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Tentative Methods of Test for

AMOUNT OF MOISTURE IN TEXTILE MATERIALS'

ASTM Designation: D 2654 - 67 T

These Tentative Methods have been approved by the sponsoring commit-
tee and accepted by the Society in accordance with established procedures,
for use pending adoption as standard. Suggestions for revisions should
be addressed to the Society at 1916 Race St., Philadelphia, Pa. 19103.

1. Scope tile matter is present on or in the ma-

1.1 These methods cover the deter- terial to be tested.
mination of the moisture content in tex- 1.1.3 Option 3—Distillation with tol-
tile materials. These methods are applica- uene is the preferred method for jute and
ble to all fibers, natural and man-made, grease wool in any circumstance, and is
and in all forms from bulk fiber or fila- the preferred method for any material
ments to finished fabrics, subject to the where it is known or suspected that a
limitations set forth in 1.1.1 through significant quantity of nonaqueous and
1.1.3. non-water-miscible volatile matter is
1.1.1 Option 1—Oven-drying using present. It also has the best reproducibil-
ambient air heated to 105 C may be used ity of the three options and, therefore,
in any situation in which a simple and may be preferred in case of dispute.
convenient method for routine process 1.2 Blends of fibers may also be tested
control or in-plant evaluation is needed. by these methods.
It is not recommended for jute or grease 1.3 Options 1 and2 describe alternative
wool, or for acceptance testing in com- procedures for weighing the dried speci-
mercial transactions. mens; a procedure for weighing the
1.1.2 Option 2—Oven-drying using specimens in the oven while hot, and a
desiccated air heated to 105 C and other procedure for sealing the specimens in a
refinements in technique may be used as moisture-tight weighing container and
a basis for commercial transactions for cooling it in a desiccator before weighing
all materials for which it is known that no il at room temperature.
significant quantity of nonaqueous vola- NOTE 1—Other methods for determining the
1
Under the standardization procedure of the amount of moisture in textile materials are
Society, these methods are under the jurisdic- covered in ASTM Method D 2495, Moisture in
tion of the ASTM Committee D-13 on Textile Cotton (Oven-Drying Method),'ASTM Method
Materials, and are the direct responsibility of D 1576, Moisture in Wool by Oven-Drying,2
Subcommittee B-3 on Atmospheric Conditions ASTM Method D 2462, Moisture in Wool by
and Regains. A list of committee members may
be found in the ASTM Year Book.
Accepted June 26, 1907. lOd'J Book of ASTM Standards, Part 25.
590
 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654) 591

Distillation with Toluene,2 and ASTM Method weight. The value of a particular com-
D 681, Methods of Test for Jute Rove and modity will vary over a significant range
Plied Yarn for Electrical and Packing Purposes.2
with a variation in the amount of water
2. Definitions it contains.
2.1 Moisture Content, n.—The amount 4.1.2 Besides the effect of the moisture
of moisture in a material determined un- present when the material is received,
der prescribed conditions and expressed the moisture present at the time of test-
as a percentage of the mass of the moist ing and subsequent handling and proc-
material, that is, the original mass com- essing can be quite important.
prising the dry substance plus any mois- 4.1.2.1 Some textile fibers, particu-
ture present. larly cellulosic fibers and wool, have
2.2 Moisture Regain, n.—The amount physical properties that vary signifi-
of moisture in a material determined un- cantly with the amount of moisture pres-
der prescribed conditions and expressed ent, such as tensile strength, crimp,
as a percentage of the moisture-free ma- torsional rigidity, etc.
terial. 4.1.2.2 Optimum conditions for proc-
2.3 Moisture-Free, adj.—The condi- esses, such as in carding, include mois-
tion of a material that has been exposed ture content as an important parameter.
in an atmosphere of desiccated air until 4.1.2.3 Control of blends is sometimes
there is no progressive significant change critically dependent on the moisture con-
in its mass. tent of the components.
4.1.2.4 Control of the mass per unit
NOTE 2—The term "mass" in the above area of fabric and the linear density of
definitions is the correct designation for the yarn depends on control of moisture
property commonly designated as "weight."
content.
2.4 For definitions of other terms used 4.1.2.5 Quantitative analyses of fiber
in this method, refer to ASTM Defini- mixtures require information on moisture
tions 1) 123, Terms Relating to Textile present.
Materials.23 4.2 In these methods, three options
are given, the choice depending primarily
3. Summary of Methods on the degree of accuracy required in the
3.1 These methods include two options result. Oven-drying methods have the
based on drying in an oven, and one op- virtue of simplicity and economy, but are
tion based on distillation with an immis- subject to interferences. For example,
cible solvent. More detailed summaries when ambient air is passed through the
can be found in 5.1, 13.1, and 21.1. oven and heated to 105 C, a slight
amount of residual moisture may be re-
4. Uses and Significance tained because of the relative humidity
4.1 The measurement of moisture con- of the ambient air. When the standard
tent or of dry liber weight (Note 2) is atmosphere for testing textiles is heated
important for several reasons, including to 105 C its relative humidity is 1.25 per
the following: cent. Under these conditions, the weight
4.1.1 Large quantities of fibers and (Note 2) of any oven-dry material is
manufactured products containing some greater than its weight when moisture-
water are bought and sold on the basis of free. If the relative humidity of the am-
bient air is known, the amount of
Appears in this publication. moisture retained by a specimen may be
592 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654)

