AATCC Test Method 20A-2017

Fiber Analysis: Quantitative

Developed in 1957 by AATCC Commit- When used in commerce for the repre- mon terms or in A Glossary of AATCC
tee RA24; revised 1958, 1959, 1975, sentation of the nominal fiber content of Standard Terminology (located else-
1995, 2000, 2004, 2005, 2007, 2008, end use items such as garments, moisture where in this Technical Manual).
2010, 2011, 2012, 2013, 2014, 2017; regain is typically added back to bone dry
reaffirmed 1971, 1978, 1981, 1989; edi- numbers generated. ASTM D1909, Stan- 4. Safety Precautions
torially revised 1980, 1982 (new title), dard Table of Commercial Moisture Re-
1985, 2002, 2009, 2015. Related to ISO gains for Textile Fibers, can be used for NOTE: These safety precautions are
17751 and 1833 and IWTO 58. this purpose. for information purposes only. The pre-
2.3 The procedure for determining fi- cautions are ancillary to the testing proce-
ber composition by mechanical separa- dures and are not intended to be all inclu-
1. Purpose and Scope tion is applicable to those textiles sive. It is the user’s responsibility to use
wherein the different fibers making up its safe and proper techniques in handling
1.1 This method presents individual materials in this test method. Manufac-
procedures for the quantitative determi- composition are segregated in separate
yarns, or plies, in the textile product. turers MUST be consulted for specific
nation of moisture content, nonfibrous details such as material safety data sheets
content and fiber composition of textiles. 2.4 The chemical procedures for fiber
composition described herein are applica- and other manufacturer’s recommenda-
1.2 The procedures for the determina- tions. All OSHA standards and rules
tion of fiber composition include me- ble to most of the current, commercial
production fibers within each generic must also be consulted and followed.
chanical, chemical and microscopical 4.1 Good laboratory practices should
methods. They are applicable to blends of class listed. Known exceptions are noted
in Table II. However, there may be in- be followed. Wear safety glasses in all
the following generic classes: laboratory areas.
stances in which a method may not be
Natural Fibers Man-Made Fibers fully adequate for a newly developed fi- 4.2 All chemicals should be handled
Cotton Acetate ber falling within one of the listed generic with care.
Hair Acrylic classes and for re-used and/or physically 4.3 Perform the soxhlet extractions in
Hemp Modacrylic or chemically modified fibers. Caution Section 9, Nonfibrous Material—Clean
Linen Nylon (see 17.1) should be exercised when applying these Fiber Content, using hexane and ethyl al-
Ramie Olefin methods to such cases. cohol inside an adequately ventilated lab-
Silk Polybenzimidazole oratory hood. CAUTION: Hexane and
2.5 The microscopical procedures for fi-
Wool Polyester ethyl alcohol are highly flammable.
Rayon ber composition are applicable to all fibers
and their accuracy depends to a consider- 4.4 Perform Chemical Analysis Proce-
Spandex
Triexta able extent upon the ability of the analyst dure No. 1 (Table II, 100% acetone) in-
to identify the individual fibers present. side a ventilated laboratory hood. CAU-
2. Uses and Limitations However, owing to the tedious nature of TION: Acetone is highly flammable.
this technique, its use is generally limited 4.5 Hexane, ethyl alcohol and acetone
2.1 The procedure given for the removal to those mixtures which cannot be sepa- are flammable liquids and should be
of nonfibrous materials will remove most, rated mechanically or chemically; e.g., stored in the laboratory only in small
but not all, of these components. Each mixtures of hair and wool and mixtures of quantities away from heat, open flame
treatment is applicable only to certain cat- cotton, linen, hemp and/or ramie. and sparks.
egories of these substances and no general 4.6 In preparing, dispensing, and han-
scheme can be given that is all inclusive. 3. Terminology dling hydrochloric acid (20%), sulfuric
2.1.1 Some of the newer finishes may acids (59.5% and 70%), and formic acid
present special problems and the analyst 3.1 clean-fiber content, n.—the amount (90%) used in Chemical Analysis Proce-
will have to deal with these cases as they of fiber after removal of nonfibrous dure Methods No. 2, 3, 4, and 6 (Table
arise. Thermosetting resins and crosslink- content. II), use chemical goggles or face shield,
ing latices are not only difficult to re- 3.2 fiber, n.—in textiles, a generic impervious gloves and an impervious
move but in some cases cannot be wholly term for any one of the various types of apron. Concentrated acids should be han-
removed without destroying the fiber. matter that form the basic elements of a dled only in an adequately ventilated lab-
2.1.2 When it is necessary to modify a textile and which are generally character- oratory hood. CAUTION: Always add
procedure, or use a new one, one should ized by flexibility, fineness and high ratio acid to water.
make sure that the fibrous portion of the of length to thickness. 4.7 In preparing ammonium hydroxide
specimen under test is not attacked. 3.3 moisture content, n.—that part of (8:92) for use in Chemical Analysis Pro-
2.2 Fiber composition is generally ex- the total mass of a material that is ab- cedure Method No. 4 (Table II, 70% sul-
pressed in the laboratory either on the sorbed or adsorbed water, compared to furic acid), use chemical goggles or face
oven-dry weight of the textile as received the total mass. shield, impervious gloves and an imper-
or on the oven-dry weight of the clean fi- 3.4 nonfibrous content, n.—products vious apron. Dispense, mix and handle
ber after nonfibrous materials are first re- such as fiber finishes, yarn lubricants, ammonium hydroxide only in an ade-
moved from the textile before the fiber slasher sizing, fabric softeners, starches, quately ventilated laboratory hood.
analysis is carried out, or if the treatments china-clay, soaps, waxes, oils and resins 4.8 An eyewash/safety shower should
described in Section 9 are incapable of re- which are applied to fiber, yarn, fabric or be located nearby and a self-contained
moving them, any such materials present apparel. breathing apparatus should be readily
will increase the percentage of the fiber 3.5 Additional terms used in this test available for emergency use.
constituent with which they are removed method can be found in standard chemi- 4.9 Exposure to chemicals used in this
during the analysis. cal dictionaries, in dictionaries of com- procedure must be controlled at or below

