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Designation: D1795 − 13

Standard Test Method for

Intrinsic Viscosity of Cellulose1
This standard is issued under the fixed designation D1795; 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.

1. Scope solution, and also that of the solvent, is determined at 25°C by

1.1 This test method covers the determination of the intrin- means of a calibrated glass capillary-type viscometer. The
sic viscosity of purified celluloses such as bleached wood relative viscosity is calculated and the corresponding intrinsic
pulps, cotton linters, and regenerated cellulose. It is applicable viscosity is read from a table.
to all cellulose samples with an intrinsic viscosity of 15 dl/g or
4. Significance and Use
less. Most native (unpurified) celluloses have intrinsic viscos-
ity values too high for measurement by this test method. 4.1 This test is a sensitive measure of the degradation of
cellulose resulting from the action of heat, light, acids, alkalies,
NOTE 1—The use of cuprammonium hydroxide solution for regular oxidizing and reducing agents, and the like, used in its
viscosity determination is described in Method T 206 m-55 of the
Technical Association of Pulp and Paper Industry on “Cuprammonium processing or purification. The intrinsic viscosity value may be
Disperse Viscosity of Pulp,” and Joint Army-Navy Specifications JAN- converted to degree of polymerization (DP) or to intrinsic
C-206. fluidity, if desired.
1.2 The values stated in SI units are to be regarded as 4.2 Solutions of cellulose are not Newtonian liquids; that is,

standard. iTeh Standards

standard. No other units of measurement are included in this their viscosity depends upon the rate-of-shear or velocity
gradient during measurement. This effect is smaller for samples

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1.3 This standard does not purport to address all of the of low molecular mass (DP) and at low concentrations than for
safety concerns, if any, associated with its use. It is the high-DP samples and at high concentrations. For the celluloses
responsibility of the user of this standard to establish appro- and concentrations included within the limits set forth in this
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priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
test method, the effect of rate-of-shear is assumed to be
negligible for referee purposes. For other conditions and for
research purposes this assumption may be invalid, but to
2. Referenced Documents discuss ways of accounting for this effect is beyond the scope
ASTM D1795-13
2.1 ASTM Standards:2 of the present test method.
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D445 Test Method for Kinematic Viscosity of Transparent
and Opaque Liquids (and Calculation of Dynamic Viscos- 5. Apparatus
ity) 5.1 Viscometer, Glass, Capillary Type—The Cannon-
D629 Test Methods for Quantitative Analysis of Textiles Fenske, Ubbelohde, or similar capillary type instrument as
E1 Specification for ASTM Liquid-in-Glass Thermometers described in Test Method D445 is recommended. In order to
E2251 Specification for Liquid-in-Glass ASTM Thermom- avoid correction for the kinetic energy effect, choose a viscom-
eters with Low-Hazard Precision Liquids eter with a small enough capillary to give an outflow time of 80
s or more for the Cannon-Fenske type. (A size 100 viscometer
3. Summary of Test Method is normally used for the sample solution and a size 50 for the
3.1 A weighed sample of the material is dissolved in a 0.5 M solvent.)
cupriethylenediamine hydroxide solution. The viscosity of this 5.2 Thermometer—ASTM Kinematic Viscosity Thermom-
eter for use at 25°C, having a range from 19 to 27°C and
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint conforming to the requirement for Thermometer 17C as
and Related Coatings, Materials, and Applications and is the direct responsibility of prescribed in Specification E1. Thermometric devices such as
Subcommittee D01.36 on Cellulose and Cellulose Derivatives. RTDs, thermistors and liquid-in-glass thermometers (as speci-
Current edition approved June 1, 2013. Published July 2013. Originally approved
fied in Specification E2251) of equal or better accuracy in the
in 1960. Last previous edition approved in 2007 as D1795 – 96 (2007)ε1. DOI:
10.1520/D1795-13. specified temperature range, may be used.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.3 Bath—A constant-temperature bath at 25°C suitable for
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 immersion of the viscometer so that the reservoir or the top of
the ASTM website. the capillary, whichever is uppermost, is immersed at least 50

