AATCC Test Method 89-2003

Mercerization in Cotton
Developed in 1958 by AATCC Commit- ing of barium hydroxide, sodium carbon- 7. Reagents and Materials
tee RA66; editorially revised 1974, ate and hydrochloric acid. Concentrated
1984, 1986, 1988, 1990, 1992; reaf- acids should be handled only in an 7.1 Hydrochloric acid (HCl) standard-
firmed 1974, 1977, 1980, 1989, 1998, adequately ventilated laboratory hood. ized approx. 0.1N.
2003; editorially revised and reaffirmed CAUTION: Always add acid to water. 7.2 Barium hydroxide reagent
1985, 1994. 4.4 Petroleum solvent can be a com- [Ba(OH)2] approximately 0.25N (see
bustible or flammable liquid, depending 13.1).
on which solvent is used, and presents a 7.3 Phenolphthalein.
1. Purpose and Scope hazard. Ethanol and methanol are flam- 7.4 Petroleum solvent [BP 30-60°C
mable liquids. Flammable liquids should (86-140°F)].
1.1 This test method provides a method be stored in the laboratory only in small 7.5 Alcohol (95% ethanol or anhy-
for the determination of the presence of containers away from heat, open flame drous methanol).
mercerization in dyed and undyed cotton and sparks. These chemicals should not 7.6 Enzyme, starch-solubilizing.
yarns and fabrics. In addition, the test be used near an open flame. 7.7 Soap, neutral, granular (see 13.2).
will give an indication of the complete- 4.4.1 Carry out reflux procedure in a 7.8 Water, distilled.
ness of the reaction between the cotton well ventilated hood with an electrical 7.9 Cotton yarn, unmercerized for ref-
and the mercerization bath. heating mantle or a water bath as the heat erence (standard cotton) (see 13.3).
source.
2. Principle 4.4.2 Use chemical goggles or face 8. Test Specimens
shield, impervious gloves and an imper-
2.1 Carefully scoured specimens of the 8.1 A minimum of 5 g of each sample
vious apron when handling organic sol-
cotton to be tested and unmercerized cot- and of the unmercerized standards are
vents.
ton are immersed in separate baths of bar- scoured as directed after which a 2 g
ium hydroxide solution for a definite time 4.5 An eyewash/safety shower should specimen of each scoured sample is
period. Aliquot portions of each soaking be located nearby and an organic vapor weighed and placed in clean, dry glass-
bath and of fresh barium hydroxide solu- respirator and a self-contained breathing stoppered flasks.
tion are then titrated with hydrochloric apparatus should be readily available for
acid. emergency use.
4.6 Exposure to chemicals used in this 9. Procedure
2.2 The ratio of the amount of barium
hydroxide absorbed by the mercerized procedure must be controlled at or below 9.1 Scouring. The purpose of the
specimen to that absorbed by the unmer- levels set by governmental authorities scouring operation is to remove all extra-
cerized specimen multiplied by 100 gives [e.g., Occupational Safety and Health neous matter, leaving the cotton cellulose
the barium activity number. Administration’s (OSHA) permissible in as pure a form as possible and without
exposure limits (PEL) as found in 29 changing it chemically.
CFR 1910.1000 of January 1, 1989]. In 9.1.1 The samples to be tested (at least
3. Terminology addition, the American Conference of 5 g each), together with the standard un-
3.1 mercerization, n.—a process for Governmental Industrial Hygienists mercerized cotton, are refluxed together
irreversibly altering the physical charac- (ACGIH) Threshold Limit Values (TLVs) successively for 1 h with petroleum sol-
teristics and appearance of natural cellu- comprised of time weighted averages vent [boiling point 30-60°C (86-140°F)],
losic fibers by swelling in strong alkali. (TLV-TWA), short term exposure limits 1 h with alcohol (95% USP ethanol, No.
(TLV-STEL) and ceiling limits (TLV-C) 30 specially denatured alcohol, 95% or
are recommended as a general guide for anhydrous methanol may be used), and
4. Safety Precautions
air contaminant exposure which should for 1 h with distilled water (see 13.4).
NOTE: These safety precautions are be met (see 13.7). 9.1.2 Following these three extrac-
for information purposes only. The pre- tions, starches are removed as follows:
cautions are ancillary to the testing proce- 5. Limitations 9.1.3 Cover the sample with distilled
dures and are not intended to be all inclu- water containing 3% of a commercial
sive. It is the user’s responsibility to use 5.1 The test cannot be used satisfacto- starch-solubilizing malt enzyme solution
safe and proper techniques in handling rily if durable finishes or fibers other than and heat to 60 ± 5°C (140 ± 9°F). Main-
materials in this test method. Manufac- cotton are present. tain the solution at this temperature for a
turers MUST be consulted for specific period of 1 h. Pour off the enzyme solu-
details such as material safety data sheets 6. Apparatus tion, rinse and then scour as follows.
and other manufacturer’s recommenda- 9.1.4 Boil the samples together for 1 h
tions. All OSHA standards and rules 6.1 Burette (preferably automatic) (see
in 1 L of water containing 10 g of a neu-
must also be consulted and followed. 13.4).
tral soap and 2 g of soda ash. Wash re-
4.1 Good laboratory practices should 6.2 Flask, Erlenmeyer, with reflux peatedly in warm water until free from
be followed. Wear safety glasses in all tube. soap and alkali, i.e., until neutral to phe-
laboratory areas. 6.3 Flasks, glass-stoppered, 250 mL. nolphthalein, squeeze and dry. The sam-
4.2 All chemicals should be handled 6.4 Flasks, Erlenmeyer, 125 mL. ples and the standard unmercerized cot-
with care. 6.5 Bottles, storage, 250-500 mL. ton are dried in an oven at 100°C (212°F)
4.3 Use chemical goggles or face 6.6 Beaker, 1500 mL. until thoroughly dry. The samples are
shield, impervious gloves and an imper- 6.7 Pipette, 10 mL. then allowed to come to room conditions.
vious apron during dispensing and mix- 6.8 Drying oven. Each sample should then be cut into

