Designation: D 1720 – 03

Standard Test Method for

Dilution Ratio of Active Solvents in Cellulose Nitrate
Solutions1
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* 3. Terminology
1.1 This test method covers the determination of the volume 3.1 Definitions of Terms Specific to This Standard:
ratio of hydrocarbon diluent to active solvent required to cause 3.1.1 dilution ratio, n—the maximum number of unit vol-
persistent heterogeneity (precipitation) in a solution of cellu- umes of a diluent that can be added to a unit volume of solvent
lose nitrate. to cause the first persistent heterogeneity (precipitation) in the
1.2 The values stated in SI units are to be regarded as the solution at a concentration of 8 g cellulose nitrate per 100 mL
standard. The values given in parentheses are for information of combined solvent plus diluent and at a temperature of 25 6
only. 3°C.
1.3 The following applies to all specified limits in this NOTE 1—The dilution ratio decreases as the cellulose nitrate concen-
standard; for purposes of determining conformance with this tration at the end point increases. It is, therefore, necessary to set an
standard, an observed value or a calculated value shall be arbitrary concentration of cellulose nitrate as part of the dilution ratio
rounded off “to the nearest unit” in the last right-hand digit term. For this purpose 8.0 g of cellulose nitrate per 100 mL of solvent plus
used in expressing the specification limit, in accordance with diluent has been adopted.
the rounding-off method of Practice E 29.
4. Significance and Use
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.1 By use of standard or reference grade materials for any
responsibility of the user of this standard to establish appro- two of the three components, namely, oxygenated solvent,
priate safety and health practices and determine the applica- diluent, or cellulose nitrate, the effect of different batches or
bility of regulatory limitations prior to use. For specific hazard different types of the third component can be determined.
statements, see Section 6. 4.2 This test method is applicable for the determination of
1.5 For hazard information and guidance, see the supplier’s the following:
Material Safety Data Sheet. 4.2.1 The dilution ratio of toluene as the standard diluent to
an oxygenated solvent under test, using as the solute standard
2. Referenced Documents cellulose nitrate as defined in 5.2.
2.1 ASTM Standards: 2 4.2.2 The dilution ratio of a hydrocarbon diluent under test
D 301 Test Methods for Soluble Cellulose Nitrate to n-butyl acetate as the standard solvent, using as a solute
D 841 Specification for Nitration Grade Toluene standard cellulose nitrate as defined in 5.2.
D 4615 Specification for n-Butyl Acetate (All Grades) 4.2.3 The dilution ratio of toluene, as the standard diluent, to
E 29 Practice for Using Significant Digits in Test Data to n-butyl acetate as the standard solvent, using as the solute
Determine Conformance with Specifications cellulose nitrate of varying solubility characteristics.
4.3 The information developed through this test may be
useful in the formulation of cellulose-based lacquers and
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint adhesives.
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. 5. Materials
Current edition approved Dec. 1, 2003. Published December 2003. Originally
approved in 1960. Last previous edition approved in 1996 as D 1720 – 96 (2000). 5.1 n-Butyl Acetate (90 to 92 %), conforming to Specifi-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or cation D 4615.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on NOTE 2—This grade of n-butyl acetate contains 8 to 10 % n-butyl
the ASTM website. alcohol.

*A Summary of Changes section appears at the end of this standard.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D 1720 – 03
5.2 Cellulose Nitrate, conforming to the Sampling section by a water aspirator or other vacuum source, the alcohol-wet
(Appearance, Ash, and Stability requirements) of Test Methods cellulose nitrate will be dried in about 4 h.
D 301 and of such quality that, when used in determining the 7.3 If larger quantities of cellulose nitrate are required, the
toluene dilution ratios of n-butyl acetate and methyl n-propyl drying equipment described in the Procedure section of Drying
ketone, it will give results between the following limits: Samples of Test Methods D 301 may be used.
Toluene Dilution Ratio

