AATCC Test Method 94-2002
Finishes in Textiles: Identification
Developed in 1959 by AATCC Commit-
tee RR45; revised 1961, 1962, 1965,
1987; reaffirmed 1969, 1973, 1977,
1985, 2002; editorially revised 1974;
editorially revised and reaffirmed 1992,
1997.
1. Purpose and Scope
1.1 This test method gives guidelines
for qualitative identification of various
finish components present on textile fab-
rics, yarns or fibers.
1.2 The identification scheme may in-
volve any or all of the following ap-
proaches:
1.2.1 Sequential solvent extractions
followed by identification of extracts by
infrared spectroscopy (IR), gas chroma-
tography (GC), high performance liquid
chromatography (HPLC), thin layer chro-
matography (TLC), nuclear magnetic res-
onance spectroscopy (NMR) or other in-
strumental or wet-chemical methods.
1.2.2 Direct measure of elemental or
chemical species on fabric by X-ray fluo-
rescence spectroscopy, infrared reflectance
spectroscopy, furnace atomic absorption
spectroscopy, and other instrumental or
wet-chemical analysis methods.
1.2.3 Identification of specific finish-
ing components by chemical spot tests on
the textile or extracts from textiles.
2. Uses and Limitations
2.1 This test method is a flexible set of
guidelines for identification of textile fin-
ishes. Appropriate adjustments and modi-
fications will be needed as finishing
chemicals change and as new analytical
test methods are developed.
2.2 Any chemical which is on the tex-
tile prior to finishing may be present on
the finished fabric and could be removed
and/or detected as finish. Warp sizes,
[e.g., starches, acrylics, waxes, poly-
esters, poly(vinyl alcohol)], dyes, dye fix-
atives, binders, spin finishes, natural
gums, sugars, optical brighteners, and
processing chemicals (e.g., surfactants,
bleach stabilizers, dye carriers, and oils)
may be present by design or unintention-
ally. A working knowledge of these
chemicals is needed to properly detect
and identify them. Where possible, sup-
plier should be consulted for further
information.
3. Terminology
3.1 chemical finish, n.—chemical
material other than colorants and residual
130 TM 94-2002
Copyright © 2005 American Association of Textile Chemists and Colorists
processing chemicals added to textiles to
impart desired functional or aesthetic
properties to the textile product.
NOTE: Chemical finish will hereafter
be referred to as finish.
4. Safety Precautions
NOTE: These safety precautions are
for information purposes only. The pre-
cautions are ancillary to the testing proce-
dures and are not intended to be all inclu-
sive. It is the user’s responsibility to use
safe and proper techniques in handling
materials in this test method. Manufac-
turers MUST be consulted for specific
details such as material safety data sheets
and other manufacturer’s recommenda-
tions. All OSHA standards and rules
must also be consulted and followed.
4.1 Good laboratory practices should
be followed. Wear safety glasses in all
laboratory areas.
4.2 Use chemical goggles or face
shield, impervious gloves and an imper-
vious apron during dispensing and mix-
ing of alkalis, acids and organic solvents.
Concentrated acids should be handled
only in an adequately ventilated labora-
tory hood. CAUTION: Always add acid
to water.