estimated from published data.4 This necessary because a specimen cannot be

interference may be circumvented by loaded into the flask without considerable
utilizing desiccated air as specified by the exposure, with possible change in the
second option included in this method. moisture present.
However, when using either of the oven-
drying options, there may be an addi- OPTION 1—DRYING IN AN OVEN
tional loss in weight, other than water, SUPPLIED WITH AMBIENT AIR
caused by the evaporation of volatile 5. Summary
matter, the amount depending on the
5.1 A sample of the material to be
characteristics and amount of any added
tested is exposed to a stream of air,
oils or emulsions. The third option, dis-
heated to 105 C, until no further loss of
tillation with toluene, is free of both of
mass occurs. The total mass lost in this
these types of interference, but should be
process is assumed to be moisture and is
used with caution if it is suspected that
expressed either as moisture content or
any steam-distillable, water soluble sub-
moisture regain (see 2.1 and 2.2).
stances such as glycols, are present. Dis-
tillation with toluene is known to be a 6. Apparatus
satisfactory method for jute where a de-
composition problem exists when jute is 6.1 Oven, ventilated and thermo-
exposed to air heated to 105 C and may statically controlled in the temperature
also be satisfactory for any other bast range of 105 ± 2 C throughout the en-
fibers where a similar problem exists. closure. The oven may be either the
4.3 It is sometimes possible, when forced draft or convection type.
sampling material for moisture measure- 6.2 Weighing Containers, to be used if
ment, to select sampling units of a size the specimens are to be weighed in the
which coincide with the size required by oven. These may be perforated metal
the testing method for a specimen. In baskets or shallow pans, of a size to fit
these instances, the weight (Note 2) may the particular oven in which they are
be determined immediately, and, if the used. For specimens containing particles
weight of the oven-dry material is to be of foreign matter that are easily shaken
determined, no intermediate steps are out, use baskets made of or lined with
necessary. However, in other instances, wire screening fine enough to hold the
it may be necessary or desirable to per- trash.
form some intermediate manipulation 6.3 Weighing Containers, capable of
with the material, such as compositing or being sealed (such as glass weighing bot-
sub-sampling. For such instances, in or- tles) if the specimen is to be cooled in a
der to circumvent the problem of desiccator before weighing in the ambient
moisture loss or gain after sampling, atmosphere.
provisions are made in these methods to 6.4 Weighing Containers, to be used
stabilize the material in the working at- when specimens are to be weighed outside
mosphere, and equations are provided the oven, after cooling in a desiccator.
with correction terms to relate the meas- These may be glass weighing bottles or
ured moisture content or regain to the other containers that can be sealed to
amount which existed at the time when prevent loss of moisture.
the sample was taken. When the toluene 6.5 Desiccator, large enough to hold
distillation option is used, stabilization is one or more weighing containers (for an
alternative in which the specimens are
* Toner, R. K., Bower, C. F., and Whitwell, weighed outside the oven).
J. C, Textile Research Journal, Vol. 17, No. 1,
Jan. 1947, p. 7. 6.6 Desiccant—Any suitable non-caus-
 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654) 593