80 TM20A-2017 AATCC Technical Manual/2018

Copyright © 2017 American Association of Textile Chemists and Colorists
levels set by governmental authorities 6.6 Hydrochloric acid (HCl) (20%). plete pattern (see 17.4).
(e.g., Occupational Safety and Health Dilute HCl, sp gr 1.19, with water until 7.1.4 In the case of yarns, not less than
Administration’s [OSHA] permissible the specific gravity of the solution is 1.10 a 2-meter length should be taken.
exposure limits [PEL] as found in 29 at 20°C.
CFR 1910.1000; see web site: 6.7 Sulfuric acid (H2SO4) (59.5%). Test Methods
www.osha.gov for latest version). In ad- Add H2SO4, sp gr 1.84, slowly to water.
8. Moisture Content
dition, the American Conference of Gov- After the solution has cooled to 20°C, ad-
ernmental Industrial Hygienists (AC- just the density to a value between 1.4902 8.1 Procedure. Place not less than 1 g
GIH) Threshold Limit Values (TLVs) and 1.4956 g/mL. of the textile to be tested in a previously
comprised of time weighted averages 6.8 Sulfuric acid (H2SO4) (70%). Add tared weighing bottle and immediately
(TLV-TWA), short term exposure limits H2SO4, sp gr 1.84, slowly to water. After replace the cover. Weigh to the nearest
(TLV-STEL) and ceiling limits (TLV-C) the solution has cooled to 20 ± 1°C, ad- 0.1 mg using the analytical balance and
are recommended as a general guide for just the density to a value between 1.5989 record the weight. Place the uncovered
air contaminant exposure which should and 1.6221 g/mL. weighing bottle containing the specimen
be met (see 17.2). 6.9 Sulfuric acid (H2SO4) (1:19). in an oven maintained at 105-110°C for
Slowly stir 1 volume of H2SO4, sp gr 1.5 h. At the end of the time period, re-
5. Apparatus 1.84, into 19 volumes of water. move the bottle from the oven, immedi-
6.10 Sodium hypochlorite (NaOCl). ately replace the cover and put it in the
5.1 Analytical balance, capable of Prepare a solution of NaOCl, 5.25% desiccator. When the bottle and contents
weighing to 0.1 mg. available chlorine. Sodium hypochlorite have cooled to room temperature, remove
5.2 Oven, maintained at 105-110°C. based household bleach (nominally them from the desiccator and reweigh.
5.3 Desiccator, containing anhydrous 5.25%) has been found to be acceptable. Repeat the heating and reweighing pro-
silica gel, calcium sulfate (such as Drie- 6.11 Sodium bisulfite (NaHSO3) (1%). cess for periods of 30 min until the
ite) or its equivalent. Freshly prepared. weight is constant to within ± 0.001 g and
5.4 Soxhlet extractor, 200 mL capac- 6.12 Formic acid (HCOOH) (90%), sp record the constant weight.
ity. gr of 1.202 at 20°C. 8.2 Calculations.
5.5 Constant temperature bath, adjust- 6.13 Ammonium hydroxide (NH4OH) 8.2.1 Calculate the moisture content of
able, capable of controlling temperature (8:92). Mix 8 volumes of NH4OH, sp gr the specimen as follows:
to ± 1°C. 0.90, with 92 volumes of water.
5.6 Weighing bottle, 100 mL capacity, 6.14 Herzberg stain. Add the previ- A–B
glass, with ground glass cover. (Alter- ously prepared solution A to solution B; M = ------------- × 100
A–T
nate: aluminum weighing can; same size, allow to stand overnight; decant the clear
tight cover.) liquid into a dark colored glass bottle and where:
5.7 Erlenmeyer flask, 250 mL capac- add a leaf of iodine. M = moisture content, percent.
ity, ground glass stopper. A = weight of sample before drying +
Solution A Solution B
5.8 Beaker, borosilicate heat resistant bottle.
glass, 250 mL capacity. Zinc Chloride 50 g Potassium
Iodide 5.5 g B = weight of sample after drying +
5.9 Filtering crucible, fritted glass, bottle.
Water 25 mL Iodine 0.25 g
coarse porosity, 30 mL. T = tare weight of weighing bottle.
Water 12.5 mL
5.10 Suction flask, with adapter, to
hold filtering crucible. 6.15 Isopropanol (C3H7)HO (70%)
5.11 Weighing bottle, large enough to 6.16 N,N-Dimethylacetamide 9. Nonfibrous Material—Clean Fiber
hold filtering crucible. CH3C(O)N(CH3)2 Content
5.12 Microscope, equipped with a 6.17 Methanol (CH3OH), reagent grade. 9.1 Procedure. Take a specimen of not
moveable stage and a cross-hair ocular, 6.18 Sodium Hydroxide (NaOH), pellet, less than 5 g, dry it to constant weight in
200-250X magnification. 95% reagent grade. an oven at 105-110°C (see 8.1), record
5.13 Projection microscope, capable of 6.19 Xylenes (C6H4(CH3)2), mixed, 95% the oven-dry weight to the nearest 0.1 mg
500X magnification. reagent grade. using an analytical balance and then sub-
5.14 Fiber cutter: A device comprised 6.20 Lithium Chloride (LiCl), crystal ject it to one, or more, of the following
of two razor blades, a threaded pin and reagent grade. treatments, as appropriate. When specific
an assemblage that will hold the blades type of nonfibrous content is known, only
rigidly in position. The device is operated that specific treatment, or treatments,
7. Sampling
by applying pressure vertically down- need be performed; otherwise, all treat-
ward. It cuts fibers approximately 250 µm 7.1 It is not possible to give specific in- ments must be applied.
in length. structions for taking a laboratory test 9.1.1 Hexane Treatment (for removal
5.15 Wedge scale: Strips of heavy pa- sample from all types of textile materials of oils, fats, waxes, etc.). Extract the
per or Bristol board imprinted with a to which these methods may be applica- dried specimen with hexane in a soxhlet
wedge for use at 500X magnification. ble; but a few general recommendations extractor, siphoning over a minimum of
5.16 Flask cover (see 17.16). will be given. six times. Air dry, and then dry at 105-
7.1.1 The sample should be as repre- 110°C to constant weight. For an alterna-
6. Reagents sentative as possible of the lot of material tive to soxhlet extractor, see 17.15.
from which it was taken. 9.1.2 Alcohol Treatment (for removal
6.1 Ethyl alcohol (95%), pure or dena- 7.1.2 If a reasonably large lot is avail- of soaps, cationic finishes, etc.). Extract
tured. able, and if it is possible to do so, sam- the dried specimen with ethyl alcohol in a
6.2 Hexane (C6H14). plings should be taken from different, soxhlet extractor, siphoning over a mini-
6.3 Hydrochloric acid (HCl), 0.1N. widely separated areas or parts of the lot. mum of six times. Air dry, and then dry at
6.4 Enzyme solubilizing preparation. 7.1.3 In the case of fabrics where there 105-110°C to constant weight. For an al-
6.5 Acetone (CH3COCH3), reagent is a definite repetition in the pattern, the ternative to soxhlet extractor, see 17.15.
grade. sample should include all yarns in a com- 9.1.3 Aqueous Treatment (for removal

