ASTM D1720-96
(Test Method)Standard Test Method for Dilution Ratio of Active Solvents in Cellulose Nitrate Solutions
Standard Test Method for Dilution Ratio of Active Solvents in Cellulose Nitrate Solutions
SCOPE
1.1 This test method covers the determination of the volume ratio of hydrocarbon diluent to active solvent required to cause persistent heterogeneity (precipitation) in a solution of cellulose nitrate.
1.2 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 Section 6.
1.3 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
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Designation: D 1720 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Dilution Ratio of Active Solvents in Cellulose Nitrate
Solutions
This standard is issued under the fixed designation D 1720; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope two of the three components, namely, oxygenated solvent,
diluent, or cellulose nitrate, the effect of different batches or
1.1 This test method covers the determination of the volume
different types of the third component can be determined.
ratio of hydrocarbon diluent to active solvent required to cause
4.2 This test method is applicable for the determination of
persistent heterogeneity (precipitation) in a solution of cellu-
the following:
lose nitrate.
4.2.1 The dilution ratio of toluene as the standard diluent to
1.2 This standard does not purport to address all of the
an oxygenated solvent under test, using as the solute standard
safety concerns, if any, associated with its use. It is the
cellulose nitrate as defined in 5.2.
responsibility of the user of this standard to establish appro-
4.2.2 The dilution ratio of a hydrocarbon diluent under test
priate safety and health practices and determine the applica-
to n-butyl acetate as the standard solvent, using as a solute
bility of regulatory limitations prior to use. For specific hazard
standard cellulose nitrate as defined in 5.2.
statements, see Section 6.
4.2.3 The dilution ratio of toluene, as the standard diluent, to
1.3 For hazard information and guidance, see the supplier’s
n-butyl acetate as the standard solvent, using as the solute
Material Safety Data Sheet.
cellulose nitrate of varying solubility characteristics.
2. Referenced Documents
5. Materials
2.1 ASTM Standards:
2 5.1 n-Butyl Acetate (90 to 92 %), conforming to Specifica-
D 301 Test Methods for Soluble Cellulose Nitrate
tion D 4615.
D 841 Specification for Nitration Grade Toluene
D 4615 Specification for n-Butyl Acetate (All Grades)
NOTE 2—This grade of n-butyl acetate contains 8 to 10 % n-butyl
alcohol.
3. Terminology
5.2 Cellulose Nitrate, conforming to the Sampling section
3.1 Definitions of Terms Specific to This Standard:
(Appearance, Ash, and Stability requirements) of Methods
3.1.1 dilution ratio—the maximum number of unit volumes
D 301 and of such quality that, when used in determining the
of a diluent that can be added to a unit volume of solvent to
toluene dilution ratios of n-butyl acetate and methyl n-propyl
cause the first persistent heterogeneity (precipitation) in the
ketone, it will give results between the following limits:
solution at a concentration of 8 g cellulose nitrate per 100 mL
Toluene Dilution Ratio
of combined solvent plus diluent and at a temperature of 25 6
3°C. n-butyl acetate 2.73 to 2.83
methyl n-propyl ketone 3.80 to 3.90
NOTE 1—The dilution ratio decreases as the cellulose nitrate concen-
5.3 Toluene (Toluol), conforming to Specification D 841.
tration at the end point increases. It is, therefore, necessary to set an
arbitrary concentration of cellulose nitrate as part of the dilution ratio
6. Hazards
term. For this purpose 8.0 g of cellulose nitrate per 100 mL of solvent plus
diluent has been adopted.
6.1 Soluble cellulose nitrate is a flammable material, the
degree of flammability varying with the extent and nature of
4. Significance and Use
the wetting medium. Cellulose nitrate is always wet with water
4.1 By use of standard or reference grade materials for any
or alcohol in commercial handling, shipping, and storage, in
which condition it presents no unusual hazard. Dry cellulose
nitrate, if ignited by fire, spark, or static electricity, burns very
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
rapidly. Do not store samples of dry cellulose nitrate at any
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
time. Dry only that portion required for immediate test. Wear a
Current edition approved Nov. 10, 1996. Published January 1997. Originally
face shield when the oven is opened after samples have been
published as D 1720 – 60 T. Last previous edition D 1720 – 93.
2 heated. Wet excess material and the samples left after testing
Annual Book of ASTM Standards, Vol 06.03.
Annual Book of ASTM Standards, Vol 06.04. with water and dispose of properly.
D 1720
TABLE 1 Volume of Solvent Required to Dissolve Cellulose
7. Drying Cellulose Nitrate
Nitrate
7.1 Dry not more than 20 g of cellulose nitrate at a time by
Probable Dilution Ratio, volume of mL of Solvent per5gof Cellulose
spreading in a thin layer on a tray at room temperature for 12
diluent:volume of solvent Nitrate at 25°C
to 16 h, or on top of a 100°C oven where the temperature is 35
1 25.0
to 40°C for about 8 h (Warning, see 6.1). Alternatively, use a
2 16.7
3 12.5
steam or hot water-heated oven maintained at 45 to 50°C to dry
4 10.0
specimens in about 8 h. For safety reasons, the oven should
5 8.3
have the latch removed.
7.2 Another simple way to dry small quantities of cellulose
concentration of cellulose nitrate in solvent is required, disper-
nitrate is to use a drier assembled from common laboratory
sion may be more quickly accomplished by adding a measured
apparatus. The assembled drier is shown in Fig. 1. Hot air from
portion of the diluent to the flask. This reduces the solids
a laboratory electric oven is drawn through wet cellulose
concentration and thus lowers the viscosity of the solution,
nitrate contained in a brass tube hooked up through a thistle
making it easier to dissolve the cellulose nitrate.
tube, or small funnel, and suction flask to a water aspirator or
other vacuum source. The brass pipe should be about 40 mm in
9. Procedure
diameter and 200 mm long, these relative dimensions having
9.1 Add the diluent, maintained at 25 6 3.0°C, to the flask
been found to give efficient results. Such a tube will hold about
from a buret in small additions. Five-millilitre increments may
25 g, dry weight, of wet cellulose nitrate. The pipe is insulated
be added at first, but these shall be decreased to about 0.5 mL
to conserve heat. The suction flask end of the brass tube is fitted
as the end point is approached. After ea
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