AATCC TM20A-2021

Test Method for Fiber Analysis: Quantitative

1. Purpose and Scope dard Table of Commercial Moisture Re- for information purposes only. The pre-
gains for Textile Fibers, can be used for cautions are ancillary to the testing proce-
1.1 This method presents individual this purpose. dures and are not intended to be all inclu-
procedures for the quantitative determi- 2.3 The procedure for determining fi- sive. It is the user’s responsibility to use
nation of moisture content, nonfibrous ber composition by mechanical separa- safe and proper techniques in handling
content and fiber composition of textiles. tion is applicable to those textiles materials in this test method. Manufac-
1.2 The procedures for the determina- wherein the different fibers making up its turers MUST be consulted for specific
tion of fiber composition include me- composition are segregated in separate details such as material safety data sheets
chanical, chemical and microscopical yarns, or plies, in the textile product. and other manufacturer’s recommenda-
methods. They are applicable to blends of 2.4 The chemical procedures for fiber tions. All OSHA standards and rules
the following generic classes: composition described herein are applica- must also be consulted and followed.
ble to most of the current, commercial 4.1 Good laboratory practices should
Natural Fibers Man-Made Fibers production fibers within each generic be followed. Wear safety glasses in all
Cotton Acetate class listed. Known exceptions are noted laboratory areas.
Hair Acrylic in Table II. However, there may be in- 4.2 All chemicals should be handled
Hemp Aramid (see 17.17) stances in which a method may not be with care.
Linen meta-aramid fully adequate for a newly developed fi- 4.3 Perform the soxhlet extractions in
Ramie para-aramid ber falling within one of the listed generic Section 9, Nonfibrous Material—Clean
Silk Modacrylic classes and for re-used and/or physically Fiber Content, using hexane and ethyl al-
Wool Nylon (see 17.1) or chemically modified fibers. Caution cohol inside an adequately ventilated lab-
Olefin should be exercised when applying these oratory hood. CAUTION: Hexane and
Polybenzimidazole (see 17.17) methods to such cases. ethyl alcohol are highly flammable.
Polyester 2.5 The microscopical procedures for fi- 4.4 Perform Chemical Analysis Proce-
Rayon ber composition are applicable to all fibers dure No. 1 (Table II, 100% acetone) in-
Spandex and their accuracy depends to a consider- side a ventilated laboratory hood. CAU-
Triexta able extent upon the ability of the analyst TION: Acetone is highly flammable.
to identify the individual fibers present. 4.5 Hexane, ethyl alcohol and acetone
2. Uses and Limitations However, owing to the tedious nature of are flammable liquids and should be
this technique, its use is generally limited stored in the laboratory only in small
2.1 The procedure given for the removal to those mixtures which cannot be sepa- quantities away from heat, open flame
of nonfibrous materials will remove most, rated mechanically or chemically; e.g., and sparks.
but not all, of these components. Each mixtures of hair and wool and mixtures of 4.6 In preparing, dispensing, and han-