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Copyright © 2017 American Association of Textile Chemists and Colorists
of water soluble materials). Immerse the 11. Chemical Analysis—General mg. Transfer into a 250 mL Erlenmeyer
dried specimen for 30 min in water at 50°C flask. Add 50-150 mL of 20% hydrochlo-
using a 100:1 liquid to fabric ratio. Stir 11.1 Specimen Preparation. Before ric acid (100 mL reagent/g of sample);
occasionally or use a mechanical shaker. analyses are undertaken, the laboratory shake vigorously and let stand for 5 min
Rinse 3 times in fresh portions of water test sample should be disintegrated, ho- at 15-25°C. Shake again and let stand for
and dry at 105-110°C to constant weight. mogenized and a portion of the homoge- 15 min. Shake for a third time (see 17.6)
9.1.4 Enzyme Treatment (for removal nate taken for the chemical treatment(s). and filter the mixture through a dried
of starch, etc.). Immerse the dried speci- In the case of a fabric, one should un- weighed fritted-glass crucible. Wash into
men in aqueous solution of the enzyme ravel it into its individual yarns, cut the the crucible any residue left in the flask
preparation following the manufacturer’s yarns into lengths not greater than 3 mm, using a little more 20% hydrochloric
recommendations as to concentration, thoroughly mix the cut pieces and then acid. Apply suction to drain the excess li-
liquid to fabric ratio and temperature and take a representative portion for the spe- quor from the filter residue. Wash the
time of immersion. Rinse thoroughly cific determination. An alternate proce- residue in the crucible with about 40 mL
with hot water and dry at 105-110°C to dure, suitable in many cases, is to grind of 20% hydrochloric acid and then with
constant weight. the sample using a Wiley Mill, homoge- water until the filtrate is neutral to litmus.
9.1.5 Acid Treatment (for removal of nize the ground fibers by slurrying them Disconnect the suction and add to the
amino resins). Immerse the dried speci- in a water suspension in a Waring crucible about 25 mL of ammonium hy-
men in 100 times its weight of 0.1N HCl Blender and taking the representative droxide (8:92) allowing the fiber residue
at 80°C for 25 min, stirring occasionally. portion from the dried homogenate for to soak for 10 min before applying suc-
Rinse thoroughly with hot water and dry the specific determination. Yarns are tion to drain it. Wash the residue with
at 105-110°C to constant weight. treated the same way but omitting the un- about 250 mL of water, allowing it to
9.2 Calculations. necessary steps. soak in the water for about 15 min. After
9.2.1 Calculate the nonfibrous content 11.2 Method Application. A tabula- the final washing, apply suction to re-
of the specimen as follows: tion of appropriate chemical treatments move rinse water, and dry the crucible
for binary fiber mixtures is given in Table and residue in an oven at 105-110°C to
C–D I. To use this table one enters at the left constant weight. Record the dry weight to
N = -------------- × 100 side on the line listing one of the compo-
C the nearest 0.1 mg.
nents of the binary mixture and moves to
where: the box under the column listing the other 12.3 Method No. 3, 59.5% Sulfuric
N = nonfibrous materials, percent. component and the number therein is the acid: Weigh accurately a 0.5-1.5 g por-
C = dry weight, specimen, before method, or methods, that are applicable tion of the clean, dry, prepared specimen
treatment. for that specific combination. The un- and record the weight to the nearest 0.1
D = dry weight, specimen, after treat- bracketed methods are those that dissolve mg. Transfer into a 250 mL Erlenmeyer
ment. the fiber at the left side of the diagram flask. Add 50-150 mL of 59.5% sulfuric
while the bracketed ones dissolve the fi- acid (100 mL reagent/g of sample) and
9.2.2 Calculate the clean fiber content shake vigorously for 1 min. Let stand for
ber at the top of the diagram. Mixtures of
of the specimen as follows: 15 min at a temperature of 15-25°C.
more than two components may be ana-
lyzed by proper application of a sequence Shake again and let stand for another 15
D min, shake for a third time (see 17.6) and
F = ---- × 100 of the individual methods. Table II pre-
C then filter the mixture through a dried
sents the relative solubilities of the vari-
where: ous fibers in all the reagents and, from weighed fritted-glass crucible. Wash into
F = clean fiber content, percent; other this, one can select the proper methods the crucible any residue left in the flask
terms as in 9.2.1 and their sequence for the analysis of using three 10 mL aliquots of 59.5% sul-
multifiber mixtures (see 17.5). furic acid. Apply suction to drain the ex-
9.2.3 Additional techniques for the ex- cess liquor from the fiber residue after
traction and analysis of textile finishes can the addition of each aliquot. Wash the
be found in AATCC Test Method (TM) 12. Chemical Analysis Procedures residue in the crucible with 50 mL of sul-
94, Finishes in Textiles: Identification. 12.1 Method No. 1, 100% Acetone: furic acid (1:19), then with water until
Weigh accurately a 0.5-1.5 g portion of the filtrate is neutral to litmus. Discon-
10. Mechanical Separation the clean, dry, prepared specimen and nect the suction and add to the crucible
record the weight to the nearest 0.1 mg. about 25 mL of ammonium hydroxide
10.1 Procedure. Remove the non- (8:92), allowing the fiber residue to soak
fibrous materials using the appropriate Transfer into a 250 mL Erlenmeyer flask.
Add 100 times its weight of acetone and for 10 min before applying suction to
treatment (see 9.1). Separate the compo- drain it. Wash the residue with about 150
nent yarns by mechanical dissection; agitate vigorously for 15 min keeping the
temperature at 40-50°C. Decant the liq- mL of water, allowing it to soak in the
combine those yarns, or plies, having the water for about 15 min. After the final
same fiber composition and determine uid from the undissolved residue, add a
fresh portion of acetone and agitate for a washing, apply suction to remove the
the oven-dry weight of each generic type rinse water and dry the crucible and fiber
present. few more minutes. Repeat the decanting
and agitation process one more time and residue in an oven at 105-110°C to con-
10.2 Calculation. Calculate the content stant weight. Record the weight of the dried
then filter the undissolved residue by suc-
of each generic fiber as follows: residue to the nearest 0.1 mg (see 17.7).
tion through a dried weighed, fritted-
W glass, filtering crucible. Dry the crucible 12.4 Method No. 4, 70% Sulfuric acid:
X i = ------i × 100 and residue in air and then in an oven at Weigh accurately a 0.5-1.5 g portion of
E
105-110°C to constant weight. Record the clean, dry, prepared specimen and
where: the weight of the dried residue to the record the weight to the nearest 0.1 mg.
Xi = content of fiber i, percent. nearest 0.1 mg. Transfer into a 250 mL Erlenmeyer flask.
Wi = oven-dry weight of fiber i, after 12.2 Method No. 2, 20% Hydrochloric Add 50-150 mL of 70% sulfuric acid
separation. acid: Weigh accurately a 0.5-1.5 g por- (100 mL reagent/g of sample) and shake
E = weight of clean, oven-dry speci- tion of the clean, dry, prepared specimen vigorously for 1 min. Let stand for 15
men taken for analysis. and record the weight to the nearest 0.1 min at a temperature of 15-25°C. Shake

