ASTM D1720-96(2000)
(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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 1720 – 96 (Reapproved 2000)
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 4. Significance and Use
1.1 This test method covers the determination of the volume 4.1 By use of standard or reference grade materials for any
ratio of hydrocarbon diluent to active solvent required to cause two of the three components, namely, oxygenated solvent,
persistent heterogeneity (precipitation) in a solution of cellu- diluent, or cellulose nitrate, the effect of different batches or
lose nitrate. different types of the third component can be determined.
1.2 This standard does not purport to address all of the 4.2 This test method is applicable for the determination of
safety concerns, if any, associated with its use. It is the the following:
responsibility of the user of this standard to establish appro- 4.2.1 The dilution ratio of toluene as the standard diluent to
priate safety and health practices and determine the applica- an oxygenated solvent under test, using as the solute standard
bility of regulatory limitations prior to use. For specific hazard cellulose nitrate as defined in 5.2.
statements, see Section 6. 4.2.2 The dilution ratio of a hydrocarbon diluent under test
1.3 For hazard information and guidance, see the supplier’s to n-butyl acetate as the standard solvent, using as a solute
Material Safety Data Sheet. standard cellulose nitrate as defined in 5.2.
4.2.3 The dilution ratio of toluene, as the standard diluent, to
2. Referenced Documents
n-butyl acetate as the standard solvent, using as the solute
2.1 ASTM Standards: cellulose nitrate of varying solubility characteristics.
D 301 Test Methods for Soluble Cellulose Nitrate
5. Materials
D 841 Specification for Nitration Grade Toluene
D 4615 Specification for n-Butyl Acetate (All Grades) 5.1 n-Butyl Acetate (90 to 92 %), conforming to Specifi-
cation D 4615.
3. Terminology
NOTE 2—This grade of n-butyl acetate contains 8 to 10 % n-butyl
3.1 Definitions of Terms Specific to This Standard:
alcohol.
3.1.1 dilution ratio—the maximum number of unit volumes
5.2 Cellulose Nitrate, conforming to the Sampling section
of a diluent that can be added to a unit volume of solvent to
(Appearance, Ash, and Stability requirements) of Test Methods
cause the first persistent heterogeneity (precipitation) in the
D 301 and of such quality that, when used in determining the
solution at a concentration of 8 g cellulose nitrate per 100 mL
toluene dilution ratios of n-butyl acetate and methyl n-propyl
of combined solvent plus diluent and at a temperature of 25 6
ketone, it will give results between the following limits:
3°C.
Toluene Dilution Ratio
NOTE 1—The dilution ratio decreases as the cellulose nitrate concen-
n-butyl acetate 2.73 to 2.83
tration at the end point increases. It is, therefore, necessary to set an
methyl n-propyl ketone 3.80 to 3.90
arbitrary concentration of cellulose nitrate as part of the dilution ratio
term. For this purpose 8.0 g of cellulose nitrate per 100 mL of solvent plus
5.3 Toluene (Toluol), conforming to Specification D 841.
diluent has been adopted.
6. Hazards
6.1 Soluble cellulose nitrate is a flammable material, the
This test method is under the jurisdiction of ASTM Committee D01 on Paint
degree of flammability varying with the extent and nature of
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
the wetting medium. Cellulose nitrate is always wet with water
Current edition approved Nov. 10, 1996. Published January 1997. Originally
or alcohol in commercial handling, shipping, and storage, in
published as D 1720 – 60 T. Last previous edition D 1720 – 93.
2 which condition it presents no unusual hazard. Dry cellulose
Annual Book of ASTM Standards, Vol 06.03.
Annual Book of ASTM Standards, Vol 06.04. nitrate, if ignited by fire, spark, or static electricity, burns very
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 1720
TABLE 1 Volume of Solvent Required to Dissolve Cellulose
rapidly. Do not store samples of dry cellulose nitrate at any
Nitrate
time. Dry only that portion required for immediate test. Wear a
Probable Dilution Ratio, volume of mL of Solvent per5gof Cellulose
face shield when the oven is opened after samples have been
diluent:volume of solvent Nitrate at 25°C
heated. Wet excess material and the samples left after testing
1 25.0
with water and dispose of properly.
2 16.7
3 12.5
7. Drying Cellulose Nitrate
4 10.0
5 8.3
7.1 Dry not more than 20 g of cellulose nitrate at a time by
spreading in a thin layer on a tray at room temperature for 12
to 16 h, or on top of a 100°C oven where the temperature is 35
to 40°C for about 8 h (Warning, see 6.1). Alternatively, use a
8.2 On an analytical balance, weigh 5 6 0.01 g of the
steam or hot water-heated oven maintained at 45 to 50°C to dry
cellulose nitrate into a 125-mL cork-stoppered, preweighed
specimens in about 8 h. For safety reasons, the oven should
Erlenmeyer flask, or other suitable container. From a buret add
have the latch removed.
the volume of solvent indicated in Table 1. Swirl the flask until
7.2 Another simple way to dry small quantities of cellulose
the cellulose nitrate is completely dissolved. When a high
nitrate is to use a drier assembled from common laboratory
concentration of cellulose nitrate in solvent is required, disper-
apparatus. The assembled drier is shown in Fig. 1. Hot air from
sion may be more quickly accomplished by adding a measured
a laboratory electric oven is drawn through wet cellulose
portion of the diluent to the flask. This reduces the solids
nitrate contained in a brass tube hooked up through a thistle
concentration and thus lowers the viscosity of the solution,
tube, or small funnel, and suction flask to a water aspirator or
making it easier to dissolve the cellulose nitrate.
other vacuum source. The brass pipe should be about 40 mm in
diameter and 200 mm long, these relative dimensions having
9. Procedure
been found to give efficient results. Such a tube will hold about
9.1 Add the diluent, maintained at 25 6 3.0°C, to the flask
25 g, dry weight, of wet cellulose nitrate. The pipe is insulated
from a buret in small additions. Five-millilitre increments may
to conserve heat. The suction flask end of the brass tube is fitted
be added at first, bu
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