4.3 Special precautions must be ob-
served when using perchloric acid. All
work must be done in an exhaust hood
made of non-combustible material. Fre-
quent wash down of the exhaust system is
recommended as accumulated perchlor-
ate combinations are often explosive. Ad-
dition of dehydrating agents, unless con-
trolled, will lead to the anhydrous acid
which is unstable. Care must be taken in
handling perchloric acid. Use eye and
face protection, and flush any spill or
splash to the skin or eyes with water
immediately.
4.4 Hexane and methanol are flamma-
ble liquids and should be stored in the
laboratory only in small containers away
from heat, open flames and sparks. These
chemicals should not be used near an
open flame.
4.5 Carry out reflux procedure in a
well ventilated hood with an electrical
heater or a water bath as the heating
source. Use chemical goggles or face
shield, impervious gloves and an im-
pervious apron when handling organic
solvents.
4.6 An eyewash/safety shower, organic
vapor respirator and a self-contained
breathing apparatus should be located
nearby for emergency use.
4.7 Care should be taken in handling
hot weighing bottles and crucibles. Se-
vere burns can result from skin contact.
4.8 Manufacturer’s safety recommen-
dations should be followed when operat-
ing laboratory testing equipment.
4.9 Exposure to chemicals used in this
procedure must be controlled at or below
levels set by governmental authorities
[e.g., Occupational Safety and Health
Administration’s (OSHA) permissible
exposure limits (PEL) as found in 29
CFR 1910.1000 of January 1, 1989]. In
addition, the American Conference of
Governmental Industrial Hygienists
(ACGIH) Threshold Limit Values (TLVs)
comprised of time weighted averages
(TLV-TWA), short term exposure limits
(TLV-STEL) and ceiling limits (TLV-C)
are recommended as a general guide for
air contaminant exposure which should
be met (see 14.1).
5. Sample Preparation
5.1 Textile samples should be dried at
105 ± 1°C and desiccated to constant
weight prior to weighing for subsequent
extractions.
6. Solvent Extraction Procedures
6.1 Extraction with different solvents is
intended to remove as many finishing
chemicals as possible in a sequential or-
der. The extraction scheme presented
here (see Table I) was chosen on the basis
of solvent polarity, solubility, volatility,
economy and safety.
6.2 Changes in chemical finishes,
safety considerations or personal prefer-
ences may dictate the use of other sol-
vents. It is the responsibility of the user to
determine which finish types may be re-
moved by different solvents.
6.3 Some finishes may not be soluble
in any solvent. An alternate method for
insoluble finishes such as fully cross-
linked polymers [e.g., some acrylics,
polyurethanes, silicones and poly(vinyl
acetates)] would be to dissolve all of the
fibrous material with a suitable solvent,
leaving the residue of finish for further
analysis (see AATCC Method 20, Fiber
Analysis: Qualitative, Table V).
6.4 Procedure. A weighed textile sam-
ple (1-10 g depending on the size of the
extractor) is extracted in sequence by the
solvents in Table I, using Soxhlet reflux
or beaker extractions depending on
equipment availability. Extraction times
may range from 45 min to several hours
AATCC Technical Manual/2006