treatment is applicable only to certain cat- cotton, linen, hemp and/or ramie. dling hydrochloric acid (20%), sulfuric
egories of these substances and no general acids (59.5% and 70%), and formic acid
scheme can be given that is all inclusive. (90%) used in Chemical Analysis Proce-
2.1.1 Some of the newer finishes may 3. Terminology
dure Methods No. 2, 3, 4, and 6 (Table
present special problems and the analyst 3.1 clean-fiber content, n.—the amount II), use chemical goggles or face shield,
will have to deal with these cases as they of fiber after removal of nonfibrous impervious gloves and an impervious
arise. Thermosetting resins and crosslink- content. apron. Concentrated acids should be han-
ing latices are not only difficult to re- 3.2 fiber, n.—in textiles, a generic dled only in an adequately ventilated lab-
move but in some cases cannot be wholly term for any one of the various types of oratory hood. CAUTION: Always add
removed without destroying the fiber. matter that form the basic elements of a acid to water.
2.1.2 When it is necessary to modify a textile and which are generally character- 4.7 In preparing ammonium hydroxide
procedure, or use a new one, one should ized by flexibility, fineness and high ratio (8:92) for use in Chemical Analysis Pro-
make sure that the fibrous portion of the of length to thickness. cedure Method No. 4 (Table II, 70% sul-
specimen under test is not attacked. 3.3 moisture content, n.—that part of furic acid), use chemical goggles or face
2.2 Fiber composition is generally ex- the total mass of a material that is ab- shield, impervious gloves and an imper-
pressed in the laboratory either on the sorbed or adsorbed water, compared to vious apron. Dispense, mix and handle
oven-dry weight of the textile as received the total mass. ammonium hydroxide only in an ade-
or on the oven-dry weight of the clean fi- 3.4 nonfibrous content, n.—products quately ventilated laboratory hood.
ber after nonfibrous materials are first re- such as fiber finishes, yarn lubricants, 4.8 An eyewash/safety shower should
moved from the textile before the fiber slasher sizing, fabric softeners, starches, be located nearby and a self-contained
analysis is carried out, or if the treatments china-clay, soaps, waxes, oils and resins breathing apparatus should be readily
described in Section 9 are incapable of re- which are applied to fiber, yarn, fabric or available for emergency use.
moving them, any such materials present apparel. 4.9 Exposure to chemicals used in this
will increase the percentage of the fiber 3.5 Additional terms used in this test procedure must be controlled at or below
constituent with which they are removed method can be found in standard chemi- levels set by governmental authorities
during the analysis. cal dictionaries, in dictionaries of com- (e.g., Occupational Safety and Health
When used in commerce for the repre- mon terms or in AATCC M11. Administration’s [OSHA] permissible
sentation of the nominal fiber content of exposure limits [PEL] as found in 29
end use items such as garments, moisture 4. Safety Precautions CFR 1910.1000; see web site: www.
regain is typically added back to bone dry osha.gov for latest version). In addition,
numbers generated. ASTM D1909, Stan- NOTE: These safety precautions are the American Conference of Govern-