tic desiccant may be used provided it is specimen, at which at least 98 per cent
dried or replaced as required for effective of the weight loss ultimately achieved has
desiccation. Anhydrous calcium sulfate is occurred. This will be the normal cycle
recommended for this material in this equipment.
6.7 Sampling Containers, capable of Twenty per cent of this cycle will be the
being sealed. Mason jars have been found time interval used for additional drying
to be satisfactory where the sample size between successive weighings.
is not too large. For larger samples, bags 9.1.2 To save the time required to re-
of various plastic materials may be suita- weigh the empty containers or baskets
ble if the wall thickness is sufficient to after each use, adjust them to equal
provide a good moisture barrier (at least weight within ±0.005 g by grinding or
4 mils (approximately 0.1 mm) for poly- filing. Identify them by numbers and
ethylene, for example). record their weights. The containers must
6.8 Balance, having a capacity ade- be kept clean and their weights checked
quate for weighing specimens and con- regularly.
tainers and a sensitivity of 0.005 g. The 9.2 Open the sample container and
balance may be an integral part of the quickly weigh out a specimen of the re-
drying oven. quired size, if specimen-sized portions
7. Sampling were not obtained at the time of sam-
pling. If the specimen is adjusted to the
7.1 Sampling should be engineered to specified weight (Note 2) ±0.005 g in not
accomplish the purpose for which the more than 30 sec after the container is
test is being made, taking due account of opened, and the material is not more than
the precision required and the variability 2 percentage points in moisture content
of the material being sampled. away from the equilibrium value it would
8. Conditioning attain in the atmosphere in which the
weighing is done, no appreciable error is
8.1 For Option 1, specimens must not introduced. If these conditions cannot be
be either conditioned or preconditioned. met, and the resulting error is not tolera-
9. Procedure ble, use the stabilizing procedure de-
scribed in Option 2.
9.1 Preliminary Set-Up:
9.1.1 Different materials may have 9.3 Procedure Using an Oven Balance:
different drying curves depending on the 9.3.1 Place the specimen in a basket
degree of exposure of all parts of a speci- in the oven and dry at 105 ± 2 C until
men to the drying atmosphere and the the change in weight (Note 2) between
level of moisture present in the material. successive weighings is less than 0.1 per-
Using relatively moist material, make centage points when spacing the succes-
several preliminary runs, measuring the sive weighings according to the instruc-
weight (Note 2) lost versus the time of tions given in 9.1.1. Turn off the air
drying so that a weight-time curve can current in a forced draft type oven before
be plotted. If weighings are performed making a weighing and block off natural
outside the oven after cooling the speci- air currents present.
mens, use longer time intervals than 9.3.2 Weigh the specimen and basket
would be required if the specimens were to the nearest 0.05 g.
being weighed hot in the oven. Use un- 9.4 Procedure Using an Outside Bal-
equal intervals of drying time to avoid ance:
achieving a false equilibrium. Plot the 9.4.1 Place the specimen and container
curves and find the time, for the slowest in the oven, uncover the container, and
594 TESTS FOE AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654)

dry at 105 ± 2 C. If a glass weighing the original weight of the specimen by

bottle is used, heat the stopper in the Eq 1 as follows:
oven along with the bottle, otherwise,
W„^W„-Wt (1)
contraction of the bottle upon cooling
may make the stopper too tight to open where:
or may break the bottle. Dry until the W0 = weight of specimen as received,
change in weight (Note 2) between suc- Wg = gross weight of specimen and con-
cessive weights is less than 0.1 percentage tainer, and
points when spacing the successive weigh- Wi = weight of empty container.
ings according to the directions given in 10.1.2 If the specimen was adjusted to
9.1.1. a specified weight in the laboratory, then
9.4.2 In executing the weighings, close W0 is the weight thus obtained.
the weighing can or weighing bottle while 10.2 Calculate the weight of the oven-
it is still in the oven. Transfer the closed dry specimen by Eq 2 as follows:
container to a desiccator and cover the
Wd = wh -W.. .(2)
desiccator. While the specimen and con-
tainer are cooling, uncover the desiccator where:
two or three times, raise the cover of the Wd = weight of oven-dry specimen,
weighing container slightly for a fraction W0 = weight of specimen in basket or
of a second to equalize the air pressure, weighing bottle, and
and replace the cover on the desiccator Wc = weight of empty weighing con-
(see Note 3). When the container and tainer.
specimen have cooled to room tempera- 10.3 Calculate the moisture content
ture, weigh them to the nearest 0.005 g. by Eq 3 as follows:
Return the container and specimen to the
oven. Uncover and repeat the drying, Moisture content, per cent
cooling, and weighing at the intervals re- = W„ - Wd
quired by the directions given in 9.1.1, X 100. (3)
W0
until the change in weight between two
successive weighings is less than 0.1 per- 10.4 Calculate the moisture regain by
centage points. Record the final weight Eq 4 as follows:
and the weight of the empty container.
Moisture regain, per cent
NOTE 3—Opening the container is necessary
only when using weighing bottles with ground- W0 - Wj
X 100. (4)
glass stoppers, or other airtight containers. If it Wd
is not done, the partial vacuum created inside
the bottle may make it impossible to open the 10.5 Calculate the moisture content or
bottle without breakage. A vacuum also im- moisture regain of each specimen to the
parts buoyancy to the container and decreases
the apparent weight. With weighing cans that nearest 0.01 percentage points. When the
are not completely sealed by their lids, the air mean value of several specimens is calcu-
of the desiccator is able to leak in and equalize lated, compute also the standard error of
the pressure. the mean. Since the true mean is quite
likely to lie anywhere within the range of
10. Calculations
values bounded by the mean ± one
10.1 Determine the original weight standard error, the size of this range
(Note 2) of the specimen. determines the decimal position at which
10.1.1 If the specimen was weighed as variations begin to occur. Carry only one
received in the sealed container, calculate doubtful digit in stating the mean.
 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654) 595