Group Solvent
1 Hexane
2 1,1,1-Trichloroethane
3 Methanol
4 Water
5 0.1 N Hydrochloric acid
*Burdick and Jackson
NOTE: Some types of fibers may be partially dissolved by the solvents. Pre-checks on the fiber types (see AATCC
Method 20) should be made to avoid errors.
depending on the boiling point, exchange
rate and knowledge of the history of fin-
ish removal for the textile sample in
question. The samples should be com-
pletely dried before beginning the next
solvent in the sequence. After the extrac-
tions are complete, each solvent is fil-
tered and evaporated or distilled leaving
the residual finish extract. (The extract
may be transferred to a weighing pan
prior to complete dryness; drying can
then be completed in an oven at 105
± 1°C. Calculate the percent extract as
follows:
Extract =
Weight of Residue
100 × --------------------------------------------------------------
Weight of Original Fabric
NOTE: It may be useful to neutralize
the acid extract with dropwise addition of
dilute sodium hydroxide to avoid further
degradation of the finish during evapora-
tion. The quantitative results will reflect
the presence of sodium chloride in the
dried residue. In addition, contamination
of the solution by sodium carbonate from
the reaction of sodium hydroxide with at-
mospheric carbon dioxide may interfere
with interpretation of subsequent infrared
spectra.
The percent extract, coupled with sub-
sequent identification, will be useful in
distinguishing true finish components
from residual non-finishing chemicals
that may have been left on the fabric;
e.g., natural waxes from softeners.
The extracted finish may be identified
by one of the analytical techniques de-
scribed below.
7. Infrared Spectroscopic Procedures
7.1 Infrared spectroscopy offers a very
convenient way to identify extracted fin-
ish from textiles. The basis for infrared
spectroscopy is the structural information
about a compound that can be found from
its infrared spectrum. Infrared absorption
AATCC Technical Manual/2006
Table I
Polarity Index* Typical Finishing Chemicals Removed
0.1 Oils, waxes, softeners, silicones
1.0 Small amounts of unfixed polymers, polyester resins,
acrylics, polyurethanes, poly(vinyl acetates)
5.1 Unfixed cellulose reactants, organic salts, sulfonated
organics
10.2 Unfixed cellulose reactants, urea, linear starches,
poly(vinyl alcohol)
10.2 Fixed cellulose reactants, branched starches,
inorganic salts
bands in the 4000 to 250 wavenumbers
region result from specific functional
groups in a molecule. These can be com-
pared with spectra of finishes in pub-
lished or personal libraries. Visual in-
spection by a trained analyst will quickly
identify the general type of finish. Com-
puterized search-and-match capabilities
on many infrared systems will be helpful.
For more complete information, includ-
ing typical wavenumbers for comparison
of spectra of textile materials, descrip-
tions of newer techniques such as Fourier
transform infrared spectroscopy (FTIR),
attenuated total reflectance spectroscopy
(ATR) and primary references, see 14.2.
For representative spectra of chemical
finishes, see 14.3.
7.2 Both grating instruments and
Fourier transform interferometers are
capable of producing high quality spectra
for identification and reference purposes.
Other spectroscopic techniques such as
laser-Raman spectroscopy, NMR spec-
troscopy and UV-visible spectroscopy
may also be utilized, if available, to fur-
ther identify the extracts. Figs. 1-5 repre-
sent infrared spectra run on an FTIR
spectrophotometer with MCT detector at
a resolution of 4 wavenumbers, signal
averaged over 30 scans with HAPP-
Gensel apodization cast on KRS-5 crys-
tal. Fig. 6 represents a proton NMR
spectrum of dimethyloldihydroxyethylene-
urea (DMDHEU) cellulose reactant in
deuterium oxide. Figs. 7 and 8 represent
laser-Raman spectra of aqueous solutions
of cellulose reactants using an argon ion
laser source. Figs. 9 and 10 represent
HPLC runs of cellulose reactants using
Refractive Index (R.I.) detector, 5 micron