82 TM20A-2017 AATCC Technical Manual/2018

Copyright © 2017 American Association of Textile Chemists and Colorists
 Table I—Chemical Methods for Analysis of Fiber Mixtures
Cotton,
Poly- Hemp,
Wool/ Rayon, Polyester, amide- Para- Mod- Meta- Mela- Linen,
Hair*** Spandex Silk Lyocell Triexta imide PLA aramid Olefin Nylon acrylic aramid mine Ramie Acrylic
Acetate 1 4 (5) 1 1 (5) 1 1 (9) 1 1 1 1 (10) 1 (2) N/A 1 1 1 1
Acrylic 7 8 (5) N/A 7 8 (3) (5) 7 8 (3) 7 8 (9) 78 78 78 7 8 (10) 7 8 (2) (3) (6) (1) 78 78 78
Cotton, Hemp, 4 (5) (7) (8) (5) (3) 4 (9) 4 4 4 4 (10) (2) (6) 4 (1) 4 (11) 4
Linen, Ramie,
Jute, Sisal
Melamine (5) (7) (8) (3) (4) (5) (3) (4) (9) — — — (10) (2) (6) (1) (11)
Meta-aramid (5) (7) (8) (3) (4) (5) (3) (4) (9) 11 — 11 (10) (2) (6) (1)
Modacrylic (5) 1* 1* (3) (4) (5) 1* (3) (4) 1* (9) 1* 1* 1* 1* (10) 1* (2) (6)
Nylon 2** 3 6 (5) 2** 3 6 (7) (8) (5) 2** 6 2** 3 6 (9) 2** 3 6 2** 3 6 2** 3 6 2** 3 6 (10)
Olefin 10 (5) 10 (7) (8) 10 (3) (4) (5) 10 (4) 10 (9) 10 10 10
Para-aramid (5) (7) (8) (3) (4) (5) (3) (4) (9) — —
PLA (5) (7) (8) (3) (4) (5) (3) (4) (9) —
Polyamide- (5) (7) (8) (3) (4) (5) (3) (4) (9)
imide
Polyester, (5) 9 (7) (8) (3) (4) (5) 9 (3) (4)
Triexta
Rayon, Lyocell 4 (5) (7) (8) (5)
Silk 34 (7) (8)
Spandex 78
Notes:
The unbracketed methods are those that dissolve the fiber at the left side of the diagram while the bracketed ones dissolve the fiber at the top of the diagram.
NA = Chemical Methods not applicable to separate two different fiber types of the same generic class. Use the microscopy sections of TM20A.
— = Method Under Development.
Section 11.2 contains details of table use.
1 *100% acetone: section 12.1 ***Not suitable for all modacrylic fibers
2 20% hydrochloric acid: section 12.2 ***Not suitable for all nylon fibers
3 59.5% sulfuric acid: section 12.3 ***Hair fibers referenced in TM20A are synonymous with fibers with scales on surface in Table I of TM20
4 70% sulfuric acid: section 12.4
5 sodium hypochlorite: section 12.5
6 90% formic acid: section 12.6
7 dimethylformamide section 12.7
8 N,N-dimethylacetamide section 12.8
9 alkaline methanol section 12.9
10 xylenes section 12.10
11 4% lithium chloride in
N,N-dimethylacetamide section 12.11

again and let stand for another 15 min; rite: Weigh accurately a 0.5-1.5 g portion mL reagent/g of sample) and shake fre-
shake for a third time (see 17.6) and then of the clean, dry, prepared specimen and quently over a period of 15 min (see
filter the mixture through a fritted-glass record the weight to the nearest 0.1 mg. 17.9). Decant the supernatant liquid into
crucible which has been oven-dried, Transfer into a 250 mL Erlenmeyer flask. a dried, weighed, fritted-glass crucible,
cooled in a desiccator and weighed to 0.1 Add 50-150 mL of sodium hypochlorite add another equal portion of 90% formic
mg. Wash into the crucible any residue reagent (100 mL reagent/g of sample). acid to the flask and agitate for an addi-
left in the flask using three 10 mL ali- Use a wrist shaker or stir the specimen tional 15 min. Filter the contents of the
quots of 70% sulfuric acid. Apply suction vigorously in this solution for 20 min flask through the crucible, rinse with two
to drain the excess liquor from the fiber making sure the temperature is main- 50 mL portions of 90% formic acid and
residue after the addition of each aliquot. tained at 25 ± 1°C (use constant tempera- drain with the aid of suction. Wash the
Wash the residue in the crucible with 50 ture bath) (see 17.8) and then filter residue with 50 mL of water and then al-
mL of sulfuric acid (1:19), then with wa- through a dried weighed, fritted-glass low it to soak in 25 mL of ammonium hy-
ter until the filtrate is neutral to litmus. crucible. Wash thoroughly with sodium droxide (8:92) for about 10 min. Wash
Disconnect the suction and add to the bisulfite (1%) followed by water and re- the residue thoroughly with water until
crucible about 25 mL of ammonium hy- move the excess water by suction. After the filtrate is neutral to litmus. Drain the
droxide (8:92); allow the fiber residue to the final washing, apply suction to re- residue with the aid of suction and dry in
soak for 10 min before applying suction move excess water and dry in an oven at an oven at 105-110°C to constant weight.
to drain it. Wash the residue with about 105-110°C to constant weight. Record Record the weight of the dried residue to
150 mL of water, allowing it to soak in the weight of the dried residue to the the nearest 0.1 mg.
the water for about 15 min. After the final nearest 0.1 mg. 12.7 Method No. 7, Dimethylforma-
washing, apply suction to remove excess 12.6 Method No. 6, 90% Formic acid: mide: Weigh accurately a 0.5-1.5 g por-
water and dry the crucible and fiber resi- Weigh accurately a 0.5-1.5 g portion of tion of the clean, dried, prepared speci-
due in an oven at 105-110°C to constant the clean, dry, prepared specimen and men and record the weight to the nearest
weight. Record the weight of the dry resi- record the weight to the nearest 0.1 mg. 0.1 mg. Transfer to a 250 mL Erlenmeyer
due to the nearest 0.1 mg. Transfer into a 250 mL Erlenmeyer flask. flask. Add 50-150 mL of dimethylforma-
12.5 Method No. 5, Sodium hypochlo- Add 50-150 mL of 90% formic acid (100 mide reagent (100 mL reagent/g of sam-

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Copyright © 2017 American Association of Textile Chemists and Colorists
 Table II—Solubilities of Fibers in Reagents Used in the Chemical Methods
Chemical Method
No. 11
No. 1 No. 2 No. 3 No. 4 No. 6 No. 7 No. 8 No. 9 No. 10 LiCl +
100% 20% 59.5% 70% No. 5 90% (CH3)2 CH3C(O)N NaOH + 100% CH3C(O)N
CH3COCH3 HCl H2SO4 H2SO4 NaOCl HCOOH NC(O)H (CH3)2 CH3OH C6H4(CH3)2 (CH3)2
Acetate S I S S I S S S S I ND
Acrylic I I I I* I I S S I I ND
Cotton I I SS S I I I I I I ND
Hair I I I I S I I I I I ND
Hemp I I SS S I I I I I I ND
Linen I I SS S I I I I I I ND
Modacrylic S or I* I I I I I PS PS I I ND
Nylon I S S S I S I I I I ND
Olefin I I I I I I I I I S ND
Polyester** I I I I I I I I S I ND
Ramie I I SS S I I I I I I ND
Rayon I I S S I I I I I I ND
Silk I PS S S S PS I I I I ND
Spandex I I PS PS I I S S PS I ND
Wool I I I I S I I I I I ND
Meta-aramid I I I I I I I I I I S
Para-aramid I I I I I I I I I I I
Polyamideimide I I I I I I I I I I I
Melamine I I I I I I I I I I I
PLA I I I I I I I I NA I ND
Lyocell I I S S I I I I I I ND
Polybenzimidazole NA NA NA NA NA NA NA NA NA NA NA

