Standard Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method

SIGNIFICANCE AND USE
4.1 This test provides an easy method of determining the viscosity of cellulose derivatives in a given solvent. The answers are in units commonly used in industrial practice. Such information is needed for cellulose derivatives that are to be extruded, molded, sprayed, or brushed as is or in solution.
SCOPE
1.1 This test method describes the apparatus and general procedure for making ball-drop viscosity measurements on solutions of various cellulose derivatives. Instructions for sample preparation, solution concentration, and other details are discussed in the ASTM methods for the respective cellulose derivatives.  
1.2 This test method is applicable to solutions of various cellulose derivatives having viscosities greater than 10 P, by using balls of various diameters and densities. Viscosity results are expressed preferably in poises.  
1.3 In commercial practice, viscosities are often expressed in seconds using 2.38-mm (3/32-in.) stainless steel balls.2 When the viscosity is outside the practical range for these balls (75 to 300 P), the measurement can be made using a calibrated pipet viscometer or a different ball and calculating the observed viscosity to the corresponding time for a 2.38-mm (3/32-in.) ball, even though it is a small fraction of a second.  
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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Publication Date
30-Nov-2019
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ASTM D1343-95(2019) - Standard Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D1343 − 95 (Reapproved 2019)
Standard Test Method for
Viscosity of Cellulose Derivatives by Ball-Drop Method
This standard is issued under the fixed designation D1343; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 2. Referenced Documents
1.1 This test method describes the apparatus and general 2.1 ASTM Standards:
procedure for making ball-drop viscosity measurements on D301 Test Methods for Soluble Cellulose Nitrate (With-
solutions of various cellulose derivatives. Instructions for drawn 2011)
sample preparation, solution concentration, and other details D445 Test Method for Kinematic Viscosity of Transparent
arediscussedintheASTMmethodsfortherespectivecellulose and Opaque Liquids (and Calculation of Dynamic Viscos-
derivatives. ity)
D817 Test Methods of Testing Cellulose Acetate Propionate
1.2 This test method is applicable to solutions of various
and Cellulose Acetate Butyrate
cellulose derivatives having viscosities greater than 10 P, by
D871 Test Methods of Testing Cellulose Acetate
using balls of various diameters and densities.Viscosity results
E691 Practice for Conducting an Interlaboratory Study to
are expressed preferably in poises.
Determine the Precision of a Test Method
1.3 In commercial practice, viscosities are often expressed
in seconds using 2.38-mm ( ⁄32-in.) stainless steel balls. When
3. Summary of Test Method
the viscosity is outside the practical range for these balls (75 to
3.1 A solution of the cellulose derivative is made in a
300 P), the measurement can be made using a calibrated pipet
suitable solvent and allowed to equilibrate at a chosen tem-
viscometer or a different ball and calculating the observed
perature.Astainless steel or aluminum ball is dropped into the
viscosity to the corresponding time for a 2.38-mm ( ⁄32-in.)
solution, and the time required for it to cover a measured
ball, even though it is a small fraction of a second.
distance in its fall is recorded.The viscosity of the solution can
1.4 The values stated in SI units are to be regarded as the
then be calculated in poise or recorded in seconds.
standard. The values given in parentheses are for information
NOTE 1—The choice of solvent has significant influence on viscosity.
only.
1.5 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 This test provides an easy method of determining the
responsibility of the user of this standard to establish appro-
viscosity of cellulose derivatives in a given solvent. The
priate safety, health, and environmental practices and deter-
answers are in units commonly used in industrial practice.
mine the applicability of regulatory limitations prior to use.
Such information is needed for cellulose derivatives that are to
1.6 This international standard was developed in accor-
be extruded, molded, sprayed, or brushed as is or in solution.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5. Apparatus
Development of International Standards, Guides and Recom-
5.1 Constant-Temperature Water Bath, glass-walled.
mendations issued by the World Trade Organization Technical
5.1.1 For routine testing, an aquarium viscometer is recom-
Barriers to Trade (TBT) Committee.
mended. This viscometer is a rectangular glass enclosure with
front and rear walls that have etched horizontal parallel lines
This test method is under the jurisdiction of ASTM Committee D01 on Paint
50.8 mm (2.00 6 0.02 in.) apart. The bottles containing the
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved Dec. 1, 2019. Published December 2019. Originally
approved in 1954. Last previous edition approved in 2011 as D1343 – 95 (2011). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/D1343-95R19. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2 3
When a ⁄32-in. stainless steel ball is used, the viscosities in seconds should be Standards volume information, refer to the standard’s Document Summary page on
practically the same as those obtained using the apparatus described in Section 11 the ASTM website.
of Test Methods D871 – 48, and in Section 10 of Test Methods D301 – 50, which The last approved version of this historical standard is referenced on
last appeared in the 1952 Annual Book of ASTM Standards, Part 4. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1343 − 95 (2019)
TABLE 1 Bottles
6. Calibration
Bottle Round Square
6.1 Calculate the apparatus constant, K, using the following
Capacity, oz 16 16
equation and exact dimensions of the bottle and balls used:
Weight, oz 12 12
Height, in. 6.7 7
2 3
K 5 2gr 1 2 2.104 d/D 12.09 d/D /9L
@ ~ ! ~ ! #
Inside diameter, cm 6.4
Side to side, cm . 6.0
where:
Corner to corner, cm . 7.2
g = acceleration of gravity in cgs units
r = ball radius, cm,
d = ball diameter, cm,
D = bottle diameter, cm (in the case of square bottles the
samples solutions are set inside the viscometer at a level such
average of the side to side and corner to corner
that the upper etched line of the viscometer is at least 12.7 mm
diameters shall be used), and
( ⁄2 in.) below the upper surface of the solution in the bottle,
L = distance of ball drop, cm.
and the lower etched line of the viscometer is at least 12.7 mm
( ⁄2 in.) above the bottom of the sample bottle. Suitable lighting
7. Procedure
is provided to enable the observer to sight across the parallel
etched lines, through the sample bottle and solution, avoiding
7.1 Preparation of Solution—Dry the sample and prepare a
in this manner parallax errors. With this viscometer no timing
solution as specified for the particular material. Such instruc-
markers need to be provided on the bottles.
tions are given in the viscosity sections of Test Methods D301,
5.2 Bottles and Caps:
D871, and D817. Weigh into the bottle an appropriate amount
5.2.1 Bottles, round or square, conforming to the dimen-
of dry sample and specified solvent, accurate to 0.1 g, to make
sional requirements shown in Table 1, shall be used. Screw
about 350 mLof solution.The accurate and precise make up of
caps of metal or phenolic plastic in sizes to fit the bottles and
the solution is a necessity (example: 60.00 g of cellulose
having aluminum foil or cardboard and cellophane liners may
acetate and 240.00 g solvent). Close the bottle tightly.Allow to
be used to close the bottles. Alternatively, rubber stoppers
stand a short time for the solvent to penetrate the sample. Then
covered with aluminum or tin foil, may also be used as
tumble or shake until a uniform solution is obtained. For some
closures. In this latter case, solvent loss during measurement of
samples this may require several days. Transfer to the water
viscosity can be minimized by removing the stopper, leaving
bath at 25 6 0.1°C, and allow the solution to come to
the foil in place, and making a small hole in the center of the
temperature. A practical method to determine possible solvent
foil through which the balls may be dropped.
loss during this time involves weighing the bottle immediately
5.2.2 Timing marks sha
...

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