n-butyl acetate 2.73 to 2.83

8. Preparation of Solution
methyl n-propyl ketone 3.80 to 3.90 8.1 When testing either a solvent or diluent, first estimate
5.3 Toluene (Toluol), conforming to Specification D 841. the probable dilution ratio for the unknown component in
relation to the other to determine the amount of solvent
6. Hazards required to dissolve the cellulose nitrate (Table 1). This volume
6.1 Soluble cellulose nitrate is a flammable material, the of solvent should be such that there will be approximately 10 g
degree of flammability varying with the extent and nature of of cellulose nitrate present per 100 mL of solvent plus diluent
the wetting medium. Cellulose nitrate is always wet with water at the end point.
or alcohol in commercial handling, shipping, and storage, in NOTE 3—Reference to published data on similar types of solvents or
which condition it presents no unusual hazard. Dry cellulose diluents will provide a good approximation of the amount of solvent
nitrate, if ignited by fire, spark, or static electricity, burns very required. If data are not available, several solutions with varying amounts
rapidly. Do not store samples of dry cellulose nitrate at any of solvents may be required to arrive at a suitable volume to use.
time. Dry only that portion required for immediate test. Wear a 8.2 On an analytical balance, weigh 5 6 0.01 g of the
face shield when the oven is opened after samples have been cellulose nitrate into a 125-mL cork-stoppered, preweighed
heated. Wet excess material and the samples left after testing Erlenmeyer flask, or other suitable container. From a buret add
with water and dispose of properly. the volume of solvent indicated in Table 1. Swirl the flask until
7. Drying Cellulose Nitrate the cellulose nitrate is completely dissolved. When a high
concentration of cellulose nitrate in solvent is required, disper-
7.1 Dry not more than 20 g of cellulose nitrate at a time by sion may be more quickly accomplished by adding a measured
spreading in a thin layer on a tray at room temperature for 12 portion of the diluent to the flask. This reduces the solids
to 16 h, or on top of a 100°C oven where the temperature is 35 concentration and thus lowers the viscosity of the solution,
to 40°C for about 8 h (Warning, see 6.1). Alternatively, use a making it easier to dissolve the cellulose nitrate.
steam or hot water-heated oven maintained at 45 to 50°C to dry
specimens in about 8 h. For safety reasons, the oven should 9. Procedure
have the latch removed.
7.2 Another simple way to dry small quantities of cellulose 9.1 Add the diluent, maintained at 25 6 3.0°C, to the flask
nitrate is to use a drier assembled from common laboratory from a buret in small additions. Five-millilitre increments may
apparatus. The assembled drier is shown in Fig. 1. Hot air from be added at first, but these shall be decreased to about 0.5 mL
a laboratory electric oven is drawn through wet cellulose as the end point is approached. After each addition, stopper the
nitrate contained in a brass tube hooked up through a thistle flask and swirl vigorously to disperse any gel or precipitate
tube, or small funnel, and suction flask to a water aspirator or thrown down by local overconcentration of diluent (Note 4).
other vacuum source. The brass pipe should be about 40 mm in When precipitation persists after at least 2 min of vigorous
diameter and 200 mm long, these relative dimensions having swirling, the initial end point has been reached, as indicated by
been found to give efficient results. Such a tube will hold about the presence of gel particles in the solution or on the sides of
25 g, dry weight, of wet cellulose nitrate. The pipe is insulated the flask (Note 5). Determine the total volume of diluent added
to conserve heat. The suction flask end of the brass tube is fitted to the flask at this point.
with a thistle tube, or a small funnel, over the mouth of which NOTE 4—Take care to prevent loss of volatile components by evapo-
is tied a silk cloth screen. An indentation made in the funnel ration. Avoid contact of the solution with the stopper.
edge allows insertion of the thermometer. The funnel and NOTE 5—Presence of a uniform fine haze that is usually formed when
thermometer are held in place by means of a rubber stopper. aliphatic hydrocarbons are used as diluents must not be confused with the
When using an oven temperature of 85°C and vacuum supplied gel end point.