Example 1—The following set of meas- centage points squared calculated on the
urements, 7.7, 8.1, 8.3, 8.1, 8.6, has a basis of moisture content, and
mean of 8.16 and a standard error of the 12.1.2 Between-laboratory, 0.20 per-
mean of 0.148. The set of values included centage points squared calculated on the
by ± one standard error is bounded by basis of moisture content.
8.012 and 8.308. The first place after the As a consequence, the within-labora-
decimal point is therefore uncertain, and tory precision at a probability of 0.95 is
the mean should be reported as 8.2. (See expected to be ±0.39 percentage points
ASTM Recommended Practice E 29, for a single determination and ±0.28
Indicating Which Places of Figures Are percentage points for the average of two
to Be Considered Significant in Speci- determinations. If each of two labora-
fied Limiting Values,6 for a discussion of tories measures two specimens of a uni-
rounding-off procedures.) form material, the results should be ex-
Example 2—The following set of meas- pected to agree, at a probability level of
urements, 6.1, 12.7, 11.3, 7.6, 9.5, has a 0.95 to within ±1.30 percentage points.
mean of 9.44 and a standard error of the 12.2 The measurements for this inter-
mean of 1.19. The set of values included laboratory test were performed by lab-
by the mean ± one standard error is oratories having better than average skill
bounded by 8.25 and 10.63. The first and extensive experience. The predictions
place before the decimal is therefore un- made above, therefore, may prove to be
certain and the mean should be reported optimistic and should be used with cau-
as 9. tion.
11. Report OPTION 2—DRYING IN AN OVEN
11.1 State that the tests were made as SUPPLIED WITH DESICCATED
directed in ASTM Method D 2654, Op- AIR
tion 1, and report the following informa-
tion: 13. Summary
11.1.1 The average moisture content 13.1 A sample of the material to be
or moisture regain to the number of tested is exposed to a stream of air which
decimal places determined as described has been dried so as to contain not more
in 10.5. than 0.01 g of water per 1000 liters and
11.1.2 Sample identification, kind of heated to 105 C until no further loss in
material, and the conditions under which weight (Note 2) occurs. The total weight
the specimens were taken. lost in this process is assumed to be mois-
11.1.3 Whether the test was made us- ture and is expressed as either moisture
ing an oven balance or an outside bal- content or moisture regain (see 2.1
ance. and 2.2).
12. Precision and Accuracy 14. Apparatus
12.1 From an interlaboratory test con- 14.1 Ventilated Drying Oven, main-
ducted in 1963 in which four laboratories tained at a temperature of 105 ± 2 C
measured twelve specimens, each of a throughout the enclosure. The specimen
nominally uniform material, the follow- shall not be subject to direct radiation
ing components of variance were esti- from the heating elements. The oven shall
mated : be supplied with a current of air at a rate
12.1.1 Within-laboratory, 0.04 per- sufficient to change the air in the en-
6
1969 Book of ASTM Standards, Part 30. closure at least once every 4 min. The
62-4
596 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654)