C-18 reverse phase column, with 100%
water mobile phase pumping at 1.0 mL/
min. Fig. 11 represents an X-ray fluores-
cence spectrum taken from a scanning
electron microscope image using a liquid
nitrogen cooled detector with an energy
range of 0-5 kiloelectron-volts. For other
examples of infrared spectra, see 14.3
Copyright © 2005 American Association of Textile Chemists and Colorists
and 14.4.
7.3 Infrared Sample Preparation.
7.3.1 Techniques. Finish samples can
be prepared for infrared analysis by one
of the following methods: dissolve the
extract in suitable solvent, for analysis as
a liquid or as a cast film; grind the textile
sample to small particle size and mull in
mineral oil; pelletize the extract or
ground textile sample into a homoge-
neous mixture with potassium bromide
(KBr) (see 14.2).
7.4 Infrared Analysis.
7.4.1 Obtain a spectrum of the sample
or extract prepared by one of the above
techniques. The identity of the applied
finish is confirmed by comparison of the
sample spectrum with known infrared
spectra. For more accurate identification,
the spectrum of the known compound
should be obtained with the same appli-
cation and extraction history as the un-
known finish.
7.4.2 Softeners. Quaternary ammo-
nium compounds, polyethylenes, polyox-
yethylene glycols, polyurethanes and
polyacrylates are partially soluble in
trichloroethylene or 1,1,1-trichloroethane.
The extract is concentrated and trans-
ferred to a clean KBr disk.
7.4.3 Durable Press Finishing Agents.
Since most durable press finishing agents
can be extracted with either water or hy-
drochloric acid, this provides an alternate
method for removing finishes for infrared
spectroscopy. Approximately 0.2 g fab-
ric, cut into small squares, is refluxed for
5 min in 0.1 N HCl. The solution is then
decanted into a 50 mL round-bottom
flask with 350 mg spectral grade KBr and
evaporated to dryness on a rotary evapo-
rator while the flask is immersed in an
ice-salt bath to prevent further hydrolysis.
Final drying over phosphorus pentoxide
produces a residue that is mixed with
more KBr (in a 50 mg:300 mg ratio) and
pressed into a disk. A spectrum is ob-
tained and compared to that of known
compounds, with spectra of hydrolyzates
of known compounds preferable for ac-
curate comparison.
Another method of sample preparation
for identification of durable press finishes
by infrared spectroscopy is to grind the
fabric and pelletize it with spectral grade
KBr. Differential infrared spectra relative
to ground unfinished fabric are then ob-
tained. KBr disks containing equivalent
amounts of specimen in both beams of a
double beam spectrophotometer compen-
sate for the fabric bands. Computerized
spectral subtraction techniques may also
be used to achieve differential spectra.
7.4.4 A quick alternative for acquiring
infrared spectra of finishes was described
in the 1972 Intersectional Technical Pa-
per Competition presented by AATCC
Rhode Island Section (see 14.5). The
method relies on the transfer of finish by
TM 94-2002 131
solvent from a small rectangle of fabric
placed on the surface of an ATR crystal.
The solvent is evaporated leaving a thin
film of finish residue. The crystal is
placed in the ATR accessory holder and
the spectrum recorded.
8. Direct Spectroscopic Analysis of Fabric
8.1 With certain types of accessories
and spectroscopic techniques, it is pos-
sible to acquire direct spectra of both the
fabric substrate and the finishing com-
ponents on it. These techniques may in-
clude infrared reflectance with ATR and
diffuse reflectance accessories, photo-
acoustic spectroscopy (PAS), laser-
Raman spectra, electron spectroscopy for
chemical analysis (ESCA) and near infra-
red reflectance spectroscopy (NIR). In
many cases, computerized spectral sub-
traction techniques are useful in identify-
ing small amounts of finish on fabric.
9. Chromatographic Procedures
9.1 Chromatography is a very useful
method for the separation and tentative
identification of some of the finishes on
textile fabrics. After separation is accom-
plished, identification is made by chro-