84 AATCC TM20A-2021 AATCC Manual of International Test Methods and Procedures/2022

Copyright © 2021 American Association of Textile Chemists and Colorists
mental Industrial Hygienists (AC-GIH) 6. Reagents 6.15 Isopropanol (C3H7)HO (70%)
Threshold Limit Values (TLVs) com- 6.16 N,N-Dimethylacetamide
prised of time weighted averages (TLV- 6.1 Ethyl alcohol (95%), pure or dena- CH3C(O)N(CH3)2
TWA), short term exposure limits (TLV- tured. 6.17 Methanol (CH3OH), reagent grade.
STEL) and ceiling limits (TLV-C) are 6.2 Hexane (C6H14). 6.18 Sodium Hydroxide (NaOH), pellet,
recommended as a general guide for air 6.3 Hydrochloric acid (HCl), 0.1N. 95% reagent grade.
contaminant exposure which should be 6.4 Enzyme solubilizing preparation. 6.19 Xylenes (C6H4(CH3)2), mixed, 95%
met (see 17.2). 6.5 Acetone (CH3COCH3), reagent reagent grade.
grade. 6.20 Lithium Chloride (LiCl), crystal
5. Apparatus 6.6 Hydrochloric acid (HCl) (20%). reagent grade.
Dilute HCl, sp gr 1.19, with water until 6.21 Epoxy release agent for use with
5.1 Analytical balance, capable of the specific gravity of the solution is 1.10 castable mounting materials.
weighing to 0.1 mg. at 20°C. 6.22 Epoxy resin suitable for creating
5.2 Oven, maintained at 105-110°C. 6.7 Sulfuric acid (H2SO4) (59.5%). castable mounts.
5.3 Desiccator, containing anhydrous Add H2SO4, sp gr 1.84, slowly to water. 6.23 Epoxy hardener compatible with
silica gel, calcium sulfate (such as Drie- After the solution has cooled to 20°C, ad- the selected epoxy resin.
ite) or its equivalent. just the density to a value between 1.4902 6.24 Cyclohexanone (CH2)5CO.
5.4 Soxhlet extractor, 200 mL capac- and 1.4956 g/mL.
ity. 6.8 Sulfuric acid (H2SO4) (70%). Add 7. Sampling
5.5 Constant temperature bath, adjust- H2SO4, sp gr 1.84, slowly to water. After
able, capable of controlling temperature the solution has cooled to 20 ± 1°C, ad- 7.1 It is not possible to give specific in-
to ± 1°C. just the density to a value between 1.5989 structions for taking a laboratory test
5.6 Weighing bottle, 100 mL capacity, and 1.6221 g/mL. sample from all types of textile materials
glass, with ground glass cover. (Alter- 6.9 Sulfuric acid (H2SO4) (1:19). to which these methods may be applica-
nate: aluminum weighing can; same size, Slowly stir 1 volume of H2SO4, sp gr ble; but a few general recommendations
tight cover.) 1.84, into 19 volumes of water. will be given.
5.7 Erlenmeyer flask, 250 mL capac- 6.10 Sodium hypochlorite (NaOCl). 7.1.1 The sample should be as repre-
ity, ground glass stopper. Prepare a solution of NaOCl, 5.25% sentative as possible of the lot of material
5.8 Beaker, borosilicate heat resistant available chlorine. Sodium hypochlorite from which it was taken.
glass, 250 mL capacity. based household bleach (nominally 7.1.2 If a reasonably large lot is avail-
5.9 Filtering crucible, fritted glass, 5.25%) has been found to be acceptable. able, and if it is possible to do so, sam-
coarse porosity, 30 mL. 6.11 Sodium bisulfite (NaHSO3) (1%). plings should be taken from different,
Freshly prepared. widely separated areas or parts of the lot.
5.10 Suction flask, with adapter, to 7.1.3 In the case of fabrics where there
hold filtering crucible. 6.12 Formic acid (HCOOH) (90%), sp
gr of 1.202 at 20°C. is a definite repetition in the pattern, the
5.11 Weighing bottle, large enough to sample should include all yarns in a com-
hold filtering crucible. 6.13 Ammonium hydroxide (NH4OH)
(8:92). Mix 8 volumes of NH4OH, sp gr plete pattern (see 17.4).
5.12 Microscope, equipped with a 7.1.4 In the case of yarns, not less than
moveable stage and a cross-hair ocular, 0.90, with 92 volumes of water.
6.14 Herzberg stain. Add the previ- a 2-meter length should be taken.
200-250× magnification.
5.13 Projection microscope, capable of ously prepared solution A to solution B;
500× magnification. allow to stand overnight; decant the clear
Test Methods
liquid into a dark colored glass bottle and
5.14 Fiber cutter: A device comprised add a leaf of iodine.
of two razor blades, a threaded pin and 8. Moisture Content
an assemblage that will hold the blades
rigidly in position. The device is operated Solution A Solution B 8.1 Procedure. Place not less than 1 g
by applying pressure vertically down- Zinc Chloride 50 g Potassium of the textile to be tested in a previously
ward. It cuts fibers approximately 250 µm Iodide 5.5 g tared weighing bottle and immediately
in length. Water 25 mL Iodine 0.25 g replace the cover. Weigh to the nearest
5.15 Wedge scale: Strips of heavy pa- Water 12.5 mL 0.1 mg using the analytical balance and
per or Bristol board imprinted with a record the weight. Place the uncovered
wedge for use at 500× magnification. weighing bottle containing the specimen
5.16 Flask cover (see 17.16). in an oven maintained at 105-110°C for
5.17 Wet grinder/polisher equipped 1.5 h. At the end of the time period, re-
44.50 mm
move the bottle from the oven, immedi-
12.70 mm

