AATCC TM206-2020 Test Method for Free and Hydrolyzed FormaldehydeWater Extraction 游离甲醛和水解甲醛的试验方法：水萃取

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AATCC Manual of International Test Methods and Procedures/2023 AATCC TM206-2020 435

1. Purpose and Scope

1.1 This test method is applicable to

wettable (non-hydrophobic) textile fab-

rics that may contain free or hydrolyzed

formaldehyde, particularly fabrics fin-

ished with chemicals containing formal-

dehyde. It provides a water extraction

process and a subsequent colorimetric

analysis of the amount of free and hydro-

lyzed formaldehyde extracted.

2. Principle

2.1 A weighed fabric specimen is sub-

merged in a flask filled with deionized

water. The sealed or capped flask is

placed in a water bath at a controlled tem-

perature for a specified length of time.

The amount of formaldehyde extracted

into the water is then determined colori-

metrically.

3. Terminology

3.1 free formaldehyde, n.—formalde-

hyde that is not bonded to a finish or a

fabric. In this form, formaldehyde can be

readily extracted from the fabric by im-

mersion in water.

3.2 hydrolyzed formaldehyde, n.—

although originally part of larger chemi-

cal structure, such as a crosslinking reac-

tant, the formaldehyde is cleaved from

the larger molecule and dissolved into the

water.

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 practice should be

followed. Wear safety glasses in all labo-

ratory areas.

4.2 When handling glacial acetic acid

to prepare Nash reagent, use chemical

goggles or face shield, impervious gloves

and an impervious apron during prepara-

tion. Concentrated acids should be han-

dled only in an adequately ventilated lab-

oratory hood. CAUTION: Always add

acid to water.

4.3 Formaldehyde is a carcinogen. Use

in an adequately ventilated laboratory

hood. Avoid inhalation or skin contact.

Use chemical goggles or face shield, im-

pervious gloves and an impervious apron

when working with formaldehyde (see

8.1 and 9.1).

4.4 An eyewash/safety shower should

be located nearby and a self-contained

breathing apparatus should be readily

available for emergency use.

4.5 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; see www.osha.gov for

latest version). 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 ex-

posure which should be met (see 14.3).

5. Uses and Limitations

5.1 The procedure is intended for use

in the range of free and hydrolyzed form-

aldehyde on non-hydrophobic fabric

from 20 µg/g up to about 3500 µg/g. This

test method approximates hydrolyzed

formaldehyde and closely simulates nor-

mal user conditions. However, TM206 is

an aqueous immersion method and fab-

rics with a propensity for bleeding could

be a concern; if the dye has an absor-

bance in the range of 412nm, it could in-

terfere with the spectrophotometric mea-

surement. It is not intended to

approximate formaldehyde released un-

der hot storage conditions.

5.2 Alternatively, AATCC TM112,

Test Method for Formaldehyde Release

from Fabric: Sealed Jar (see 14.1), deter-

mines free and hydrolyzed formaldehyde

and additional formaldehyde as generated

under more severe conditions than this

test method. The appropriate test should

be chosen based on that distinction (see

14.2).

6. Apparatus, Reagents, Materials

6.1 250-mL Erlenmeyer flasks with

stoppers.

6.2 Weighing balance, with a minimum

sensitivity of 0.01 g.

6.3 Thermostatically controlled water

bath: 40 ± 1°C (105 ± 2°F).

6.4 Nash reagent prepared from ammo-

nium acetate, acetic acid and acetylace-

tone and water (see 7.1).

6.5 Formaldehyde solution, approxi-

mately 37% (see 4.3).

6.6 Volumetric flasks, 50, 250, 500 and

1000-mL, Class A.

6.7 Volumetric pipettes, 1, 2, 3, 5, 10,

15, 20, 25, 30 and 100-mL, all calibrated

“to deliver” and meeting Class A volume

accuracy and flow time requirements, or

a digital, variable-volume pipette capable

of meeting Class A requirements.

6.8 A 1-L clean brown glass bottle.

6.9 Spectrophotometer, capable of

reading absorbance to a minimum of

three decimal places, at a wavelength of

412 nm.

