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1、? Copyright 2005 American Association of Textile Chemists and Colorists AATCC Technical Manual/2006TM 20A-200557 Developed in 1957 by AATCC Committee RA24; revised 1958, 1959, 1975, 1995, 2000, 2004, 2005; reaffirmed 1971, 1978, 1981, 1989; editorially revised 1980, 1982 (new title), 1985, 2002. Re-
2、 lated to ISO 1833. 1. Purpose and Scope 1.1 This method presents individual procedures for the quantitative determi- nation of moisture content, nonfibrous content and fiber composition of textiles. 1.2 The procedures for the determina- tion of fiber composition include me- chanical, chemical and m
3、icroscopical methods. They are applicable to blends of the following generic classes: Natural FibersMan-Made Fibers CottonAcetate HairAcrylic HempModacrylic LinenNylon (see 17.1) RamieOlefin SilkPolyester WoolRayon Spandex 2. Uses and Limitations 2.1 The procedure given for the re- moval of nonfibro
4、us materials will re- move most, but not all, of these compo- nents. Each treatment is applicable only to certain categories of these substances and no general scheme can be given that is all inclusive. Some of the newer fin- ishes may present special problems and the analyst will have to deal with
5、these cases as they arise. Thermosetting resins and crosslinking latices are not only diffi- cult to remove but in some cases cannot be wholly removed without destroying the fiber. When it is necessary to modify a procedure, or use a new one, one should make sure that the fibrous portion of the spec
6、imen under test is not attacked. Fiber composition is generally expressed either on the oven-dry weight of the textile as received or on the oven-dry weight of the clean fiber after nonfibrous materials are first removed from the textile before the fiber analysis is carried out, or if the treat- men
7、ts described in Section 9 are incapa- ble of removing them, any such materials present will increase the percentage of the fiber constituent with which they are removed during the analysis. 2.2 The procedure for determining fi- ber composition by mechanical separa- tion is applicable to those textil
8、es wherein the different fibers making up its composition are segregated in separate yarns, or plies, in the textile product. 2.3 The chemical procedures for fiber composition described herein are applica- ble to most of the current, commercial production fibers within each generic class listed. Kno
9、wn exceptions are noted in Table II. However, there may be in- stances in which a method may not be fully adequate for a newly developed fi- ber falling within one of the listed generic classes and for re-used and/or physically or chemically modified fibers. Caution should be exercised when applying
10、 these methods to such cases. 2.4 The microscopical procedures for fi- ber composition are applicable to all fibers and their accuracy depends to a consider- able extent upon the ability of the analyst to identify the individual fibers present. However, owing to the tedious nature of this technique,
11、 its use is generally limited to those mixtures which cannot be sepa- rated mechanically or chemically; e.g., mixtures of hair and wool and mixtures of cotton, linen, hemp and/or ramie. 3. Terminology 3.1 clean-fiber content, n.the amount of fiber after removal of nonfibrous content. 3.2 fiber, n.in
12、 textiles, a generic term for any one of the various types of matter that form the basic elements of a textile and which are generally characterized by flexibility, fineness and high ratio of length to thickness. 3.3 moisture content, n.that part of the total mass of a material that is ab- sorbed or
13、 adsorbed water, compared to the total mass. 3.4 nonfibrous content, n.products such as fiber finishes, yarn lubricants, slasher sizing, fabric softeners, starches, china-clay, soaps, waxes, oils and resins which are applied to fiber, yarn, fabric or apparel. 3.5 Additional terms used in this test m
14、ethod can be found in standard chemi- cal dictionaries, in dictionaries of com- mon terms or in A Glossary of AATCC Standard Terminology (located elsewhere in this TECHNICAL MANUAL). 4. Safety Precautions NOTE: These safety precautions are for information purposes only. The pre- cautions are ancilla
15、ry to the testing proce- dures and are not intended to be all inclu- sive. It is the users 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 manufacturers re
16、commenda- 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 All chemicals should be handled with care. 4.3 Perform the soxhlet extractions in Section 9, Nonfibrous MaterialClean
17、Fiber Content, using Fluorocarbon 113 (such as Freon TF) or hydrochlorofluoro- carbon (such as Genesolv 2000) and ethyl alcohol inside an adequately ventilated laboratory hood. CAUTION: Ethyl alco- hol is highly flammable. 4.4 Perform Chemical Analysis Proce- dure No. 1 (Table II, 100% acetone) in-