with 10 in platen for use with 10-in. abra-

sive discs. ately replace the cover and put it in the
desiccator. When the bottle and contents
5.18 Adhesive-backed abrasive discs,
have cooled to room temperature, remove
10-in. (grit: 120, 240, 320, 400, 600, 800,
6.35 mm them from the desiccator and reweigh.
1200).
19.00 × Repeat the heating and reweighing pro-
5.19 1-gallon vacuum chamber with cess for periods of 30 min until the
pump capable of maintaining vacuum 19.00 mm
25.40 mm

weight is constant to within ± 0.001 g and

pressure of at least 25 in-Hg. record the constant weight.
5.20 2-piece castable mounting cups, 8.2 Calculations.
1.5 in. 8.2.1 Calculate the moisture content of
5.21 Rigid mounting card: non-absor- the specimen as follows:
bent yarn sample mounting card for use 31.75 mm
with epoxy resin mounting method. See
Fig. 1 for dimensions suitable for 1.5-in. A–B
Fig. 1—Rigid Mounting Card M = ------------- × 100
sample cups. (all tolerances are ±0.38 mm). A–T

AATCC Manual of International Test Methods and Procedures/2022 AATCC TM20A-2021 85

Copyright © 2021 American Association of Textile Chemists and Colorists
where: D = dry weight, specimen, after treat- the box under the column listing the other
M = moisture content, percent. ment. component and the number therein is the
A = weight of sample before drying + method, or methods, that are applicable
bottle. 9.2.2 Calculate the clean fiber content for that specific combination. The un-
B = weight of sample after drying + of the specimen as follows: bracketed methods are those that dissolve
bottle. the fiber at the left side of the diagram
T = tare weight of weighing bottle. D while the bracketed ones dissolve the fi-
F = ---- × 100 ber at the top of the diagram. Mixtures of
C
9. Nonfibrous Material—Clean Fiber more than two components may be ana-
Content where: lyzed by proper application of a sequence
F = clean fiber content, percent; other of the individual methods. Table II pre-
9.1 Procedure. Take a specimen of not terms as in 9.2.1 sents the relative solubilities of the vari-
less than 5 g, dry it to constant weight in ous fibers in all the reagents and, from
an oven at 105-110°C (see 8.1), record 9.2.3 Additional techniques for the ex- this, one can select the proper methods
the oven-dry weight to the nearest 0.1 mg traction and analysis of textile finishes can and their sequence for the analysis of
using an analytical balance and then sub- be found in AATCC TM94, Test Method multifiber mixtures (see 17.5).
ject it to one, or more, of the following for Finishes in Textiles: Identification.
treatments, as appropriate. When specific
12. Chemical Analysis Procedures
type of nonfibrous content is known, only 10. Mechanical Separation
that specific treatment, or treatments, 12.1 Method No. 1, 100% Acetone:
need be performed; otherwise, all treat- 10.1 Procedure. Remove the non-
Weigh accurately a 0.5-1.5 g portion of
ments must be applied. fibrous materials using the appropriate
treatment (see 9.1). Separate the compo- the clean, dry, prepared specimen and
9.1.1 Hexane Treatment (for removal record the weight to the nearest 0.1 mg.
of oils, fats, waxes, etc.). Extract the nent yarns by mechanical dissection;
Transfer into a 250 mL Erlenmeyer flask.
dried specimen with hexane in a soxhlet combine those yarns, or plies, having the
same fiber composition and determine Add 100 times its weight of acetone and
extractor, siphoning over a minimum of agitate vigorously for 15 min keeping the
six times. Air dry, and then dry at 105- the oven-dry weight of each generic type
temperature at 40-50°C. Decant the liq-
110°C to constant weight. For an alterna- present.
uid from the undissolved residue, add a
tive to soxhlet extractor, see 17.15. 10.2 Calculation. Calculate the content
fresh portion of acetone and agitate for a
9.1.2 Alcohol Treatment (for removal of each generic fiber as follows:
few more minutes. Repeat the decanting
of soaps, cationic finishes, etc.). Extract and agitation process one more time and
the dried specimen with ethyl alcohol in a W then filter the undissolved residue by suc-