6.10 Test tubes (see 14.4).

6.11 Distilled or deionized water.

Hereafter, referred to as deionized water.

6.12 pH meter, calibrated and accurate

to 0.01

7. Preparation of Nash Reagent

7.1 Nash Reagent: In a 1000-mL volu-

metric flask, dissolve 150 g of ammo-

nium acetate in 800-mL of deionized wa-

ter; add 3.0 + 0.1 mL of glacial acetic

acid and 2.0 + 0.1 mL of acetylacetone.

Add deionized water up to the 1000-mL

level and mix. Store in a capped brown

bottle.

7.1.1 Newly made Nash Reagent re-

quires a 12 h wait period before being

used as the reagent darkens slightly in

color during that time period. The reagent

may be used up to 8 weeks after it is

made. However, since the sensitivity may

change slightly over a long period of

time, it is good practice to run a calibra-

tion curve weekly or when used to correct

for the slight changes in the standard

curve.

8. Preparation of Standard Solution and

Calibration

8.1 Prepare a 1500 µg/mL stock solu-

tion of formaldehyde by diluting 3.8-mL

of reagent grade formaldehyde solution

(approximately 37%, see 4.3) to 1.0-L

with deionized water in a volumetric

flask. Equilibrate the stock solution for a

minimum of 24 h in a capped/stoppered

flask before standardization. Determine

the concentration of formaldehyde in the

AATCC TM206-2020

Test Method for Free and Hydrolyzed Formaldehyde:

Water Extraction

Provided by Accuris under license with AATCC

Licensee=Underwriters Laboratories - Ho Chi Ming City, Vie/5909636157, User=Le,

Not for Resale, 11/23/2023 20:10:19 MST

No reproduction or networking permitted without license from Accuris

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436 AATCC TM206-2020 AATCC Manual of International Test Methods and Procedures/2023

stock solution by a standard method (see

Section 9. Standardization of Stock

Formaldehyde Solution, or any other

suitable procedure such as sodium sulfite

titration using 0.1 N HCl (see 14.5).

Record the actual concentration of this

standardized stock solution. This stock

solution will keep for at least four weeks

and is used to prepare standard dilutions.

8.1.1 A 1:10 dilution of the standard-

ized formaldehyde stock solution is pre-

pared by pipetting 25-mL of the standard-

ized stock solution into a 250-mL

volumetric flask and diluting to the mark

with deionized water. The stock solution

is then titrated and its concentration is de-

termined as µg/mL.

8.2 A 5-concentration calibration

curve, which may include zero, is sug-

gested. Prepare the calibration curve by

pipetting from the following: 0, 1, 3, 5,

10, 15, 20 and 30-mL volumes of the

1:10 dilution into 500-mL volumetric

flasks then adding deionized water to the

500-mL level. (If, for example, the stan-

dardized stock solution were found to be

1470 µg/mL by titration, calculate new

values for the calibration curve abscissa;

i.e., 0.0, 0.29, 0.88, 1.47, 2.94, 4.41, 5.88,

8.82 µg/mL using regression analysis.)

8.2.1 When 1, 3, 5, 10, 15, 20 and 30-

mL aliquots of the 1:10 dilution of the

standardized stock solution from 8.1 are

diluted with deionized water in 500-mL

volumetric flasks, formaldehyde solu-

tions containing approximately 0.30,

0.90, 1.5, 3.0, 4.5, 6.0 and 9.0 µg/mL

formaldehyde respectively will be ob-

tained. Record the calculated concentra-

tion of each solution as determined by

section 9 Standardization of Stock Form-

aldehyde. The equivalent concentrations

of the formaldehyde in the test fabric

based on the weight of accurately known

1 g of the test fabric and 100-mL of water

in the Erlenmeyer flasks will be 100

times the accurate concentrations of these

standard solutions.

8.3 Use 5 mL aliquots of each of the

standard solutions and the procedure de-

scribed in 11.4-11.7 to prepare a calibra-

tion chart in which µg/mL formaldehyde

are plotted against absorbance.

9. Standardization of Formaldehyde Stock

Solution

9.1 The stock solution containing ap-

proximately 1500 µg/mL of formalde-

hyde must be standardized in order to

produce precise calculations from the cal-

ibration curve required in colorimetric

analysis.