matographic comparison to known com-
pounds either in pure form or after being
subjected to the same application and ex-
traction history as the unknown; identifi-
cation requires comparison under at least
two different sets of chromatographic
conditions. Alternatively, the chromato-
graphic peak of interest may be identified
spectroscopically on line or after isola-
tion. For most analyses, Soxhlet extracted
residues or their derivatives may be ana-
lyzed by GC, HPLC or TLC. Applica-
tions included in this section are simple
techniques for use with basic GC or
HPLC. For information on more complex
and diverse instruments and methods see
14.2.
9.2 Gas Chromatography. Gas Chro-
matography involves the separation of a
mixture of volatile substances as it is car-
ried through a column of surfaces that in-
teract differentially with the various com-
ponents of the mixture.
9.2.1 Formaldehyde. Formaldehyde re-
leased from fabrics may be detected by
GC. A fabric sample is enclosed in a vial
with a defined headspace and conditioned
under precise temperature and humidity.
Samples of the headspace gas are injected
for GC analysis. This system can also be
used to determine the amount of metha-
nol released by hydrolysis of methylated
N-methylol groups found in some dura-
ble press resins. Since the FID signal
from formaldehyde is not very strong, a
methanizer may be placed between the
column and the flame for conversion of
formaldehyde to methane. Alcohols are
also converted to corresponding hydro-
132 TM 94-2002
Copyright © 2005 American Association of Textile Chemists and Colorists
carbons. Conditions for formaldehyde
analysis are:
Column: 3 m Porapak T
Injection time: 9 s
Bath: 65°C
Needle: 150°C
Oven: 120°C
Injection port: 180°C
Detector: 480°C
A photoionization detector may also be
used for increased sensitivity. For further
information on this type of analysis see
14.2.
9.2.2 Softeners, Lubricants, and Emul-
sifiers. Solvents such as hexane or Freon
113 are used to extract softeners, lubri-
cants and emulsifiers from fabrics. These
three groups of products are commonly
made from fatty acids and fatty acid es-
ters or their derivatives. Some of these
compounds can be chromatographed di-
rectly and some must be made into deriv-
atives to be better detected by GC.
Other long chain fatty compounds are
more easily analyzed after derivatization.
Monocarboxylic acids are esterified,
usually with methanol, and these methyl
esters are analyzed as follows: Column:
45 m × 0.25 mm DEGS open tubular
column. Column temperature: 180°C.
Silylation, another method of derivati-
zation of fatty acids and fatty alcohols,
forms non-polar, volatile, thermally sta-
ble ethers. These ethers form easily, and
the reactions are performed in screw-
capped vials. The column used for analy-
sis is chosen according to the type of
compound that was silylated. The silyl
derivatives of glycerol and mono- and
diglycerides for example, are chromato-
graphed on a 1 ft OV-1 column. Quater-
nary ammonium salt derivatives require a
5% SE-30 column. For more detailed dis-
cussion of this application see 14.2.
Paraffin waxes, often used as softeners,
lubricants, water repellents and winding
lubricants are analyzed directly by GC.
Instrument conditions for paraffin wax
or alpha-olefin C-30+ type hydrocarbons
are:
Column: 6 ft × 1/8 in. stainless steel
(SS) OV-101, 5%
Column temperature: 200C-290°C at
10C/min then hold 11 min
Detector: Flame Ionization Detector
(FID) at 350°C
Injection port: 350°C
Carrier: Helium
Flow: 30 mL/min
Polyols. Water extracts of fabrics may
be analyzed by GC to detect ethylene and
diethylene glycols. Glycols are fre-
quently used with or in durable press res-
ins. Instrument conditions are:
Column: 6 ft × 1/8 in. stainless steel
(SS) Tenax GC, 60/80 mesh
Column temperature: 200°C
Detector: Flame Ionization Detector
(FID) at 250°C
Table II—Solvent Systems for Separating
Dye Classes
Dye Class Systema
Acid Propanol:Acetone:Water:Acetic Acid
(5:5:3:1)
Pyridine:Butyl Acetate:Water (9:6:5)