*Depending on type
**Compatible for triexta
KEY TO SYMBOLS: S = SOLUBLE
PS = PARTIALLY SOLUBE (Method not applicable)
SS = SLIGHTLY SOLUBLE (Usable but correction factor required)
I = INSOLUBLE
NA = Not Applicable ND = Not Determined
Section 11.2 contains details of table use.

ple). Agitate for 20 min keeping the tem- tering crucible. Dry the crucible and resi- flask cover. Heat to the boiling tempera-
perature at 98 ± 1°C. Decant the liquid due in air then in an oven at 105-110°C to ture and stir with a magnetic stirrer for 20
from the undissolved residue, add a fresh constant weight. Record the weight of the min. Decant the liquid from the undis-
portion of dimethylformamide and agi- dried residue to the nearest 0.1 mg. solved residue. Rinse well with 70% iso-
tate for a few more minutes. Repeat the 12.9 Method No. 9, Alkaline Metha- propanol, and repeat the decanting and
decanting and agitation process one more nol: Weigh accurately a 0.5-1.5 g portion agitation process. Filter the undissolved
time rinsing well with 70% isopropanol, of clean dried, prepared specimen and residue by suction through a dried,
and then filter the undissolved residue by record the weight to the nearest 0.1 mg. weighed, fritted glass filtering crucible.
suction through a dried, weighed fritted Add 18 g of reagent grade sodium hy- Dry the crucible and residue in air and
glass filtering crucible. Dry the crucible droxide in a pellet form to 200 mL of then in an oven at 105-110°C to constant
and residue in air and then in an oven at methanol (dissolution of the NaOH is weight. Record the weight of the dried
105-110°C to constant weight. Record mildly exothermic) in a 250 mL Erlenm- residue to the nearest 0.1 mg.
the weight of the dried residue to the eyer flask. Heat to 65°C mixing thor- 12.11 Method No. 11, 4% Lithium
nearest 0.1 mg. oughly. Add specimen and stir using a Chloride in N,N-Dimethylacetamide:
12.8 Method No. 8, N,N-Dimethylace- magnetic stirring bar and flask cover. Af- Weigh accurately a 0.5-1.5 g portion of
tamide: Weigh accurately a 0.5-1.5 g por- ter 5 min of immersion, decant the liquid the clean, dried, prepared specimen and
tion of clean, dried, prepared specimen from the undissolved residue, rinse using record the weight to the nearest 0.1 mg.
and record the weight to the nearest 0.1 70% isopropanol and then filter the un- Transfer to a 250 mL Erlenmeyer flask.
mg. Transfer to a 250 mL Erlenmeyer dissolved residue by suction through a Add 50-150 mL of 4% lithium chloride
flask. Add 50-150 mL of N,N-dimethy- dried, weighed, fritted glass filtering cru- in N,N-dimethylacetamide reagent (100
lacetamide reagent. Agitate for 20 min cible. Dry the crucible and residue in air mL reagent/g of sample). Agitate for 180
keeping the temperature at 70 ± 1°C. De- and then in an oven at 105-110°C to con- min keeping the temperature at 65 ± 1°C.
cant the liquid from the undissolved resi- stant weight. Record the weight of the Decant the liquid from the undissolved
due, add a fresh portion of the N,N- dried residue to the nearest 0.1 mg. residue, add a fresh portion of 4% lithium
dimethylacetamide and agitate for a few 12.10 Method No. 10, Xylene: Weigh chloride and agitate for 5-10 min. Repeat
more minutes. Repeat the decanting and accurately a 0.5-1.5 g of clean, dried, pre- the decanting and agitation process one
agitation process one more time rinsing pared specimen and record the weight to more time rinsing well with 70% isopro-
well with 70% isopropanol, and then fil- the nearest 0.1 mg. Transfer to a 250 mL panol, and then filter the undissolved res-
ter the undissolved residue by suction Erlenmeyer flask. Add 50-150 mL of xy- idue by suction through a dried, weighed
through a dried, weighed fritted glass fil- lenes under a fume hood and cover with a fritted glass filtering crucible. Dry the