9.2 An aliquot of the stock solution is

reacted with an excess of sodium sulfite

followed by a back-titration with stan-

dard acid solution to a pH of 9.5.

9.2.1 Apparatus: 10 mL-volumetric pi-

pette, 50-mL volumetric pipette, 50-mL

burette, 150-mL beaker.

9.2.2 Reagents: 1.0 M sodium sulfite

(126 g Anhydrous Na2SO3/L), 0.02 N sul-

furic acid (can be purchased in standard-

ized form from chemical supply compa-

nies or must be standardized from

standard NaOH solution). Do not use

commercial standardized sulfuric acid

that has been stabilized with formalde-

hyde. If there is a doubt, check with the

chemical supplier.

9.2.3 Procedure:

A. Pipette 50-mL of the 1.0 M sodium

sulfite (Na2SO3) into the beaker.

B. Pipette 10-mL of the stock formal-

dehyde solution to a beaker.

C. Titrate the solution with the stan-

dard 0.02 N H2SO4 to an endpoint of pH

of 9.5.

9.2.4 Record the volume of acid used

to the nearest 0.01-mL. (The volume of

acid should be approximately 25-mL for

0.02 N acid.)

Calculations:

C = (30,030) (A) (N)/10

where:

C= Wt/Vol concentration of formal-

dehyde (µg/mL)

A= Vol of acid used (mL)

N= Normality of acid

9.3 Repeat the titration standardization

in duplicate or triplicate. Average the re-

sults.

9.4 Use the determined concentration

in preparing the calibration curve for the

colorimetric

analysis.

10. Test Specimens

10.1 Samples should immediately be

placed into separate zipper-type closure

plastic bags when sampled. As an extra

precaution for maintaining their original

state the samples may be wrapped in alu-

minum foil before being placed in the

plastic bags.

10.2 Cut approximately 1-g specimens;

weigh each one to ± 0.01 g. Perform in

duplicate for each sample. If there is a de-

lay in testing the 1-g specimens once they

are cut, they should be put back into the

zipper-type closure plastic bags (and re-

wrapped in foil if previously done) until

testing commences.

11. Procedures

11.1 Pipette 100.0-mL of deionized

water into each Erlenmeyer flask. Place a

fabric specimen in each flask. The fabric

should be completely submerged in the

water and not float on the surface (see

14.6). A stirring rod may be used to push

and keep the fabric below the water sur-

face. Cap the flasks and place them in the

water bath at 40 ± 1°C (105 ± 2°F) for 60

± 2 min. Shake the flasks every 5 min by

hand or use an ultrasonic water bath for

agitation. If using an ultrasonic bath,

check the water frequently for tempera-

ture changes.

11.2 Remove the flasks from the water

bath.

11.3 Remove the fabric from the

flasks. Recap the flasks and shake them

to mix any condensation formed on the

sides. Allow solutions to cool for 30 min.

11.4 Pipette 5-mL of Nash reagent into

a suitable number of test tubes, small (50-

mL) Erlenmeyer flasks, or other suitable

flasks (colorimeter or spectrophotometer

tubes can be used directly, see 14.4) and

pipette 5-mL of the reagent into at least

one additional tube for a reagent blank.

Add 5-mL aliquots from each of the sam-

ple incubation jars to the tubes. Reagent

blanks are prepared by adding 5-mL of

the Nash reagent and 5-mL of deionized

water to the tubes.

11.5 Mix and place the tubes in a 40 ±

1°C (105 ± 2°F) water bath for 30 ± 1

min. Remove tubes from bath. Cap with

stoppers or plastic paraffin film and allow

to cool to room temperature away from

direct light.

11.6 Read the absorbance in the spec-

trophotometer against the reagent blank

at 412 nm. Caution: Exposure of the de-

veloped yellow color to direct sunlight

for a period of time will cause some fad-

ing. If there is appreciable delay in read-

ing the tubes after color development and

strong sunlight is present, care should be

exercised to protect the tubes from light.

Otherwise the color is stable for consider-

able time (at least overnight) and reading

may be delayed (see 14.7 and 14.8).