Butanol:Ethanol:Water (2:1:1)
Propanol:aqueous ammonia (28%)
(1:1)
Basic Butanol:Ethanol:Water:Acetic Acid
(10:1:1:1)
Benzene:Methanol (9:1)
Direct Propanol:Acetone:Water:Acetic Acid
(5:5:3:1)
Butyl Acetate:Pyridine:Water (5:5:2)
Butanol:Acetone:Water (5:5:3)
Organic Layer of
Butanol:Water:aqueous ammonia
(2:1:1)
Disperse Benzene:Acetone (9:1)
Benzene:Chloroform:Acetone (5:2:1)
Plastic Carbon Tetrachloride:Benzene (1:9)
Solvent Carbon Tetrachloride:Benzene (1:1)
Vat Toluene:Pyridine (6:4)
Benzene:Nitrobenzene:Acetone (8:1:1)
Butanol:Butyl Acetate:
Nitrobenzene:Acetone (3:3:3:1)
Butyl Acetate:Pyridine:Water (5:4:2)
Benzene:Pyridine:Dioxane:Acetone
(20:2:2:1)
a
Ratios are volumes of solvents; e.g., to make an
eluent such as propanol:acetone:water:acetic acid
(5:5:3:1), five volumes of propanol, five volumes of
acetone, three volumes of water, and one volume of
acetic acid are mixed (see 14.2).
Injection port: 250°C
Carrier: Helium at 30 mL/min
9.3 Thin Layer Chromatography Pro-
cedures. TLC is the separation of compo-
nents of a substance by differential travel
in a solvent phase over an absorbent plate
and can be an analytical tool for a variety
of textile extracts such as surfactants, dye
carriers, resins, polyester oligomers and,
more commonly, dyes. Reasons for utiliz-
ing TLC include small sample size, pre-
liminary work for HPLC method devel-
opment or two-dimensional separation.
For additional information see 14.2.
9.3.1 TLC Plates. For simplicity and
uniformity in TLC separations pre-coated
plates can be purchased from various
manufacturers. The plates may be coated
with absorbents such as alumina, cellu-
lose, octadecyl groups (C-18) bonded to
silica, or silica gel. A coating of C-18
bonded to silica is suitable for resin anal-
ysis. Dual phase TLC plates with the two
phases at right angles to each other may
be used for separation of emulsified prod-
ucts such as waxes or latex.
9.3.2 Size. The sample size should be
very small. Use of a microliter syringe is
recommended. When analyzing the fab-
ric extracts it may be necessary to place
AATCC Technical Manual/2006
successive spots on top of each other. Column: CN (reverse phase) Under these conditions, other finishes
Spots should be thoroughly dried before Flow rate: A range of 1-1.5 mL/min including uron, triazones and glycols in
developing. Eluent: 40% water/42% methanol/ the resin can also be identified.
9.3.3 Solvent System. Once the fabric 18% isopropyl alcohol
extract is obtained and the chromato- Detector: UV at 254 nm 10. Elemental Analysis
graphic plate or strip is spotted with the 9.4.2 Resin Finishes. Some resins can
sample, determine the correct eluent or 10.1 Determination of the elemental
be extracted with water. HPLC is ideal content of finished textiles can be used to
solvent. The solvent system used in TLC for critical comparison of resin finishes.
relates directly to that used in liquid chro- indicate the presence of various finishing
See an example in Fig. 9 for a chromato- agents. Increased nitrogen content on
matography. For examples of solvent sys- gram of DMDHEU resin.
tems for various textile chemicals, refer treatment of fabric, as determined by tra-
The following conditions were used: ditional Kjeldahl analysis or by instru-
to Table I. Table II gives some solvent Column: C-18 (reverse phase)
systems for various dyes. For additional mental nitrogen analyzers, can suggest
information on solvent systems see 14.2. Eluent: 100% water the presence of durable press reactants.
9.3.4 Development. Place the TLC Detector: Refractive index Nonmetallic elements such as phospho-
plate and solvent in a sealed developing Flow rate: 1.0 mL/min rus, chlorine and bromine from flame
chamber which can be a small inexpen-
sive jar with a lid. Better resolution is
achieved by using the smallest applica- Table III—Chemical Spot Tests
tion volume possible and by placing a
strip of filter paper which is solvent satu- Reference
rated in the chamber. The solvent level Substance Reagents Employed Reaction Note
should be slightly lower than the level of