current of air shall be pre-dried (less than quate for weighing specimens and con-
0.01 g of water per 1000 liters) by circu- tainers, and a sensitivity of 0.005 g. The
lating through dehydrating units. The balance may be an integral part of the
air shall pass freely through the speci- drying oven.
mens. The oven may be combined with a
balance in which case facilities should be 15. Sampling, Selection and Number of
provided for shutting off the flow of air Specimens
during the weighing. 15.1 Take a lot sample as directed in
14.2 Weighing Containers, to be used the applicable material specification, or
if the specimens are weighed in the oven. as agreed upon by the parties interested
These may be perforated metal baskets in the test results. In the absence of any
or shallow pans, of a size to fit the partic- specification, take a lot sample as di-
ular oven in which they are used. For rected in ASTM Method D 2525, Devis-
specimens containing particles of foreign ing a Sampling Plan for Various Forms of
matter that are easily shaken out, use Wool for the Determination of Moisture
baskets made of or lined with wire screen- Content;2 ASTM Method D 1441, Sam-
ing fine enough to hold the trash. pling Cotton Fibers for Testing2; or
14.3 Weighing Containers, capable of ASTM Method D 2258, Sampling Yarn
being sealed (such as glass weighing bot- for Testing.8
tles) if the specimen is to be cooled in a 15.2 Use extreme care to prevent gain
desiccator before weighing in the am- or loss of moisture during the sampling
bient atmosphere. operation and in the transfer of material
14.4 Weighing Containers, to be used to the sampling container. Weigh each
when specimens are to be weighed out- portion of the sample and its container
side the oven, after cooling in a desiccator. immediately after sampling. Subtract the
These may be glass weighing bottles or tare weight of the container to obtain the
other containers that can be sealed to net weight at time of sampling, W0.
prevent loss of moisture. 15.3 When it is possible to select a
14.5 Desiccators, large enough to hold sampling unit of a size suitable for use as
as many weighing containers as will be a specimen, proceed directly to 17. Pro-
used at one time (for the alternative in cedure, otherwise proceed as directed in
which the specimens are weighed outside Method D 25252 for the reduction of the
the oven). lot sample to a laboratory sample or sam-
14.6 Desiccant—Any suitable non- ples, and the selection of specimens. Note
caustic desiccant may be used provided that for Option 2, the instructions given
it is re-dried or replaced as required for in 16. Conditioning, are to be applied to
effective desiccation. Anhydrous calcium the sample before the specimens are se-
sulfate is recommended. lected. The size of the specimen required
14.7 Sampling Containers, capable of is determined by the particular oven-dry-
being sealed. Mason jars have been found ing equipment used.
to be satisfactory where the sample size 15.4 Take a minimum of two speci-
is not too large. For larger samples, bags mens per laboratory sample.
of various plastic materials may be suita-
ble if the wall thickness is sufficient to 16. Conditioning
provide a good moisture barrier (at least 16.1 Condition the previously weighed
4 mils (approximately 0.1 mm) for poly- lot sample (or laboratory sample(s)) by
ethylene, for example). exposure to moving air in the laboratory
14.8 Balance, having a capacity ade- atmosphere in which sampling and
62-5
 TESTS FOR AMOUNT OI MOISTURE IN TEXTILE MATERIALS (D 2654) 597

weighing are to be done until moisture covered container in a desiccator, loosen

equilibrium for testing is achieved. the cover, and cool the specimen and con-
NOTE 4—Preconditioning is not required.
tainer to approximately room tempera-
Conditioning at 65 per cent relative humidity ture. When cooling is completed, set the
as directed in ASTM Method D 1776," Condi- cover firmly on the container, remove
tioning Textiles and Textile Products for Test- from the desiccator, and weigh. Replace
ing, is acceptable and may be done if desired. the specimen and container in the oven
An atmosphere of 65 per cent relative humidity
is not, however, necessary, since the object of and dry for an additional 20 per cent of
the conditioning for the purpose of this test is the normal cyle (see 9.1.1). Repeat the
merely to stabilize the sample in order that drying, cooling, and weighing until con-
changes in moisture will not occur while the stant weight is attained (Note 3).
specimens are being prepared and weighed.