84 TM20A-2017 AATCC Technical Manual/2018

Copyright © 2017 American Association of Textile Chemists and Colorists
crucible and residue in air and then in an 14. Microscopical Analysis Procedures from the sample and render them to sta-
oven at 105-110°C to constant weight. ple by removing twist and drawing out fi-
Record the weight of the dried residue to 14.1 Preparation of Slides. bers. Align the fibers parallel to each
the nearest 0.1 mg. 14.1.1 Longitudinal Sections of Vege- other so as to form a well blended tuft.
12.12 Calculations: Calculate the con- table Fibers (cotton, flax, ramie, etc.): A Prepare a slide following the instructions
tent of each generic fiber type as deter- swatch of fabric measuring at least 5 × 5 of TM20, Section 9.3.
mined by any one of the above applicable cm should be available. Count the num-
14.2 Fiber Counting.
chemical methods using one of the fol- ber of yarns in both the warp and filling
and select from each direction at random 14.2.1 Fibers Viewed Through Micro-
lowing equations: scope: Place the slide prepared as in 14.1
12.12.1 If the fiber is dissolved by the a number of yarns that is proportional to
the fabric count. The combined number on the moveable stage on a microscope
test reagent: equipped with a crosshair ocular and hav-
of warp and filling yarns should total at
G–H least 20 (see 17.10). If the sample is in ing a magnification of 200-250X. Begin
X i = ---------------i × 100 to count near either the upper or lower
G yarn form, take at least a two-meter
length and, from it, cut not less than corner of the field and, as the slide is
12.12.2 If the fiber is insoluble in the twenty 5-cm sections at random. Cut ap- moved slowly across the field in the hori-
test reagent: proximately 2.5 cm of each yarn, or yarn zontal direction, identify and count all fi-
H section, into lengths of 0.5-1 mm. The bers passing through the center of the
X i = -----i × 100 shorter the lengths the easier it is to pre- crosshairs. After each trip across the
G field, move the slide 1-2 mm vertically
pare a homogeneous fiber suspension.
where: Collect the cut fibers on a paper of con- and identify and count the fibers as the
Xi = content of fiber i, percent. trasting color and transfer to a 125 mL field is again traversed. Repeat this pro-
G = weight of clean, dry, prepared Erlenmeyer flask. Add sufficient water so cedure until the whole slide has been cov-
specimen that after stoppering the flask and shaking ered. The spacing between each traverse
Hi = weight of dried residue after the contents, a uniform and fairly dense is dependent upon the number of fiber
treatment fiber suspension is obtained. Quick boil- sections on the slide. If a fiber passes the
ing or the addition of a few glass pellets crosshair more than once, record each
13. Microscopical Analysis, General facilitates the separation of the fibers. Us- passing (see 17.11). In a similar manner,
ing a glass-marking pencil, draw two par- count the fibers by moving the slide verti-
13.1 The following procedure may be cally. The combined horizontal and ver-
used for the quantitative analysis of tex- allel lines about 1 in. apart across a glass
slide. With a wide-mouth pipette, draw tical counts should total at least 1000
tiles containing two or more fiber types fibers.
which cannot be separated readily by me- 0.5-1 mL of the well shaken suspension
and place it between the two reference 14.2.2 Projected Images of Fibers: Cal-
chanical or chemical methods. The pro- ibrate the microprojector so that it will
cedures rely on the ability of a technician lines on the slide. The amount of liquid
taken is dependent upon the density of give a magnification of 500X in the plane
to identify and count, by means of a mi- of the projected image. To do this, place
croscope, the relative number of fibers of the suspension. Just sufficient liquid
should be placed on the slide so that—af- a stage micrometer (having units of
each type in a prepared specimen. Such a 0.01 mm) on the stage of the micro-
count will result in a percent blend by ter evaporation—a thin, uniform film of
fibers remains. After all of the moisture projector with its scale toward the objec-
number of fibers. In order to convert this tive and place a large sheet of white, non-
result to a percent by weight, the size of has evaporated from the slide, stain the
fibers with Herzberg stain and cover with glare paper in the projection plane.
the fibers being counted and their respec- Lower or raise the microscope until an
tive densities must be included in the cal- a cover glass.
14.1.2 Longitudinal Sections of Wool, interval of 0.20 mm on the stage micro-
culation. meter will measure 100 mm when
13.2 Microscope slides may be pre- Hair and other round Fibers: Select a rep-
resentative swatch, or yarn sections, as in sharply focused in the center of the paper.
pared to scan longitudinal or cross-section Place the slide prepared as in 14.1 on the
views of a fiber sample. The fiber images 14.1.1. With a fabric swatch, remove the
outermost yarns in both directions so that stage of the microprojector with the cover
may be viewed either through a micro- glass toward the objective. Draw a 10-cm
scope or as projected onto a horizontal the warp and filling yarns are protruding
approximately 1 cm. Lay the sample flat diameter circle in the center of the white
plane. While either viewing method may paper in the projection plane. All mea-
be used for identification and counting of on a table and, using a fiber cutter, force
the blades vertically downward into the surements and counts are to be made
fibers, the projection method is specifi- within this circle. Begin to count near
cally used for measuring fiber diameters warp fringe. Repeat the operation with
the filling fringe. Remove the device with either the upper or lower corner of the
using a wedge scale (see 14.3.2). field and proceed exactly as described in
13.3 Methods which may be used to the top plate up, release the tension on the
cutting blades and remove them together 14.2.1 (see 17.12).
identify fibers during the fiber counting
procedures are discussed in TM20, Fiber by their ends between the thumb and 14.2.3 Video Imaging of Fibers: Using
Analysis: Qualitative. They include the forefinger. Carefully separate the blades a video monitor with a crosshair placed in
following: so that the cut fiber sections will adhere the center of the screen coupled to a
to the edge of one or both blades. Place a video camera attached to a correctly ad-
AATCC 20 few drops of mineral oil on a clean slide justed transmitted light microscope scan
Herzberg stain (zinc chloro- Section 9.9.1 and, with a dissecting needle, scrape the the slide as outlined in 14.2.1.
iodide) fiber sections onto the oil. Thoroughly 14.3 Fiber Measurement.
Acid phloroglucinol reagent Section 9.9.2 disperse the fibers in the oil with the dis- 14.3.1 Fibers with Noncircular Cross-
Longitudinal appearance Tables I and II secting needle and cover with a cover Sections:
Cross-section appearance Tables I and II and
Appendix I
glass. For yarn samples, align the sec- 14.3.1.1 Paper Tracing Method: Pre-
tions side-by-side and perform the above pare a slide as described in 14.1.3. Place
It is recommended that reference tests operation starting with the use of the fiber this slide on the stage of the microprojec-
be made on known fibers rather than plac- cutter. tor and project the image onto a sheet of
ing total reliance on photographic repro- 14.1.3 Cross-Sections of Fibers: Select graph paper having one millimeter
ductions and word descriptions of colors. representative yarns, or yarn sections, squares. Trace the image of the fibers on

AATCC Technical Manual/2018 TM20A-2017 85

Copyright © 2017 American Association of Textile Chemists and Colorists
the graph paper using a sharpened pencil, scribed above using another tuft of fibers. fiber type. Final values should be in µm2
taking care not to retrace fibers previ- Continue to trace and count on the new (see 17.13). Considerable variation can
ously traced. If there are not sufficient fi- slide until 100 fibers of each type have occur in the average diameter of hair and
bers on the slide to provide 100 of each been tallied. Calculate the mean cross-sec- wool fibers. Thus, for accurate results on
type, prepare another slide as described tional area automatically using the statisti- any specific sample, the fiber diameters
above using another tuft of fibers. Con- cal functions of the digital image analysis must be measured. If, however, maximum
tinue to trace and to count on the new software. Final values should be in µm2. accuracy is not required, the diameters
slide until 100 fibers of each type have 14.3.2 Fibers with Circular Cross- given in Tables III and IV may be used.
been tallied. By counting squares, and Sections: Prepare a slide as described in 14.3.2.2 Measurement with Digital Im-
parts of squares, determine the cross- 14.1.2. Be sure to make measurements on age Analysis Software: Using a correctly
sectional area of each individual fiber of the same day that the slide was prepared. calibrated image analysis system measure
each type. Calculate the mean cross- Position the slide in the microprojector or the diameter of the individual fibers in
sectional area for each fiber type present microscope so that all areas of the slide question.
by summing the individual values re- can be reached. 14.4 Calculations. Calculate the content
corded for that type and dividing the sum 14.3.2.1 Measurement with Wedge of each fiber as percent by weight using
by the total number of fibers of that type Scale and Microprojector: Bring each in- equation 1 if 14.3.1 was used to determine
measured. Final values should be in mm2. dividual fiber being measured into sharp average area of fiber cross-section images,
14.3.1.2 Digital Tracing Method: Pre- focus on the wedge scale. Adjust the posi- and equation 2 if section 14.3.2 was used
pare a slide as described in 14.1.3. Place tion of the scale until the fiber image is to determine fiber diameters (see 17.14).
this slide on the stage and adjust until a projected on the wedge with a fine line Ni × Ai × Si
clear well formed image appears on the and mark on the wedge the point that cor- X i = -------------------------------
- (1)
video monitor. Use of a 50X objective responds to the width of the fiber midway Σ( N × A × S)
with C mount video camera coupling has of its length. Traverse the slide and mea-
been found acceptable for most fiber types. sure successive fibers of each type follow- N i × D2i π/4 × S i
X i = ------------------------------------------
- (2)
Using correctly calibrated image analysis ing a planned course. Measure fibers only Σ ( N × D π/4 × S )
2