11.7 Determine the µg/mL formalde-

hyde (HCHO) in the sample solutions us-

ing the prepared calibration curve (see

8.3 and 14.9).

12. Calculations and Report

12.1 Calculate the amount of formalde-

hyde released for each specimen to the

nearest µg/g using the following equation:

F = (C) (100)/W

where:

F= concentration of formaldehyde

(µg/g),

C= concentration of formaldehyde in

solution as read from the calibra-

tion curve

W= weight of the test specimen, g.

12.2 If performing both this test and

AATCC TM112, care should be used in

reporting calculated results as this test

uses 100-mL of water and AATCC

TM112 uses 50-mL.

13. Precision and Bias

13.1 Precision.

13.1.1 Interlaboratory tests. One inter-

Provided by Accuris under license with AATCC

Licensee=Underwriters Laboratories - Ho Chi Ming City, Vie/5909636157, User=Le,

Not for Resale, 11/23/2023 20:10:19 MST

No reproduction or networking permitted without license from Accuris

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AATCC Manual of International Test Methods and Procedures/2023 AATCC TM206-2020 437

laboratory study (ILS) of AATCC

TM206 was conducted in 2015. Some of

the three participating laboratories used

two operators, each of whom tested mul-

tiple specimens of the same material. Sin-

gle operators in each participating labora-

tory ran minimum of two determinations

on the same fabric having low formalde-

hyde levels in the range of 50-100 µg/

mL. The results from all participants

were evaluated using basic descriptive

statistics and analyzed by analysis of

variance (ANOVA).

13.1.2 Calculation of components of

variance (see Table I) was thought to be

appropriate and critical differences (see

Table II) and confidence limits (see Table

III) were calculated for this low level-

formaldehyde fabric as shown below.

13.1.3 When two or more laboratories

wish to compare test results, it is recom-

mended that laboratory level be estab-

lished between them prior to beginning

test comparisons.

13.1.4 If comparisons are made be-

tween laboratories on a single fabric con-

taining a low level of free formaldehyde

content, the critical differences in the col-

umn, single level, in Table II should be

used.

13.1.5 The number of determinations

per laboratory average also determines

the critical difference.

13.2 Bias.

13.2.1 The formaldehyde release of a

fabric can be defined only in terms of a

test method. There is no independent

method for determining the true value.

As a means of estimating free formalde-

hyde content from a fabric under the con-

ditions of AATCC TM206, the method

has no known bias.

13.2.2 AATCC TM206 generally is ac-

cepted by the textile and apparel indus-

tries as a referee method.

14. Notes

14.1 Available from AATCC, P.O. Box

12215, Research Triangle Park NC 27709; tel:

+1.919.549.8141; fax: +1.919.549.8933; or-

dering@aatcc.org; www.aatcc.org.

14.2 Formaldehyde is a component of, or

precursor to, many fabric finishes. As part of

the application the finish is cured, which may

result in self-crosslinking of the finish and/or

crosslinking of the finish with the fabric. In-

complete crosslinking, or hydrolysis in later

storage, can result in the presence of hydro-

lyzed formaldehyde on the fabric. This test is

to determine the amount of free and hydro-

lyzed formaldehyde. Warm moist conditions

can (further) hydrolyze cross-linked finishes

and release more formaldehyde. AATCC

TM112 determines free and hydrolyzed form-

aldehyde and additional formaldehyde as gen-

erated under more severe conditions than this

test method. The appropriate test should be

chosen based on that distinction.

14.3 Available from Publications Office,

ACGIH, Kemper Woods Center, 1330

Kemper Meadow Dr., Cincinnati OH 45240;

tel: 513-742-2020; www.acgih.org.

14.4 The ratio of reagent to sample solu-

tions can be adjusted, within limits, to suit the

individual absorbance range and optical path

length of the sampling tubes or cuvettes of the

particular photometric instrument being used.

For example, although 5-mL reagent to 5-mL

sample solution has been found convenient for

several types of instruments, other 1:1 ratios,

such as a ratio of 2-mL reagent to 2-mL sam-

ple may be more suitable for others. The same

ratio should be used with the standards as with

the sample. The use of spectrophotometer

tubes directly for color developments avoids

the transfer step of test tubes to spectropho-

tometer cells, and may save considerable time

when many determinations are to be made.

