol 14.03.
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D 301
4.2 Dry small quantities required for ash and nitrogen tests 10. Precision and Bias
by spreading in a thin layer on a tray at room temperature for
10.1 Precision—Statistical analysis of intralaboratory (re-
12 to 16 h, followed by oven-drying in crucibles or weighing
peatability) test results on a sample containing approximately
bottles1hat100 to 105°C. The oven used for drying cellulose
0.015 % ash indicates a precision of 60.015 % absolute at the
nitrate should have the latch removed. Wear a face mask (see
95 % confidence level.
12.2) when the oven is opened after samples have been heated.
10.2 Bias—No statement of bias can be made as no suitable
4.3 Dry larger quantities of water-wet material required for
reference material is available as a standard.
viscosity and toluene dilution tests, or a small quantity for
stability tests, by blowing warm compressed air (at a tempera-
NITROGEN
ture of 60 to 65°C, and a pressure of 40 to 60 psi (275 to 415
kPa)) through the sample placed in a cylindrical holder with a
11. Significance and Use
screen over one end for ⁄2 to 1 h. Provide the compressed air
11.1 The nature and strength of solvent systems required for
line with a safety plug (Note 1) of Wood’s metal, which melts
cellulose nitrate are dependent upon the nitrogen content.
at 70 to 75°C, so the air will be diverted from the sample if a
Mismatches of solvent with nitrogen level can result in poor
temperature of 70°C is exceeded.
solution quality and colloid and gel formation.
NOTE 1—Information on the availability of a suitable fusible plug
11.2 An alternative preferred method can be found in Test
assembly may be obtained from ASTM Headquarters.
Method D 4795.
4.4 If the material is alcohol-wet, it is necessary to modify
12. Apparatus
the drying procedure. After placing the required amount of
12.1 Nitrometer—Use the duPont Nitrometer, which is il-
cellulose nitrate in the cylindrical holder, pour in sufficient
distilled or iron-free water to fill it. Allow the bulk of the liquid lustrated in Figs. 1-4.
12.2 Face Mask—A face mask, so constructed that a heavy
to drain off. Then dry by blowing warm air through the holder
as described in 4.3. piece of cellulose acetate sheeting protects the face.
NOTE 2—Precaution: The cellulose acetate mask must be worn during
ASH
the generation and measurement of the gas as a precaution in case of an
explosion.
5. Significance and Use
13. Procedure
5.1 Ash accounts for the nonsoluble, nonfilm forming por-
13.1 Calibrate the measuring tube accurately in the usual
tion of the polymer. It may affect solution clarity and film
manner, using mercury as the calibrating liquid.
properties.
13.2 Standardize the apparatus as follows:
13.2.1 Fill the compensating, measuring, and reaction tubes
6. Apparatus
and their rubber connections with mercury. Run 20 to 30 mL of
6.1 Porcelain Crucibles, Coors No. 3 or equivalent.
H SO (ACS grade, 94.5 6 0.5 %) into the reaction bulb
2 4
6.2 Muffle Furnace, maintained at 550 6 25°C.
through the cup at the top and admit about 210 mL of air. Close
the stopcocks, shake the bulb well, and allow to stand
7. Reagents
overnight. This desiccates the air which is then run into the
7.1 Ethyl Alcohol. compensating tube until the mercury is about on a level with
the 12.50 % mark on the measuring tube, the two tubes being
7.2 Acetone.
held at the same height. Then seal the compensating tube using
7.3 Castor Oil.
a small blowpipe flame.
13.2.2 As a preferred alternative, nitrogen may be used in
8. Procedure
place of air.
8.1 Dry the cellulose nitrate as described in 4.2 and place a
13.2.3 Place in weighing bottles 0.95 6 0.05-g portions of
specimen of approximately 4.0 g in a tared and ignited
ACS grade KNO that has been recrystallized twice from
crucible. Moisten the sample in the crucible with ethyl alcohol,
distilled water and ground to pass a No. 100 (150-μm) sieve.
then gelatinize by adding a sufficient amount of 5 % solution of
Dry the specimens 2 to3hat135to 150°C. Stopper the bottles,
castor oil into the acetone. Place the crucible in a draft-free
cool in a desiccator, and weigh accurately. Transfer the KNO
hood and ignite the contents with a Bunsen flame. Allow the
to the cup of the reaction bulb and weigh the weighing bottle
material to burn without further addition of heat until a charred
to obtain the weight of sample used. Add 1.0 mL of water and
residue remains. Place the crucible in a muffle furnace at 550
stir the mixture in the cup with a small glass stirring rod to
6 25°C for 90 min. Remove carefully the crucible from the
liberate the entrained bubbles of air; work the undissolved
muffle furnace to avoid loss of ash, cool in a desiccator, and
crystals into the lower part of the cup, keeping them below the
weigh accurately.
surface of the solution. It is not necessary that the KNO
dissolve before drawing it into the reaction bulb. Make sure the
9. Calculation
lower stopcock is open; then admit the mixture to the bulb by
9.1 Calculate the percent ash as follows:
a series of quick openings of the upper stopcock, in the
Ash, %5~wt of ash/wt of dry sample!3 100 meantime keeping the crystals below the surface of the liquid.
D 301
NOTE 1—1 in. = 25.4 mm.
FIG. 1 General Assembly of Apparatus for Nitrogen Determination
In this way, all but a small amount of the KNO may be run 13.4 When the reaction is completed, allow the gas to cool
into the bulb. Rinse the cup with a second 1.0-mL portion of for 20 min; then transfer the gas to a measuring tube. By means
water; then repeat with a third 1.0-mL portion (3 mL in all). of the leveling device make careful adjustment of the mercury
This should be sufficient to dissolve all remaining particles of levels so that the mercury in the measuring tube is at the
KNO in the cup. Transfer 25 mL of the H SO (94.5 6 13.85 % mark (the theoretical percent nitrogen in KNO )ifan
3 2 4 3
0.5 %), divided in several portions, to the cup, and subse- exactly 1.000-g specimen was used, or a proportional reading
quently to the bulb by lowering the reservoir slightly and if less was used. Paste a strip of paper on the compensating
opening and closing the upper stopcock, care being taken that tube at the level of the mercury, and the standardization is
no air enters even the bore hole in the
...
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