software and a digital image capture board when their midpoint falls within the 10-
digitally capture the cross-sectional image. cm circle central located in the field. Ex- where:
Using a mouse or stylus trace around the clude from measurement those fibers that Xi is content of fiber i, percent (by
captured cross-sectional images. Use the cross another fiber at the point of mea- weight)
image analysis software to store the result- surement and those that are shorter than Ni is relative number of fibers of type i
ant cross-sectional areas. If there are not 150 µm. A minimum of 100 fibers of each Ai is average area of fiber images of
sufficient fibers on the slide to provide 100 type present should be measured. Calcu- fiber i
of each type, prepare another slide as de- late the mean cross-sectional area of each D2i is the mean of diameter squared of
fibers of type i
2
D π/4 is the mean cross-sectional
area of round cross-section fibers
Table III—Comparative Scale for Fineness of Various Textile Fibers in Micrometers (µm) of type i
Si is specific gravity of type i fiber
IWTO Super Fine Wools Grades
Σ(Ni × Ai × Si) is sum of the respective
‘X’ Value Average Fineness µ ‘X’ Value Average Fineness µ N × A × S products for each fiber
Super 80’s 19.5 ± 0.25 Super 150’s 16.0 ± 0.25 type in the blend
Super 90’s 19.0 ± 0.25 Super 160’s 15.5 ± 0.25 Σ(N × D2i π/4 × S) is sum of the re-
Super 100’s 18.5 ± 0.25 Super 170’s 15.0 ± 0.25 spective N × D2i π/4 × S products
Super 110’s 18.0 ± 0.25 Super 180’s 14.5 ± 0.25 for each fiber type in the blend
Super 120’s 17.5 ± 0.25 Super 190’s 14.0 ± 0.25 See Table V for specific gravity values.
Super 130’s 17.0 ± 0.25 Super 200’s 13.5 ± 0.25
Super 140’s 16.5 ± 0.25 Super 210’s 13.0 ± 0.25 15. Report
15.1 Report the percentage fiber con-
tent by weight of the sample analyzed.
State if nonfibrous content has been re-
moved or if results are based on other
than oven-dry weights.

16. Precision and Bias

16.1 A chemical separation interlabora-
tory test was conducted using a PET/
Wool intimate blend fabric with a nomi-
nal fiber content of 55% PET/45% Wool
according to the fabric manufacturer,
with results as noted in Tables VI and
VII.
16.1.1 Between Laboratories
Standard Deviation = 0.6305 =
0.7940% polyester
Precision: ± t.975(6df)×S = 2.45 ×
0.7940% = ± 1.9454% polyester

86 TM20A-2017 AATCC Technical Manual/2018

Copyright © 2017 American Association of Textile Chemists and Colorists
 Table IV—Fineness Ranges and Fiber Diameters of Various Textile Fibersa Table V
in Micrometers (µm)
Fiber Specific Gravity
U.S. Wool Classification Acetate 1.31
Wool Grades Wool Top Grades Pulled Wool Acrylic 1.16-1.22
Cotton 1.55
Numerical Average Blood Numerical Average Hair 1.32
System Diameter Systemc System Diameterd Grades Hemp 1.48
80s 17.7-19.1 Fine 80s 18.1-19.5 AA Linen 1.50
70s 19.2-20.5 Fine 70s 19.6-21.0 AA Modacrylic 1.28-1.38
64s 20.6-22.0 Fine 64s 21.1-22.5 AA Nylon 1.14
62s 22.1-23.4 ½ 62s 22.6-24.0 A Olefin 0.93
60s 23.5-24.9 ½ 60s 24.1-25.5 A Polyester 1.23-1.40
58s 25.0-26.4 3
/8 58s 25.6-27.0 A Polybenzimidazole 1.40
Ramie 1.51
56s 26.5-27.8 3
/8 56s 27.1-28.5 B
Rayon 1.52
54s 27.9-29.3 ¼ 54s 28.6-30.0 B Silk 1.25
50s 29.4-30.9 ¼ 50s 30.1-31.7 B Spandex 1.0-1.2
48s 31.0-32.6 ¼ 48s 31.8-33.4 B Wool 1.31
46s 32.7-34.3 Low ¼ 46s 33.5-35.1 C
44s 34.4-36.1 Common 44s 35.2-37.0 C In the case of a fiber with a range of values,
40s 36.2-38.0 Braid 40s 37.1-38.9 C knowledge of the specific type in the generic class
36s 38.1-40.2 Braid 36s 39.0-41.2 C may permit the selection of a precise specific gravity;
Hair Fibers and Silk or the density of a fiber may be determined using the
procedure described in TM20, Section 9.6.
Mohair (1) Miscellaneous Hair Fibers (1) Silk (1)
Fineness Average Average
Grade Range Fiber Fineness Fiber Fineness
40s 23.55-25.54 Vicuna 13.0-14.0 Cultivated silk 10.0-13.0 16.1.2 Between Operators within
36s 25.55-27.54 Cashmere 14.0-19.0 Tussah silk 00.0-28.5 Laboratories.
32s 27.55-29.54 Camel hair 17.0-23.0 Standard deviation = 0.0655 =
30s 29.55-31.54 Alpaca 26.0-28.0
28s 31.55-33.54 Llama 20.0-27.0
0.2559% polyester
26s 33.55-35.54 Precision: ± t.975(6df)×S = 2.45 ×
22s 35.55-38.04 0.2559% = ± 0.627% polyester
18s 38.05-40.54 16.2 Interpretation. The above statis-
Vegetable Fiber (1) Glass Fiber (2) tics apply to the PET/Wool fabric tested
Filament Staple Fiber which may represent a best case scenario
Average Diameter Theoretical Diameter Average for the determination of fiber content by
Fiber Fineness Designation Diameter Designation Diameter chemical separation. Additional studies
Cotton 16.0-21.0 D 5.3 E 7.1 are underway in conjunction with Com-
Flax (linen) 15.0-17.0 E 7.4 G 9.7 mittee RA102, Statistics Advisory, in-
Jute 15.0-20.0 G 9.0 J 11.4 volving different blend levels.
Hemp 18.0-23.0 16.3 Bias. The quantitative fiber analy-
Kapok 21.0-30.0 sis can only be defined in terms of a test
Ramie 25.0-30.0 method. There is no independent method
Theoretical Fiber Diameterd for determining the true value. As a
means of estimating this property, the
Rayon (3), Acetate (3), Nylon (4), and Vinyon (3) Casein Fiber (5)
method has no known bias.
Filament Viscose Acetate and Fiber
Denier Rayon Vinyon Nylon Grade Denier Diameter
17. Notes
1 9.6 10.3 11.1 70s 3 20
2 13.6 14.5 15.7 60s 5 25 17.1 Applicable only to Nylon 6 and Nylon
3 16.7 17.8 19.3 50s 7 30 6,6.
4 19.3 20.6 22.3 17.2 Available from Publications Office,
5 21.6 23.0 24.9 ACGIH, Kemper Woods Center, 1330 Kemper
6 23.6 25.2 27.3 Meadow Dr., Cincinnati OH 45240; tel: +1.
7 25.5 27.3 29.5 513.742.2020; web site: www.acgih.org.
8 27.3 29.1 31.5 17.3 Since sodium hypochlorite solutions
9 28.9 30.9 33.4 lose strength on standing, it is recommended
10 30.5 32.6 35.2 that they be standardized frequently. The fol-
12 33.4 35.7 38.5 lowing is a suitable method for determining
14 36.1 38.5 41.7 the available chlorine content of such solu-
16 38.6 41.2 44.5 tions: Dilute a 10 mL aliquot of the solution to
18 40.9 43.7 47.3 be tested to 250 mL with water in a volumetric
20 43.1 46.1 49.9 flask. Pipette 25 mL from the volumetric flask
a
Source of Data: to an Erlenmeyer flask; add 3-5 mL of a 10%
(1) Werner von Bergen and W. Krauss, Textile Fiber Atlas, Textile Book Publishers Inc., New York NY (1949). solution of potassium iodide (KI) and then add
(2) Owens-Corning Fiberglas Corp. 2-3 mL acetic acid (CH3COOH). Mix well
(3) American Viscose Corp. and titrate with 0.1N sodium thiosulfate
(4) E. I. du Pont de Nemours and Co. (Na2S2O3) until the yellow color of the iodine
(5) Aralac Incorporated. is nearly destroyed. Add 5 mL of a starch indi-
c
Trade application. cator solution and titrate until the blue color
d
U.S. Standards, Federal Register, January 13, 1954; Specifications for Fineness of Wool Tops and Assignment entirely disappears. Calculate the percentage
of Grade (ASTM Designation: D3992). of available chlorine by weight as follows:

AATCC Technical Manual/2018 TM20A-2017 87

Copyright © 2017 American Association of Textile Chemists and Colorists
 Table VI—Nested Factorial Design (Polyester %)
Laboratory A B C D E
Operator 1 2 3 4 5 6 7 8 9 10
58.00 57.57 58.60 58.00 57.95 58.27 58.35 59.88 58.30 57.78
58.09 57.65 58.00 57.70
58.04 57.60
Totals 174.13 172.82 116.60 115.70 57.95 58.27 58.35 59.88 58.30 57.78

Table VII—ANOVA fabric or yarn in the form of fiber bundles.

Most bundles are reduced to single fibers dur-
Degrees of Sum of Mean ing the preparation of the fiber suspension. If,
Freedom (df) Squares Square F Ratio however, some bundles do appear on the slide,
an attempt should be made to count each of
Between Laboratories 4 2.5221 0.6305 2.161 the individual fibers in the bundle.
Between Operators 17.12 A regular microscope may be used
5 0.3275 0.0655 0.224 for the fiber counting and, if a suitable cali-
within Laboratories
brating device is available, it may also be used
Residual (or error) 6 1.7501 0.2917 — for measuring fiber diameters.
Totals 15 4.5997 17.13 For further information on marking
cell numbers on a wedge scale, and for exam-
ples of calculations of how to determine the
average fiber diameter using cell numbers, see
100 aJ
Corrected cotton, % = ----------------- – 1.6 ASTM D2130, Method of Test for Diameter
F of Wool and Other Animal Fibers by Micro-
where: projection.
for raw cotton, a is 1.062 17.14 One is cautioned not to mix units;
for bleached cotton, a is 1.046 e.g., if some fiber diameters have been deter-
J is the oven-dry residue weight mined in µm, then all diameters must be in µm.
F is the oven-dry weight of clean fiber For ease of calculation, the terms D 2i and D2
before treatment. may be used in place of D 2i π/4 and D2 π/4
Corrected Regenerated Cellulose Rayon, respectively. If this is done one cannot use
both cross-sectional areas and squared diame-
% = 100 – corrected cotton percent. ters in the same equation.
17.7.2 Linen is not completely insoluble in 17.15 Any extractor capable of heating the
Fig. 1—Gelled Lyocell in left beaker; H2SO4 (59.5%). Furthermore, a small amount sample in the solvent up to 150°C while pres-
Dissolved Viscose in right beaker. of rayon remains undissolved in this solvent. surizing up to 2000 may be used. Solvent in
In addition, some types of rayon, like lyocell, use must have an auto ignition of higher than
may gel instead of dissolve in 59.5% sulfuric 200°C. The accelerated solvent extractor
Available Chlorine, % = 3.5A/B acid (see Fig. 1). In the analysis of linen/rayon (ASE) has been found to be an acceptable al-
blends, interlaboratory tests indicate that to al- ternative to Soxhlet extractor.
where: low for the above bias, the composition of the 17.16 The flask covers (reflux caps) can be
A = mL of 0.1N sodium thiosulfate used specimen should be calculated as follows: purchased from Fisher Scientific Company,
B = g of 10 mL aliquot taken Part #10-042.
100 aJ
Corrected linen, % = ----------------- – 1.6
17.4 Exception: when the pattern is smaller F
than 15 × 15 cm, a sufficient number of com- where: 18. References
plete patterns should be taken to be equivalent for undyed linen, a is 1.084
to not less than 225 cm2. for dyed linen, a is 1.105 18.1 ASTM D276, Standard Test Methods
17.5 Whenever there is any doubt about the J is the oven-dry residue weight for Identification of Fibers in Textiles.
effectiveness of a given method in dissolving F is the oven-dry weight of clean fiber 18.2 ASTM D629, Standard Test Methods
a specific fiber, or whenever there is an appli- before treatment. for Quantitative Analysis of Textiles.
cation of a method to a new type of fiber, one 18.3 ASTM D1776, Standard Practice for
should always examine the residue in the fil- Corrected Regenerated Cellulose Rayon,
Conditioning and Testing Textiles.
tering crucible after weighing. This precaution % = 100 – corrected linen percent. 18.4 ASTM D1909, Standard Table of
should always be taken when a fiber blend Commercial Moisture Regains for Textile
consists of (1) one predominate fiber with one 17.7.3 Some dyeing and finishing processes
Fibers.
(or more) minor components; or (2) one very may increase the variability and decrease the
minor fiber with one (or more) major com- accuracy of chemical separation using 59.5% 18.5 ASTM D2130, Method of Test for
ponents. H2SO4 to determine the percent fiber content Diameter of Wool and Other Animal Fibers
17.6 If a mechanical shaking machine is by weight of cellulosic blends. by Microprojection.
available, the flask may be shaken on it con- 17.8 Extreme care must be taken to control 18.6 ASTM D4920, Standard Terminology
tinuously for 30 min. both time of exposure to the reagent and the Relating to Moisture in Textiles.
17.7.1 Cotton is not completely insoluble in temperature of treatment. If either is insuffi- 18.7 Available from ASTM International,
H2SO4 (59.5%). Furthermore, a small amount cient, the desired fiber or fibers, will not be 100 Barr Harbor Dr., W. Conshohocken PA
of rayon remains undissolved in this solvent. completely dissolved. If either becomes ex- 19428; tel: +1.610. 832.9500; fax: +1.610.832.
In addition, some types of rayon, like lyocell, cessive, it will cause attack of other fibers. 9555; web site: www.astm.org.
may gel instead of dissolve in 59.5% sulfuric 17.9 A mechanical shaking machine may 18.8 IWTO Draft Test Method 58-97,
acid (see Fig. 1). In the analysis of cotton/ be used for this purpose. “Quantitative Analysis of Blends of Wool
rayon blends, interlaboratory tests indicate 17.10 For fancy woven fabrics, use all the with Specialty Fibers by Scanning Electron
that to allow for the above bias, the composi- yarns in one or more complete patterns or a Microscope.” Describes method for distin-
tion of the specimen should be calculated as representative fraction, if the pattern is large. guishing between specialty animal fibers and
follows: 17.11 Linen fibers may be present in the wool and provides numerous references.

88 TM20A-2017 AATCC Technical Manual/2018

Copyright © 2017 American Association of Textile Chemists and Colorists