Formaldehyde Chromotropic acid and sulfuric acid Purple color 14.6, 14.7
sample spotted on the plates.
9.3.5 Detection. The separated compo- Phenylhydrazine hydrochloride, hydrochloric Cherry red color 14.8
nents are detected visually (as with dyes), acid, and ferric chloride
by UV light or saturation of the plate with Starch Iodine and potassium iodide in water Purple color 14.2
iodine vapor. Saturate the plate with io- Urea p-Dimethylaminobenzaldehyde in methanol Yellow color 14.2
dine by placing a few crystals in the bot- and hydrochloric acid
tom of the detection chamber. Other Zinc Dithiazone (diphenylthiocarbozone) Cherry red color 14.2, 14.9
chemicals for the detection of noncolored in acetone
components are available from TLC sup- Zirconium Alizarin in alcohol Red to red-violet 14.9
pliers. Examples are Dragendorff reagent precipitate
used for the detection of amines and
Magnesium Quinalizarin in methanol, and Blue precipitate 14.2, 14.9
phosphomolybdic acid solution and sul- sodium hydroxide
furic acid can be used for general purpose
detection (see 12.1). Aluminum Aluminum and ammonium acetate Red color 14.2, 14.9
9.4 High Performance Liquid Chroma- Iron Hydrochloric acid and potassium ferrocyanide Deep blue color 14.2, 14.9
tography Procedures. Several fabric fin- Hydrochloric acid and potassium thiocyanate Deep red color 14.2, 14.9
ishes and extracts can be detected by Hydrochloric acid and heat Yellow color
HPLC, which relies on separation of
components carried by a liquid phase Ammonium ion Sodium hydroxide and heat Odor of ammonia 14.2
through a column and detection by UV or Chloride ion Silver nitrate and nitric acid White to gray precipitate 14.2, 14.9
RI. Formaldehyde, resins and other auxil- Nitrate ion Ferrous sulfate and sulfuric acid Brown ring forms 14.2, 14.9
iaries as well as residual chemicals from Phosphate ion Ammonium molybdate, benzidine Blue color 14.2, 14.9
prior processing can be detected. hydrochloride and ammonium acetate
9.4.1 Formaldehyde. Formaldehyde Sulfate ion Barium chloride and hydrochloric acid White precipitate 14.2
(CH2O), extracted from the fabric in
water, precipitated as formaldehyde *Phosphorus Nitric acid and ammonium molybdate Yellow color 14.2, 14.9
2,4-dinitrophenylhydrazone, and analyzed *Nitrogen Ferrous sulfate and ferric chloride Deep blue color 14.2, 14.9
by liquid chromatography, is detectable at *Sulfur Sodium nitroferricyanide Red violet color 14.2, 14.9
very low levels. To prepare the reference *Chlorine Silver nitrate in water, and nitric acid White to gray precipitate 14.2
standard, place 50 mL of a 2% formalde-
*Bromine Silver nitrate and nitric acid Yellow precipitate 14.2
hyde solution in a beaker with 50 mL of a
0.24% solution of 2,4-dinitrophenylhy- Polyvinyl alcohol Chromic acid and sodium hydroxide Brown stain 14.2
drazine (DNPH) hydrochloride (in 30% Iodine and potassium iodide and boric acid Purple color 14.2
perchloric acid). After 1 h at room tem- Polyvinyl acetate Iodine and potassium iodide Red-brown color 14.2
perature filter the precipitated hydrazone,
Sodium Uranyl nitrate Yellow precipitate 14.2
rinse first with water and then with etha- carboxymethyl-
nol, and dry. Dissolve all of the precipi- cellulose
tate in methylene chloride and analyze by
HPLC. To prepare the sample place 50 Proteins Potassium hydroxide, heat, copper sulfate Violet color 14.2
mL of extract in a 250 mL separatory Methylol Phenylhydrazine hydrochloride, hydrochloric Light pink color 14.8
funnel with 10 mL of 0.24% 2,4-DNPH melamine acid, and ferric chloride
(in 30% perchloric acid). After 1 h, ex- Methylol urea Phenylhydrazine hydrochloride, hydrochloric Pale brown color 14.8
tract the hydrazone with methylene chlo- acid, and ferric chloride
ride, condense the extract and analyze. Methylol ethylene Phenylhydrazine hydrochloride, hydrochloric Deep red brown color 14.8
Fig. 12 is a chromatogram of standard al- acid, and ferric chloride
dehydes reacted with 2,4-DNPH. Instru-
ment conditions are: *Sodium Fusion Method