Repipettes or similar devices can be used for

reagent dispensing, and disposable tip auto-

matic pipettes can be used for preparing the

sample solutions.

14.5 J. Frederick Walker, Formaldehyde,

3rd Ed. Reinhold Publication Co., New

York, 1964, p486. An alternate reference is the

Analytical Methods for a Textile Laboratory,

Third Edition, 1984, edited by J. William

Weaver (see 14.1).

14.6 It is important that the fabric be totally

submerged in the water during the extraction

process. If necessary, use a non-formaldehyde

containing surfactant. A concentration of

0.2% surfactant is recommended.

14.7 If extracted solutions are colored in

flask, refer to publication by Dilip Pasad “Op-

timization of the AATCC Sealed Jar and

HPLC Methods for Measurement of Low

Levels of Formaldehyde,” AATCC Textile

Chemist and Colorist, June 1989, Volume 21,

No 6 (see 14.1).

14.8 If the extracted solutions contain par-

ticulate matter, the solutions should be centri-

fuged or filtered to remove contaminant.

14.9 The procedure in Section 10 has been

set up to cover the range from about 0 µg/g on

the weight of the fabric to about 500 µg/g. In

fabrics containing hydrolyzed formaldehyde

in the range exceeding 1.0 Absorbance unit, it

is recommended that a ratio of 10-mL Nash

reagent to 1-mL sample be used. If this is

done, it is necessary to prepare an additional

calibration chart with 10:1 ratios of standard

solutions to Nash reagent by diluting 1, 3, 5,

10, 15 and 20 µg/mL, respectively, of the ap-

proximately 1500 µg/mL standardized stock

solution of formaldehyde to the mark with

deionized water in 500-mL volumetric flasks.

Formaldehyde solutions containing approxi-

mately 3, 9, 15, 30, 45 and 60 µg/mL respec-

tively will be obtained (see 8.3).

15. History

15.1 Revised in 2020 to update multiple

sections for clarity.

15.2 Reaffirmed 2017; editorially revised

2018, 2020 (with title change).

15.3 Developed in 2016 by AATCC Com-

mittee RA45.

Table I—Components of Variance as

Standard Deviations, Expressed in

Percentage Points

Component Variance Fabric 1

Laboratory 2.4

Operator 1.1

Specimen 2.2

Table II—Critical Differences—95.0% Confidence, Expressed in Percentage Points

Observations in Avg (N) Single Operator Within Laboratory Between Laboratory

1 13.3 6.8 9.6

2 6.7 5.3 8.6

3 4.4 4.7 8.2

4 3.3 4.3 8.0

5 2.7 4.1 7.9

6 2.2 3.9 7.8

Note: Critical differences were calculated using z = 1.960.

Table III—Confidence Limits—95.0% Confidence, Expressed in Percentage Points

Observations in Avg (N) Single Operator Within Laboratory Between Laboratory

1 9.4 4.8 6.8

2 4.7 3.7 6.1

3 3.1 3.3 5.8

4 2.4 3.0 5.7

5 1.9 2.9 5.6

6 1.6 2.8 5.5

Note: Confidence limits were calculated using z = 1.960.

Provided by Accuris under license with AATCC

Licensee=Underwriters Laboratories - Ho Chi Ming City, Vie/5909636157, User=Le,

Not for Resale, 11/23/2023 20:10:19 MST

No reproduction or networking permitted without license from Accuris

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标签： #试验方法

摘要：

本文详细介绍AATCC TM206-2020标准，即《游离甲醛和水解甲醛的试验方法：水萃取》的完整技术内容。该标准由美国纺织化学师与印染师协会（AATCC）发布，专门用于测定纺织品中游离甲醛及经水解产生的甲醛含量。测试通过将样品在水中进行萃取，采用特定化学方法分析萃取液中的甲醛浓度。本方法适用于各类纺织材料，是纺织品出口贸易、质量检测及环保合规中重要的甲醛限量检测依据。文章涵盖适用范围、试验原理、试剂与仪器、操作步骤、结果计算及精密度要求，帮助实验室人员、质量控制工程师及标准合规管理者快速掌握该

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