soxhlet extractor, siphoning over a mini- X i = ------i × 100
E tion through a dried weighed, fritted-
mum of six times. Air dry, and then dry at glass, filtering crucible. Dry the crucible
105-110°C to constant weight. For an al- and residue in air and then in an oven at
ternative to soxhlet extractor, see 17.15. where:
Xi = content of fiber i, percent. 105-110°C to constant weight. Record
9.1.3 Aqueous Treatment (for removal the weight of the dried residue to the
of water soluble materials). Immerse the Wi = oven-dry weight of fiber i, after
separation. nearest 0.1 mg.
dried specimen for 30 min in water at 50°C
using a 100:1 liquid to fabric ratio. Stir E = weight of clean, oven-dry speci- 12.2 Method No. 2, 20% Hydrochloric
occasionally or use a mechanical shaker. men taken for analysis. acid: Weigh accurately a 0.5-1.5 g por-
Rinse 3 times in fresh portions of water tion of the clean, dry, prepared specimen
and dry at 105-110°C to constant weight. 11. Chemical Analysis—General and record the weight to the nearest 0.1
9.1.4 Enzyme Treatment (for removal mg. Transfer into a 250 mL Erlenmeyer
of starch, etc.). Immerse the dried speci- 11.1 Specimen Preparation. Before flask. Add 50-150 mL of 20% hydrochlo-
men in aqueous solution of the enzyme analyses are undertaken, the laboratory ric acid (100 mL reagent/g of sample);
preparation following the manufacturer’s test sample should be disintegrated, ho- shake vigorously and let stand for 5 min
recommendations as to concentration, mogenized and a portion of the homoge- at 15-25°C. Shake again and let stand for
liquid to fabric ratio and temperature and nate taken for the chemical treatment(s). 15 min. Shake for a third time (see 17.6)
time of immersion. Rinse thoroughly In the case of a fabric, one should un- and filter the mixture through a dried
with hot water and dry at 105-110°C to ravel it into its individual yarns, cut the weighed fritted-glass crucible. Wash into
constant weight. yarns into lengths not greater than 3 mm, the crucible any residue left in the flask
9.1.5 Acid Treatment (for removal of thoroughly mix the cut pieces and then using a little more 20% hydrochloric
amino resins). Immerse the dried speci- take a representative portion for the spe- acid. Apply suction to drain the excess li-
men in 100 times its weight of 0.1N HCl cific determination. An alternate proce- quor from the filter residue. Wash the
at 80°C for 25 min, stirring occasionally. dure, suitable in many cases, is to grind residue in the crucible with about 40 mL
Rinse thoroughly with hot water and dry the sample using a Wiley Mill, homoge- of 20% hydrochloric acid and then with
at 105-110°C to constant weight. nize the ground fibers by slurrying them water until the filtrate is neutral to litmus.
9.2 Calculations. in a water suspension in a Waring Disconnect the suction and add to the
9.2.1 Calculate the nonfibrous content Blender and taking the representative crucible about 25 mL of ammonium hy-
of the specimen as follows: portion from the dried homogenate for droxide (8:92) allowing the fiber residue
the specific determination. Yarns are to soak for 10 min before applying suc-
treated the same way but omitting the un- tion to drain it. Wash the residue with
C–D necessary steps. about 250 mL of water, allowing it to
N = -------------- × 100
C 11.2 Method Application. A tabula- soak in the water for about 15 min. After
tion of appropriate chemical treatments the final washing, apply suction to re-
where: for binary fiber mixtures is given in Table move rinse water, and dry the crucible
N = nonfibrous materials, percent. I. To use this table one enters at the left and residue in an oven at 105-110°C to
C = dry weight, specimen, before side on the line listing one of the compo- constant weight. Record the dry weight to
treatment. nents of the binary mixture and moves to the nearest 0.1 mg.

86 AATCC TM20A-2021 AATCC Manual of International Test Methods and Procedures/2022

Copyright © 2021 American Association of Textile Chemists and Colorists