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1
 D1795 − 13
mm, and with provision for visibility of the instrument and the 8. Calibration of Viscometer
thermometer. Firm supports for the viscometer shall be pro- 8.1 The following directions apply to the Cannon-Fenske
vided; or the viscometer may be sealed in as an integral part of viscometer (Note 3). They should be modified according to the
the bath. Either a liquid bath with thermostatic regulation and operating instructions for other types of viscometers. The
a stirrer or a vapor bath with pressure regulation is permissible. viscometers shall be calibrated (Note 4) by means of liquids
The efficiency of the stirring and the balance between heat having known viscosities approximately equal to those of the
losses and heat input must be such that the temperature of the solvent and cellulose solutions respectively (1.2 and 12 cP,
bath medium does not vary by more than 60.1°C over the approximately).
length of the viscometer, or from viscometer to viscometer in
the various bath positions. If a vapor bath is used, there must NOTE 3—Detailed specifications and directions for filling, calibrating,
be no temperature gradient over the length of the viscometer and measurement with types of capillary viscometers most used are given
in Test Method D445.
greater than that permitted in a liquid bath. NOTE 4—Calibration of the viscometers may be avoided if both solvent
5.4 Timer—A stop watch or other spring-activated timing and solution are measured in the same instrument. Then the relative
device or electrical timing device shall be used, graduated in viscosity is nearly the ratio of outflow times for solution and solvent,
respectively. This simplification involves two assumptions. The first, that
divisions of 0.2 s or less, and accurate to within 0.05 % when the densities of solution and solvent are equal, holds very well for the
tested over not less than a 10-min period. Such electrical dilute solutions used in these tests. The second, that the kinetic energy
timing devices shall be used only on electrical circuits of correction is zero, depends upon the choice of viscometer. If the one used
continuously controlled frequency. Frequency-controlled de- gives convenient outflow times for the solution of less than 150 s, then it
vices of suitable capacity for laboratory purposes, accurate to will be too fast for the solvent. The kinetic energy correction is zero,
depending upon flow. On the other hand, if one is chosen so that the
within 1 part in 10 000 should be used. Errors exceeding outflow time for the solvent is large enough (80 s or more), then the times
0.05 % of a 10-min interval may occur in timing devices for the solutions will in most cases be inconveniently long. For some
actuated by electrical synchronous motors driven by most work, however, it may be desirable to make some sacrifice in accuracy or
public power systems, which are intermittently and not con- in convenience during measurement in order to avoid calibration and
tinuously controlled. using two sizes of viscometers.
8.2 By means of a pipet, add 7.0 mL of the calibrating liquid
6. Reagent iTeh Standards
6.1 Cupriethylenediamine Hydroxide Solution (1.00 6 0.01
to the viscometer, in a constant-temperature bath at 25 6 0.1°C
(or fill as described in Test Method D445, Appendix A).

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M), in copper, with the molar ratio of ethylenediamine to 8.3 When the liquid has reached temperature equilibrium
copper of 2 6 0.1 to 1. This solvent may be prepared in the
with the bath (in about 5 min), determine the outflow time t by

7. Reference Materials
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laboratory. It is also commercially available.3 drawing the top meniscus of the liquid above the mark between
the two bulbs and measuring the time required for the meniscus
to pass from this mark to the mark below the lower bulb. Take
7.1 Viscosity Oil Standards—Calibrating oils in the speci- the average of two or more observations, which should differ
ASTM D1795-13
fied ranges of viscosity.3 Aqueous solutions of glycerol may be by not more than 0.2 s.
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used instead of standardized oils; the compositions for various 8.4 Determine the viscometer constant C by the equation:
viscosities are given in chemical handbooks. The applicable
C 5 η/dt (1)
viscosity oil standards (Note 2) are listed in Table 1.
where:
η = viscosity of the calibrating liquid, cP,
TABLE 1 Viscosity Oil Standards d = density, g/mL, and
Viscometer Viscosity Oil Standard t = time, s.
Approximate
Absolute Viscosity
Size Designation Absolute Viscosity
Range, cPA
at 25°C, cP
9. Preparation of Sample
50 0.9 to 3.5 S-3 3.3 9.1 To avoid undesirable effects from long heating at high
100 3.3 to 13.3 S-6 7.7
A
temperature, samples should be air-dried and the moisture
For solution with density of 0.9.
content determined on a portion that is not used for measure-
ment of viscosity. The mass of air-dried samples is then
corrected for moisture to obtain the mass of oven-dried
cellulose used to calculate concentration.
NOTE 2—The viscosity oil standards are available only as 4.7- m3 (1-pt)
samples. More than 1 pt of any given oil (for example, duplicate samples) 9.2 Soft, sheeted pulp should be picked apart with tweezers
are supplied only when it is established that 1 pt is inadequate.3 or scraped with a dull knife. Hard-pressed or harsh pulp should
be slurried in water, formed into thin sheets on a Büchner
funnel, and dried at a temperature below 100°C (preferably
3
The sole source of supply of the viscosity oil standards known to the committee room temperature). Loose pulp should be picked apart by hand
at this time is Cannon Instrument Co., P. O. Box 16, State College, PA 16801. If you
to break up any lumps. Slurried or slush pulps should be
are aware of alternative suppliers, please provide this information to ASTM
International Headquarters. Your comments will receive careful consideration at a formed into thin sheets and dried. Yarn and staple should be
meeting of the responsible technical committee,1 which you may attend. washed in warm water containing a little detergent to remove