122 TM 89-2003 AATCC Technical Manual/2006

Copyright © 2005 American Association of Textile Chemists and Colorists
small pieces [approximately 3 mm (0.125 Table I—Barium Numbers: Interlaboratory Tests on Mercerized Fabrics
in.) square] for subsequent weighing.
Cloth Lab A Lab B Lab C1 Lab C2 Lab C3
9.2 Testing. Prepare and test duplicate
specimens from each sample. Weigh 2 g 80 × 80—35° Tw 118 118 117 120 114
80 × 80—55° Tw 130 131 128 132 125
of each scoured sample and of the
108 × 58—55° Tw 141 145 143 143 140
scoured standard cotton into dry 250-mL
136 × 64—55° Tw 122 123 123 122 120
flasks equipped with stoppers. (Ground 88 × 50—55° Tw 139 140 136 140 133
glass stoppers are recommended.) Add
30 mL 0.25N barium hydroxide (see 1
Fabrics scoured by Lab C, unmercerized 80 × 80 as standard.
13.5) to each flask containing a test spec- 2
Fabrics scoured by Lab A, unmercerized 80 × 80 as standard.
imen and to two empty flasks for blank 3
Fabrics scoured by Lab C, 40/2 combed mercerized yarn as standard.
determinations. Stopper each flask imme-
diately upon addition of the barium hy-
droxide and store them for at least 2 h in a
water bath at 20-25°C (68-77°F) (room tion. A barium activity number above soda ash treatment. If one sample requires sol-
temperature). Shake the flasks at frequent 150 indicates substantially complete re- vent extraction and the enzyme treatment,
intervals. After 2 h, transfer 10 mL of so- action between the cotton and the mercer- then all samples including the standard cotton
lution (see 13.6) from each container, in- izing bath. Intermediate numbers indicate must be treated together with the complete
cluding the blanks and titrate with 0.1N scouring procedure to insure the same final
either incomplete reaction or use of a state for the whole set of samples.
hydrochloric acid, using phenolphthalein weak mercerizing bath. 13.5 An automatic burette is most conve-
as an indicator. nient for the addition of the barium hydroxide
12. Precision and Bias solution to the specimens. The air outlet must
10. Calculations be equipped with an absorption tube contain-
12.1 Precision. Precision for this test ing soda lime to remove carbon dioxide. The
10.1 Using the titration figures, deter- method has not been established. Until a latter must not be allowed to enter any burette
mine the ratio of barium hydroxide ab- precision statement is generated for this that might be used, because formation of bar-
sorbed by a mercerized specimen to that test method, use standard statistical tech- ium carbonate not only affects the concentra-
absorbed by the unmercerized standard. tion of the reagent but forms a film which
niques in making any comparisons of test interferes with burette readings. A cork is fitted
Multiply this ratio by 100 to obtain the results for either within-laboratory or
barium activity number. to the bottom of the burette in such a manner
between-laboratory averages. that the 250 mL Erlenmeyer flasks containing
Example: 10 mL of barium hydroxide 12.2 Bias. Mercerization in cotton can the specimens under test are locked into place