16.2 Weigh the conditioned sample(s) 18. Calculation of Results

to the nearest 0.005 g and record the net 18.1 If the specimens were dried di-
weight(s), W (Note 2). rectly from the as-sampled condition,
NOTE 5—The weight, W, and the net weight
calculate the moisture content or mois-
at time of sampling, Wo , will be used to convert ture regain of each specimen to the near-
the observed moisture present in the conditioned est 0.01 per cent by Eq 5 or 6 as follows:
specimen to the moisture present at time of
sampling. Moisture content, per cent,

17. Procedure W„ - Wd
X 100.. (5)
W.
17.1 Place the specimen(s) in the oven
in a suitable container (see Note 6) and Moisture regain, per cent,
dry to constant weight (Note 2), defined
W. - Wd
as a lack of any progressive decrease in X 100. (6)
weight in excess of 0.1 percentage points
as determined by three successive weigh- where:
ings using the procedure in either 17.1.1 W0 = weight (Note 2) of specimen as
or 17.1.2. received, and
NOTE 6—Whether or not the specimen is Wd — oven-dry weight of specimen.
held by a container during the drying process, 18.2 If stabilizing and sub-sampling
all parts of the specimen must be exposed to have been done, calculate the moisture
freely moving air.
content or moisture regain of each speci-
17.1.1 If the weighings of the dried men to the nearest 0.01 per cent by Eq 7
specimen are to be performed with the or 8 as follows:
specimen inside the oven, perform the
Moisture content, per cent,
weighings with any forced-air circulation
turned off and any natural draft blocked.
X 100. (7)
For time of drying intervals see 9.1.1. \ W„wJ
17.1.2 If the weighings of the dried
specimen are to be performed outside the Moisture regain, per
>er cent,
oven, provide the specimen with an air-
tight container having a tight-fitting
cover. At the end of the drying period,
-(SSHX'"•• »
place the specimen in its container (which where:
is also in the oven), cover the container, W0 — net weight (Note 2) of laboralor,
and remove it from the oven. Place the sample at time of sampling,
42-5
598 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654)

W = net weight of laboratory sample outside the oven, calculated on the basis
at time of measurement, of moisture content.
W\ = net weight of specimen before 20.1.3 Between-laboratories, 0.103
drying, and percentage points squared when weighed
Wt = net weight of the oven-dry speci- in the oven, calculated on the basis of
men. moisture content.
18.3 When the mean value of several 20.2 As a consequence, the within-
specimens is calculated, compute also the laboratory precision at a probability of
standard error of the mean. Since the 0.95 is expected to be ±0.44 percentage
true mean is quite likely to lie anywhere points if weighed in the oven; ±0.25 per-
within the range of values bounded by centage points if weighed outside the
the mean ± one standard error, the size oven. The average of two determinations
of this range determines the decimal made in the same laboratory is expected
position at which variations begin to oc- to have a precision of ±0.31 percentage
cur. Carry only one doubtful figure in points if weighed in the oven, ±0.18 per-
stating the mean (see Examples 1 and 2 centage points if weighed outside the
under 10.5). oven, at a probability of 0.95.
If each of two laboratories measures
19. Report two specimens of a uniform material, at
19.1 State that the tests were made as a probability level of 0.95, the averages
directed in ASTM Method D 2654, Op- may be expected to agree to within
tion 2, and report the following informa- ±0.99 percentage points squared.
tion: 20.3 The measurements for this inter-
19.1.1 The average (arithmetic mean) laboratory test were performed by lab-
value of the results calculated for a par- oratories having better than average skill
ticular lot, stating whether it is a mois- and extensive experience. The prediction
ture content or moisture regain value. made above, therefore, may prove to be
19.1.2 The number of specimens optimistic, and should be used with
tested. caution.
19.1.3 The range of the calculated
OPTION 3—DISTILLATION WITH TOLUENE
moisture results (difference between the
largest and smallest calculated result). 21. Summary
20. Precision 21.1 A sample of (he material to be
tested is immersed in water-saturated
20.1 From an interlaboratory test
toluene, which is heated. The distilled
conducted in 1964 in which each of four
water vapor and solvent vapor condensed
laboratories measured six specimens of
are collected in a graduated trap, wherein
each of five materials: a polyester, a
the water separates from the toluene
polyamide, cotton, viscose, and wool,
and settles to the bottom. The volume ot
each test material being specially pre-
the water collected in the trap is con-
pared to be as uniform as possible, the
verted to its equivalent weight (Note 2).
following components of variance were
This weight is expressed as moisture
estimated.
content or moisture regain (see 2.1 and
20.1.1 Within-laboratories, 0.05 per-
2.2).
centage points squared when weighed in
the oven, calculated on the basis of 22. Apparatus
moisture content. 22.1 Erlenmeyer Flask? wide-mouth,
20.1.2 Within-laboratories, 0.017 per-
Corning No. 5100 or equivalent has been
centage points squared when weighed found satisfactory for this purpose.
62-S
 TESTS FOR AMOUNT or MOISTURE IN TEXTILE MATERIALS (D 2654) 599