FIG. 1 Assembled Drier

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 D 1720 – 03
TABLE 1 Volume of Solvent Required to Dissolve Cellulose
Nitrate
Probable Dilution Ratio, volume of mL of Solvent per 5 g of Cellulose
diluent:volume of solvent Nitrate at 25°C
1 25.0
2 16.7
3 12.5
4 10.0
5 8.3

9.2 Determine a second end point using the same solution.

This requires addition of solvent to redissolve the cellulose FIG. 3 Grams of Cellulose Nitrate per 100 mL of Volatile Matter
nitrate. The amount of solvent to add depends upon the amount versus Dilution Ratio
of diluent used in the initial titration. The volume of solvent to
concentration is not necessarily a straight line, the error made
be added is obtained directly from Fig. 2 and the volume of
by interpolating or extrapolating from the straight line connect-
diluent used to reach the initial end point.
ing the two points is negligible in the proximity of 8 6 1 g/100
9.3 After addition of the required volume of solvent, swirl
mL of volatile matter.
the flask to redisperse the cellulose nitrate. Then, continue the
titration with diluent to the second end point, at which point NOTE 6—Example: Assuming a probable dilution ratio of approxi-
there should be approximately 8 g of cellulose nitrate present mately 3, the following results are obtained:
per 100 mL of solvent plus diluent. Solvent
Initial Added Second
End (from End
10. Calculation Point Fig. 2) Point
10.1 Calculate the dilution ratio and cellulose nitrate con-
Cellulose nitrate, g 5.00 ... 5.00
centration at both the initial and the second end points as Solvent, mL 12.5 3 15.5
follows: Diluent, mL 35.0 ... 49.6
Solvent plus diluent, mL 47.5 ... 65.1
Dilution ratio 5 A/B (1) Dilution ratio 35/12.5 = 2.8 ... 49.6/15.5
Cellulose nitrate concentration per 100 mL of volatile matter 5 = 3.2
Cellulose nitrate per 100 mL of 10.5 ... 7.7
C/~A 1 B! volatile matter, g
From Fig. 3 the dilution ratio at 8.0 g of cellulose nitrate = 3.16
where:
A = diluent for the titration, mL, 11. Report
B = solvent used, mL, and 11.1 When testing solvents, report the ratio of the volume of
C = cellulose nitrate used, g. toluene to the volume of solvent at 8 g of cellulose nitrate per
10.2 Construct a graph for dilution ratio versus cellulose 100 mL of volatile matter.
nitrate concentration. Plot as two points on the graph (Fig. 3) 11.2 When testing diluents, report the ratio of the volume of
the two sets of values calculated as described in 10.1. One of diluent to the volume of n-butyl acetate at 8 g of cellulose
the points will be very close to 8 g/100 mL of volatile matter. nitrate per 100 mL of volatile matter.
The correct value at exactly 8 g/100 mL of volatile matter may 11.3 When testing cellulose nitrate, report the ratio of the
be interpolated by drawing a straight line connecting the two volume of toluene to the volume of n-butyl acetate at 8 g of
experimentally determined points. While the curve showing cellulose nitrate per 100 mL of volatile matter.
the relationship between the dilution ratio and cellulose nitrate
12. Precision and Bias
12.1 Precision—The following criteria should be used for
judging the acceptability of results at the 95 % confidence
level.
12.1.1 Repeatability—Two results obtained by the same
operator should be considered suspect if they differ by more
than 0.1.
12.1.2 Reproducibility—Two results obtained by operators
in different laboratories should be considered suspect if they
differ by more than 0.2.
12.2 Bias—This test method has no bias because the value
of the test result is defined only in terms of the test method.
13. Keywords
FIG. 2 Volume of Solvent to Be Added to Complete Titration 13.1 active solvents; cellulose nitrate solutions; dilution
versus Volume of Diluent Used to Reach Initial End Point ratio; hydrocarbon diluent

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 D 1720 – 03

SUMMARY OF CHANGES

Committee D01.35 has identified the location of selected changes to this standard since the last issue
(D 1720 – 96 (2000)) that may impact the use of this standard.

(1) Added reference to Practice E 29 in 1.3 of the Scope (3) Added statement to Significance and Use section to show
section. applicability to lacquers and adhesives.
(2) Added Practice E 29 to the list of Referenced Documents.

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