ASTM D1343-95(2000)
(Test Method)Standard Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method
Standard Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method
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 3/32-in. (2.38-mm) stainless steel balls. 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 3/32-in. ball, even though it is a small fraction of a second.
1.4 The values stated in inch-pound 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:D1343–95(Reapproved2000)
Standard Test Method for
Viscosity of Cellulose Derivatives by Ball-Drop Method
This standard is issued under the fixed designation D 1343; 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 D 817 Test Methods of Testing Cellulose Acetate Propi-
onate and Cellulose Acetate Butyrate
1.1 This test method describes the apparatus and general
D 871 Test Methods of Testing Cellulose Acetate
procedure for making ball-drop viscosity measurements on
E 691 Practice for Conducting an Introlaboratory Study to
solutions of various cellulose derivatives. Instructions for
Determine the Precision of a Test Method
sample preparation, solution concentration, and other details
arediscussedintheASTMmethodsfortherespectivecellulose
3. Summary of Test Method
derivatives.
3.1 A solution of the cellulose derivative is made in a
1.2 This test method is applicable to solutions of various
suitable solvent and allowed to equilibrate at a chosen tem-
cellulose derivatives having viscosities greater than 10 P, by
perature.Astainless steel or aluminum ball is dropped into the
using balls of various diameters and densities.Viscosity results
solution, and the time required for it to cover a measured
are expressed preferably in poises.
distance in its fall is recorded.The viscosity of the solution can
1.3 In commercial practice, viscosities are often expressed
2 then be calculated in poise or recorded in seconds.
in seconds using 2.38–mm ( ⁄32-in.) stainless steel balls. When
the viscosity is outside the practical range for these balls (75 to
NOTE 1—The choice of solvent has significant influence on viscosity.
300 P), the measurement can be made using a calibrated pipet
4. Significance and Use
viscometer or a different ball and calculating the observed
viscosity to the corresponding time for a 2.38-mm ( ⁄32-in.) 4.1 This test provides an easy method of determining the
ball, even though it is a small fraction of a second.
viscosity of cellulose derivatives in a given solvent. The
1.4 The values stated in SI units are to be regarded as the answers are in units commonly used in industrial practice.
standard. The values given in parentheses are for information
Such information is needed for cellulose derivatives that are to
only. be extruded, molded, sprayed, or brushed as is or in solution.
1.5 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
TABLE 1 Bottles
priate safety and health practices and determine the applica-
Bottle Round Square
bility of regulatory limitations prior to use.
Capacity, oz 16 16
2. Referenced Documents
Weight, oz 12 12
Height, in. 6.7 7
2.1 ASTM Standards:
Inside diameter, cm 6.4
D 301 Test Methods for Soluble Cellulose Nitrate
Side to side, cm . 6.0
Corner to corner, cm . 7.2
D 445 Test Method for Kinematic Viscosity of Transparent
and Opaque Liquids
5.1 Constant-Temperature Water Bath, glass-walled.
5.1.1 For routine testing, an aquarium viscometer is recom-
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
mended. This viscometer is a rectangular glass enclosure with
and Related Coatings, Materials, andApplications and is the direct responsibility of
front and rear walls that have etched horizontal parallel lines
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
50.8 mm (2.00 6 0.02 in.) apart. The bottles containing the
Current edition approved Nov. 10, 1995. Published January 1996. Originally
published as D 1343 – 54. Last previous edition D 1343 – 93. samples solutions are set inside the viscometer at a level such
When a ⁄32-in. stainless steel ball is used, the viscosities in seconds should be
that the upper etched line of the viscometer is at least 12.7 mm
practically the same as those obtained using the apparatus described in Section 11
( ⁄2 in.) below the upper surface of the solution in the bottle,
of Test Methods D 871 – 48, and in Section 10 of Specifications D 301 – 50, which
last appeared in the 1952 Annual Book of ASTM Standards, Part 4.
Annual Book of ASTM Standards, Vol 06.03.
4 5
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1343–95 (2000)
and the lower etched line of the viscometer is at least 12.7 mm 7. Procedure
( ⁄2 in.) above the bottom of the sample bottle. Suitable lighting
7.1 Preparation of Solution—Dry the sample and prepare a
is provided to enable the observer to sight across the parallel
solution as specified for the particular material. Such instruc-
etched lines, through the sample bottle and solution, avoiding
tions are given in the viscosity sections ofTest Methods D 301,
in this manner parallax errors. With this viscometer no timing
D 871, and D 817.Weigh into the bottle an appropriate amount
markers need to be provided on the bottles.
of dry sample and specified solvent, accurate to 0.1 g, to make
5.2 Bottles and Caps:
about 350 mLof solution.The accurate and precise make up of
5.2.1 Bottles, round or square, conforming to the dimen-
the solution is a necessity (example: 60.00 g of cellulose
sional requirements shown in Table 1, shall be used. Screw
acetate and 240.00 g solvent). Close the bottle tightly.Allow to
caps of metal or phenolic plastic in sizes to fit the bottles and
stand a short time for the solvent to penetrate the sample. Then
having aluminum foil or cardboard and cellophane liners may
tumble or shake until a uniform solution is obtained. For some
be used to close the bottles. Alternatively, rubber stoppers
samples this may require several days. Transfer to the water
covered with aluminum or tin foil, may also be used as
bath at 25 6 0.1°C, and allow the solution to come to
closures. In this latter case, solvent loss during measurement of
temperature. A practical method to determine possible solvent
viscosity can be minimized by removing the stopper, leaving
loss during this time involves weighing the bottle immediately
the foil in place, and making a small hole in the center of the
after adding the components, and again before performing the
foil through which the balls may be dropped.
ball drop.
5.2.2 Timing marks shall be provided around each bottle or
7.2 Viscosity Determination—Drop a 2.38-mm ( ⁄32-in.)
on the front and back of the glass-walled constant-temperature
stainless steel ball through the center of the column of solution
water bath, to avoid parallax errors. The lower timing mark
and time its fall through the marked 50.8-mm (2-in.) distance,
shall be at least 13 mm ( 0.5 in.) above the base of the bottle,
using a stop watch and taking precautions to avoid parallax
and the upper mark shall be 50.8 6 0.5 mm (2.00 6 0.02 in.
errors. If the observed time is less than 15 s or greater than 100
) above the lower mark.Apractical
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