1000-ml capacity (takes a No. 11 stop- Reflux for 1 hr or until the water no
per). longer accumulates in the trap. Assume
22.2 Distilling Receiver,'' Dean and the toluene in the flask to be water-
Stark, 10-ml capacity, graduated in 0.1 saturated and store in glass-stoppered
bottles until used. Prepare only as much
water-saturated toluene at one time as
NOTE 7—Illustrations of acceptable forms of
the glass apparatus required by this method
will be needed for the samples already
appear in ASTM Specifications E 123, for Ap- submitted.
paratus for Determination of Water by Distilla- 23.2 Potassium Dichromate Cleaning
tion.6 Solution—Prepare this solution by mix-
ing 35 ml of a saturated (at room tem-
22.3 Condenser, Liebig, sealed, with
perature) solution of potassium di-
500-mm jacket.
chromate with 1 liter of concentrated
22.4 Balance, capacity of at least 500
sulfuric acid.
g with a sensitivity of 0.05 g.
22.5 Healer, for distillation apparatus, 24. Safety Precautions
electrical with variable heat control and
arranged so that the surface of the flask 24.1 Toluene is flammable and slightly
above the lowest solution level is not toxic. It should be used in a well-venti-
heated by direct radiation. lated area, for example, under a hood,
22.6 Water Bath, with thermostatic to prevent accumulation of vapors.
controls, maintained at a temperature of 25. Sampling, Selection, and Number of
23 ± 1 C. Specimens
22.7 Sample Containers, capable of
being sealed. Mason jars have been found 25.1 Take a lot sample as directed in
to be satisfactory where the sample size the applicable material specification, or
is not too large (up to 200 g). For larger as agreed upon by the parties interested
samples, bags of various plastic materials in the test results. In the absence of any
are suitable if the wall thickness is suffi- specification, take a lot sample as di-
cient to provide a good moisture barrier. rected in Method D 2525,2 Method D
For example, for polyethylene, a wall 1441,2 or ASTM Method D 2258.3
thickness of at least 4 mils (approxi- 25.2 Use extreme care to prevent gain
mately 0.1 mm) has been found to be or loss of moisture during the sampling
satisfactory. operation and in the transfer of material
to the sampling container. Weigh each
23. Reagents portion of the sample and its container
23.1 Toluene, purified, water-satu- immediately after sampling. Subtract
rated, having a boiling range such that the tare weight (Note 2) of the con-
the solvent distills completely within a tainer to obtain the net weight at time
range of 2 C including 110.6 C. Prepare of sampling, Wo.
a solution of water-saturated toluene as 25.3 Follow the directions given in
follows: To each liter of toluene, add 50 Method D 2525 for the reduction of the
to 100 ml of distilled water. Shake for lot sample to a laboratory sample or
about 5 min and allow to settle. Decant samples and the selection of specimens.
the toluene to a flask and attach a reflux Note that for this method, the instruc-
condenser with a calibrated water trap. tions in 26. Conditioning, are to be
applied to the sample before the speci-
Corning No. 3600 or equivalent has been mens are selected. Take specimens that
found satisfactory for this purpose. weigh at least 50 g but not over 70 g.
62-5
600 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654)