2
 D1795 − 13
the finish, rinsed thoroughly, dried (at low temperature), and screw cap. Add 25.0 mL of distilled water from a pipet or buret,
fluffed. (It will be found helpful to cut yarn and long staple into insert the stopper or cap, and shake in order to wet out and
short lengths, say 13 mm (1⁄2 in.), before washing.) Fabrics disperse the sample. Sweep the air from the vessel with a
should be cut into small pieces, desized (see Test Methods stream of nitrogen and, with the nitrogen still flowing, add 25.0
D629), thoroughly washed, and dried. Raveling will be helpful mL of solvent. Stopper or cap tightly and shake vigorously by
before dissolving samples that tend to get in the solvent. hand or in a mechanical shaker until the cellulose is completely
Materials containing a considerable amount of non-cellulosic dissolved.
matter must first be purified; such treatments lie outside the NOTE 5—Most work pulp and regenerated celluloses dissolve within 5
scope of this test method. min. Mercerized celluloses do not dissolve as easily in cupriethylenedi-
amine as in cuprammonium solvent and require longer times (up to 1 h).
10. Preparation of Solution Some operators report difficulty in dissolving native celluloses including
10.1 The sample size is dependent upon the nature of the cotton linters with degree of polymerization (DP) as low as that of wood
pulps. The difficulty shows up by much poorer precision of results than the
material, smaller masses of high-viscosity celluloses and larger 1 to 2 % that is normally obtained between measurements made with two
masses of low-viscosity celluloses being used in order to keep or more solutions of the same sample. Even solutions that leave no residue
the viscosity of the solutions within rather narrow limits. on fritted-glass filters have been observed to give erratic results. Inad-
(Working at nearly constant viscosity reduces the effect of rate equate dispersion of the sample is apparently the cause, and two
modifications in procedure have been recommended in such cases. One is
of shear upon the measurements.) The concentration for each to add about 0.04 % wetting agent to the water used to wet out the
sample is chosen according to the rule: sample.4 The other requires use of cupriethylenediamine solutions of two
@ η # c 5 3.0960.5 (2) concentrations: The sample is wetted out with one solution that is 0.167 M
in copper and dispersion is completed by adding the second solution,
where: 1.000 M in copper, in such volume as to make the final copper
concentration 0.500 M.
[η] = intrinsic viscosity, dL/g, and
c = cellulose concentration, g/dL. 11. Measurement of Viscosity
Obviously, use of this rule requires knowledge of the 11.1 Transfer 7.0 mL of the solution by means of a syringe
approximate intrinsic viscosity of the sample before the con-
iTeh Standards
centration can be estimated. In routine control work, such
information is available. If it is not, Table 2 will serve as an
or pipet to a viscometer previously placed in the bath at 25°C
and flushed with nitrogen (or fill as described in Test Method
D445, Appendix A). Allow at least 5 min for the solution to
approximate guide.
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10.2 Make up a preliminary solution of about the indicated
reach bath temperature.
11.2 By applying either pressure (with nitrogen) or suction,
Sections 11 and 12. From the relativeDocument
viscosity thus obtained, Preview
concentration, and determine the viscosity as described in draw the solution into the lower bulb of the viscometer until the
top meniscus is a little above the mark between the two bulbs.
find the approximate value of the intrinsic viscosity by means Measure the time t required for the meniscus to pass from this
of Table 3. From this determine the concentration needed to
ASTM
give: [η]c = 3.0. If this preliminary solution does not give a D1795-13
mark to the mark below the lower bulb. Repeat at least twice
and average the observations, which should not differ by more
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value of [η]c of 3.0 6 0.5, prepare a second solution of the than 0.3 %.
indicated concentration for the final viscosity measurement.
11.3 In the same way, measure the outflow time t0 for the
10.3 Alkaline solutions of cellulose are known to be sensi- solvent. This of course must be determined not for the 1.00 M
tive to oxidation. Hence it is usually necessary to exclude air solvent as prepared or purchased, but for this solvent diluted
during solution of the sample; several ways of doing this are with an equal volume of water.
described in the literature, but the following is simple and
adequate: Weigh out the calculated amount of air-dried cellu- 12. Calculations
lose (corrected to oven-dry mass) and transfer quantitatively to
12.1 Calculate the viscosity, η, in centipoises, as follows:
a suitable glass or polyethylene container (capacity somewhat
more than 50 mL) that can be tightly closed by a stopper or η 5 Ctd (3)

where:
TABLE 2 Intrinsic Viscosities of Typical Samples C = viscometer constant (Section 8),
Intrinsic Approximate t = outflow time, s, and
Type of Material Viscosity, Concentration, d = density, g/mL.
dL/g g/dL
Calculate the relative viscosity, ηrel, as follows:
Regenerated cellulose (rayons) 2 to 3 1
Dissolving pulps: η rel 5 η/η 0
Low viscosity 3 to 4 1
Regular viscosity 4 to 7 0.5 where η0 is the viscosity of the solvent. Since the densities of
High viscosity 7 to 10 0.3
Cotton linters, for rayon and acetate 6 to 9 0.4 solvent and solution are practically the same, they cancel in
Paper (wood) pulps 3 to 8 0.4 determining relative viscosity. Hence a little work may be
Native cellulosesA 15 to 30 0.1 to 0.2
A
Serious error may be introduced when this test method, which neglects effects of
4
rate of shear upon viscosity, is used for native celluloses of high intrinsic viscosity. Lindsley, C. H., “Rapid Dispersion of Cellulose in Cupriethylenediamine,”
Textile Research Journal, Vol 21, 1951, p. 286.