AATCC Technical Manual/2006 TM 94-2002 133

Copyright © 2005 American Association of Textile Chemists and Colorists
retardant finishes, as well as fluorine
from soil-release finishes, can be ana-
lyzed by chemical digestion or oxygen
flask combustion followed by titration,
specific ion analysis or other instrumental
methods.
Metals on fabric, such as antimony or
titanium from flame retardants, magne-
sium or zinc from resin catalysts and so-
dium or potassium salts of other finishes,
can be determined by acid extractions or
dry ashing followed by atomic absorption
(AA) analysis or inductively coupled
plasma (ICP) analysis. X-ray fluores-
cence can be used to determine the con-
tent of many elements directly on the fab-
ric simultaneously.
11. Chemical Spot Tests
11.1 Qualitative spot tests are detection
methods based on chemical reactions em-
ploying a drop of test solution or reagent
(Table III). The chemical reaction usually
results in a characteristic color or odor.
Spot test methods should be sensitive, re-
liable and capable of being conducted
satisfactorily with small sample amounts
and simple equipment. Identification
limit is the minimum quantity of a sub-
stance dissolved in the test solution
which can be detected. Spot tests are not
designed to furnish a complete analysis
of the kind or amounts of all constituents
in a given material, but rather to deter-
mine whether or not certain elements,
compounds or classes of compounds are
present or absent. The analyst is cau-
tioned to run a blank and a known sample
Fig. 1—Infrared spectrum of a fatty ester softener.
134 TM 94-2002
Copyright © 2005 American Association of Textile Chemists and Colorists
containing the substance in question,
along with the unknown sample. Further,
tests should be repeated for confirmation
of reliability.
11.2 Several procedures are available
for spot tests: (1) a drop of test solution
and a drop of reagent can be brought to-
gether on a nonporous surface; (2) a drop
of test solution can be placed onto a me-
dium impregnated with a reagent; (3) a
drop of reagent can be placed on a solid
specimen; (4) a drop of reagent or a strip
of reagent paper can be exposed to the ac-
tion of gases evolved from the test solu-
tion or solid specimen (see Table III); and
(5) a drop of solution can be placed on a
textile and color development observed
on white filter paper held beneath the
specimen. For analysis of textile finish-
ing agents, the sample may be prepared
for one of the above treatments in several
ways. First, the test may be carried out di-
rectly on a fabric sample with no prelimi-
nary preparation. Second, the fabric may
be extracted with a selected solvent and
the test carried out with the extract as the
test solution. Third, the fabric (or textile
sample) may be destroyed by dry or wet
ashing methods, and the residue tested in
solid or dissolved form. Finally, a fusion
method may be used for substances
which form insoluble oxides on ignition.
This method involves heating the sample
with metallic sodium or potassium.
12. Report
12.1 Report any finish or finish com-
ponents detected. The report should in-
Appendix 1—Spectra
Fig. 2—Infrared spectrum of a silicone softener.
clude solvents used for extraction and
method of extract analysis (including in-
strument conditions) or should state other
specific techniques employed.
13. Precision and Bias
13.1 Precision and bias statements are
not applicable because data are not gener-
ated by this method.
14. Notes and References
14.1 Available from Publications Office,
ACGIH, Kemper Woods Center, 1330
Kemper Meadow Dr., Cincinnati OH 45240;
tel: 513/742-2020.
14.2 Analytical Methods for a Textile Labo-
ratory, Third Edition, 1984, American Associ-
ation of Textile Chemists and Colorists,
Research Triangle Park NC.
14.3 Infrared Spectra for the Identification
of Chemical Finishing Agents from Textiles,
Part I, ARDS-S-47, October 1974, Agricul-
tural Research Service, U.S. Dept. of Agricul-
ture.
14.4 Handbook of Chemical Specialties,
John E. Nettles, Chapter on Textile Fiber Pro-
cessing, Preparation and Bleaching, John
Wiley & Sons, New York.
14.5 Textile Chemist and Colorist, Vol 5,
No. 12, December 1973, p279.
14.6 Walker, J. F. Formaldehyde, Reinhold,
NY, 1964.
14.7 Feigl, F., Spot Tests in Organic Analy-
sis, 7th Edition, Elsevier, Amsterdam, 1966.
14.8 VanLoo, W. J., Jr., et al, American
Dyestuff Reporter, Vol. 45, 1956, p397.
14.9 Feigl, F., Spot Tests in Inorganic Anal-
ysis, 7th Edition, Elsevier, Amsterdam, 1966.
AATCC Technical Manual/2006
 Fig. 3—Infrared spectrum of a Fig. 4—Infrared spectrum of tris (1,3 dichloropropyl)
DMDHEU cellulose reactant. phosphate flame retardant.

Fig. 5—Infrared spectrum of a fluorochemical Fig. 6—Proton NMR spectrum of

soil release agent. DMDHEU cellulose reactant.

Fig. 7—Laser-Raman spectrum of Fig. 8—Laser-Raman spectrum of methyl

DMDHEU cellulose reactant. carbamate cellulose reactant.

AATCC Technical Manual/2006 TM 94-2002 135

Copyright © 2005 American Association of Textile Chemists and Colorists
 Fig. 9—High performance liquid chromatogram of Fig. 10—High performance liquid chromatogram of
DMDHEU cellulose reactant. a glycolated DMDHEU cellulose reactant.

Fig. 11—X-Ray fluorescence spectrum of a magnesium

chloride-aluminum chloride catalyst.

Fig. 12—Separation of 2,4-dinotrophenylhydrazine

derivatives of aldehydes: (A) solvent peak;
(B) glyceraldehyde DNPH; (C) formaldehyde DNPH;
(D) acetaldehyde DNPH; (E) propionaldehyde DNPH;
(F) isobutyladehyde DNPH.

136 TM 94-2002 AATCC Technical Manual/2006

Copyright © 2005 American Association of Textile Chemists and Colorists