25.4 Take a minimum of two speci- and add 700 ml of the water-saturated
mens per laboratory sample. toluene. When the flask with the speci-
men and the one used as a control are
26. Conditioning prepared, connect the flasks, receivers,
26.1 Condition the lot sample (or lab- and condensers and place the flasks on
oratory sample) by exposure to moving electric heaters. Start the tap water
air in the laboratory atmosphere in which flowing through the condensers. Add
the sub-sampling and weighing are to be additional water-saturated toluene
done until moisture equilibrium for test- through the tops of the condensers
ing is achieved (see Note 4). until the receiver traps are full of toluene
26.2 Weigh the conditioned sample to and it begins to run over into the flasks.
the nearest 0.05 g and record the net 27.5 Heat the toluene to the boiling
weight W (see Note 2). This weight and point and adjust the rate of distillation
the net weight at time of sampling, W<>, to 2 drops/sec.
will be used to convert the observed 27.6 When the water is accumulating
moisture present in the conditioned speci- at a rate of less than 0.1 ml/15 min,
men to the moisture present at time of increase the distilling rate to about 4
sampling. drops/sec. Wash down the condensers by
pouring water-saturated toluene in the
27. Procedure tops of the condensers. Brush the con-
27.1 Prior to using the equipment for densers down with a nylon brush satu-
this test, clean the receiver and con- rated with toluene, or dislodge any
denser with potassium dichromate clean- visible drops of water with a copper wire.
ing solution, rinse thoroughly with tap 27.7 Continue the distillation until no
water, then with methyl alcohol, and dry. change is observed in the location of the
meniscus over a 15 min-period.
NOTE 8—This cleaning operation is not 27.8 Separate the receivers containing
needed between successive determinations in the water and toluene from the flasks and
same equipment.
condensers. Place the receivers and their
27.2 Set up, as a control, a flask con- contents in the water bath which is
taining no specimen but containing 700 maintained at 23 ± 1 C. After approxi-
ml of the water-saturated toluene to mately 30 min, read the volume of water
which 5.0 ml of tap water have been in the trap, V, to the nearest 0.05 ml.
added using a volumetric pipet. After
28. Calculations
distillation, the volume of water col-
lected in the trap from this flask should 28.1 If the specimen weight is the
be between 4.95 and 5.05 ml. (This same as the stabilized weight (Note 2)
range corresponds to the reading tol- of the laboratory sample, calculate to
erance given in 27.8). If the observed the nearest 0.01 percentage points the
volume does not come within the speci- amount of moisture as moisture content
fied limits, tests made with this toluene or moisture regain by Eq 9 or 10 as
supply are not satisfactory. Repeat the follows:
tests using a new supply of water-
Moisture content, per cent,
saturated toluene.
27.3 Select a specimen, determine its
weight to the nearest 0.05 g, and desig- X 100. .(9)
('-^)
nate this weight as W\.
21A Transfer the specimen to a flask Moisture regain, per cent,
42-4
 TESTS FOR AMOUNT OF MOISTURE IN TEXTILE MATERIALS (D 2654) 601

29. Report
X 100.. (10)
\Wi-V ) 29.1 State that the tests were made
as directed in ASTM Method D 2654,
where: Option 3, and report the following in-
V = volume of the water collected in formation:
the trap, in ml, 29.1.1 The average (arithmetic mean)
Wo = original weight (Note 2) of the value of the results calculated for a par-
sample (at time of sampling), and ticular lot, stating whether it is a mois-
W\ = weight of specimen. ture content or a moisture regain value,
28.2 If the specimen weight, W\, 29.1.2 The number of specimens
represents only a portion of the sta- tested,
bilized weight of the laboratory sample, 29.1.3 The range of the moisture re-
W, calculate the amount of moisture as sults (difference between the largest and
moisture content or moisture regain smallest calculated result), and
by either Eq 11 or 12 as follows: 29.1.4 Volume of water measured for
Moisture content, per cent, the control (see 27.2).
30. Precision
30.1 An interlaboratory test con-
ducted in 1963 in which each of six
Moisture regain, per cent, laboratories measured at least 12 speci-
mens of each of three different materials
/ W0

FD
l\ X 100..(12) at two different levels of moisture con-
W\ tent yielded the following components
of variance:
30.1.1 Within-laboratories, 0.184 per-
where: centage points squared calculated on the
V = volume of the water collected in basis of moisture content.
the trap, in ml, 30.1.2 Between-laboratories, 0.016
W\ = weight (Note 2) of the specimen percentage points squared calculated on
tested, the basis of moisture content.
Wo — original weight of the sample 30.2 Data collected in 1965 from five
from which the specimen was different laboratories show an improved
taken, and estimate of the within-laboratories com-
W = stabilized weight of the sample ponent to be 0.026 percentage points
from which the specimen was squared. No additional estimates of be-
taken. tween-laboratory variance are available.
28.3 When the mean value of several 30.3 As a consequence it is expected
specimens is calculated, compute also that the within-laboratory precision of
the standard error of the mean. Since the average of the two specimens of a
the true mean is quite likely to lie any- uniform material will be within ± 0.23
where within the range of values bounded percentage points of the "true" moisture
by the mean ± one standard error, the content 95 per cent of the time. If two
size of the range determines the decimal specimens each of a uniform material are
position at which variations begin to measured by two laboratories, it is ex-
occur. Carry only one doubtful figure in pected that the laboratory averages will
stating the mean. (See Examples 1 and agree to within 0.48 percentage points
2 under 10.5.) 95 per cent of the time.
42-4 x