solution (blank) required 24.30 mL of be defined only in terms of a test method. without exposure to air during the addition of
0.1N HCl; 10 mL of barium hydroxide There is no independent method for de- barium hydroxide. The barium hydroxide solu-
from an unknown sample of cotton re- termining the true value. As a means of tion should cover the specimens, tilting the
quired 19.58 mL of 0.1N HCl; 10 mL of estimating this property, the method has flasks if necessary to accomplish this end.
barium hydroxide from unmercerized no known bias. 13.6 For the removal of 10 mL of barium
cotton (standard) required 21.20 mL of hydroxide when equilibrium has been
0.1N HCl. Therefore the barium number reached, a 10 mL pipette is used. The same pi-
of the unknown sample is: 13. Notes pette, burette, etc., should be used for the
whole set of determinations and the same
24.30 – 19.58- 13.1 The barium hydroxide reagent is pre- technique for emptying or filling pipettes and
-------------------------------- × 100 = 152 pared by shaking distilled water with slightly burettes should be used on each determina-
24.30 – 21.20 more than the calculated quantity of barium tion. The hydrochloric acid burette is also
hydroxide, allowing it to stand overnight in a equipped with a cork to which the 125 mL
10.2 Barium numbers should be run in stoppered bottle, and then siphoning the clear flask can be attached during the titration of the
duplicate and should be reported sepa- solution into a clean storage bottle. 10 mL aliquot portions of barium hydroxide,
rately. Duplicate runs should not be off 13.2 Available from AATCC, P.O. Box thereby eliminating titration errors resulting
by more than four units. The titrations 12215, Research Triangle Park NC 27709; tel: from carbon dioxide absorption by the alka-
should be within 0.1 mL for check re- 919/549-8141; fax: 919/549-8933; e-mail: or- line solution. In removing the 10 mL aliquot
sults. Skilled operators can estimate to ders@aatcc.org. portion of barium hydroxide from flasks con-
within 0.05 mL. A difference of more 13.3 Unmercerized standard cotton skeins taining specimens, the operator should use the
than four units between duplicate runs in- (40/2 ply) as used for the Draves Wetting end of his pipette to push the cotton against
Tests are particularly satisfactory. They may the wall of the flask and to express the excess
dicates inaccuracy in running the test (see be obtained from Testfabrics Inc., P.O. Box liquor. In this way, a larger amount of the solu-
Table I). 26, 415 Delaware St., W. Pittston PA 18643; tion will be available for drawing up into the
tel: 570/603-0432; fax: 570/603-0433; e-mail: pipette.
11. Interpretation testfabric@aol.com. 13.7 Available from Publications Office,
13.4 If it is known that all samples that test ACGIH, Kemper Woods Center, 1330
11.1 A barium activity number in the do not contain finish or starch, then the scour- Kemper Meadow Dr., Cincinnati OH 45240;
range of 100-105 indicates no merceriza- ing procedure may begin with the soap-and- tel: 513/742-2020.

AATCC Technical Manual/2006 TM 89-2003 123

Copyright © 2005 American Association of Textile Chemists and Colorists