18、side a ventilated laboratory hood. CAU- TION: Acetone is highly flammable. 4.5 Ethyl alcohol and acetone are flam- mable liquids and should be stored in the laboratory only in small containers away from heat, open flame and sparks. 4.6 In preparing, dispensing, and han- dling hydrochloric acid (20%)
19、, sulfuric acids (59.5% and 70%), and formic acid (90%) used in Chemical Analysis Proce- dure Methods No. 2, 3, 4, and 6 (Table II), use chemical goggles or face shield, impervious gloves and an impervious apron. Concentrated acids should be han- dled only in an adequately ventilated lab- oratory ho
20、od. CAUTION: Always add acid to water. 4.7 In preparing ammonium hydroxide (8:92) for use in Chemical Analysis Pro- cedure Method No. 4 (Table II, 70% sul- furic acid), use chemical goggles or face shield, impervious gloves and an imper- vious apron. Dispense, mix and handle ammonium hydroxide only
21、in an ade- quately ventilated laboratory hood. 4.8 An eyewash/safety shower should be located nearby and a self-contained breathing apparatus should be readily available for emergency use. 4.9 Exposure to chemicals used in this procedure must be controlled at or below levels set by governmental auth
22、orities (e.g., Occupational Safety and Health Administrations 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 (AC- GIH) Threshold Limit Values (TLVs) comprised of time weighted averages
23、(TLV-TWA), short term exposure limits (TLV-STEL) and ceiling limits (TLV-C) AATCC Test Method 20A-2005 Fiber Analysis: Quantitative Copyright 2005 American Association of Textile Chemists and Colorists 58TM 20A-2005AATCC Technical Manual/2006 are recommended as a general guide for air contaminant ex
24、posure which should be met (see 17.17). 5. Apparatus 5.1 Analytical balance, capable of weighing to 0.1 mg. 5.2 Oven, maintained at 105-110C. 5.3 Desiccator, containing anhydrous silica gel, calcium sulfate (such as Drie- ite) or its equivalent. 5.4 Soxhlet extractor, 200 mL capacity. 5.5 Constant t
25、emperature bath, adjust- able, capable of controlling temperature to 1C. 5.6 Weighing bottle, 100 mL capacity, glass, with ground glass cover. (Alter- nate: aluminum weighing can; same size, tight cover.) 5.7 Erlenmeyer flask, 250 mL capacity, ground glass stopper. 5.8 Beaker, borosilicate heat resi
26、stant glass, 250 mL capacity. 5.9 Filtering crucible, fritted glass, coarse porosity, 30 mL. 5.10 Suction flask, with adapter, to hold filtering crucible. 5.11 Weighing bottle, large enough to hold filtering crucible. 5.12 Microscope, equipped with a moveable stage and a cross-hair ocular, 200-250X
27、magnification. 5.13 Projection microscope, capable of 500X magnification (see 17.12). 5.14 Fiber cutter: A device comprised of two razor blades, a threaded pin and an assemblage that will hold the blades rigidly in position. The device is operated by applying pressure vertically down- ward. It cuts
28、fibers approximately 250 m in length (see 17.3). 5.15 Wedge scale: Strips of heavy pa- per or Bristol board imprinted with a wedge for use at 500X magnification (see 17.4). 6. Reagents 6.1 Ethyl alcohol (95%), pure or dena- tured. 6.2 Fluorocarbon 113 (such as Freon TF) or hydrochlorofluorocarbon (s
29、uch as Genesolve 2000). 6.3 Hydrochloric acid (HCl), 0.1N. 6.4 Enzyme solubilizing preparation. 6.5 Acetone (CH3COCH3), reagent grade. 6.6 Hydrochloric acid (HCl) (20%). Dilute HCl, sp gr 1.19, with water until the specific gravity of the solution is 1.10 at 20C. 6.7 Sulfuric acid (H2SO4) (59.5%). A
30、dd H2SO4, sp gr 1.84, slowly to water. After the solution has cooled to 20C, ad- just the density to a value between 1.4902 and 1.4956 g/mL. 6.8 Sulfuric acid (H2SO4) (70%). Add H2SO4, sp gr 1.84, slowly to water. After the solution has cooled to 20 1C, ad- just the density to a value between 1.5989
31、 and 1.6221 g/mL (see 17.18). 6.9 Sulfuric acid (H2SO4) (1:19). Slowly stir 1 volume of H2SO4, sp gr 1.84, into 19 volumes of water. 6.10 Sodium hypochlorite (NaOCl). Prepare a solution of NaOCl, 5.25% available chlorine. Sodium hypochlorite based household bleach (nominally 5.25%) has been found to
32、 be acceptable. 6.11 Sodium bisulfite (NaHSO3) (1%). Freshly prepared. 6.12 Formic acid (HCOOH) (90%), sp gr of 1.202 at 20C. 6.13 Ammonium hydroxide (NH4OH) (8:92). Mix 8 volumes of NH4OH, sp gr 0.90, with 92 volumes of water. 6.14 Herzberg stain. Add the previ- ously prepared solution A to solutio
33、n B; allow to stand overnight; decant the clear liquid into a dark colored glass bottle and add a leaf of iodine. Solution ASolution B Zinc Chloride50 gPotassium Iodide5.5 g Water25 mLIodine0.25 g Water12.5 mL 7. Sampling 7.1 It is not possible to give specific in- structions for taking a laboratory
34、 test sample from all types of textile materials to which these methods may be applica- ble; but a few general recommendations will be given. 7.1.1 The sample should be as repre- sentative as possible of the lot of material from which it was taken. 7.1.2 If a reasonably large lot is avail- able, and
35、 if it is possible to do so, sam- plings should be taken from different, widely separated areas or parts of the lot. 7.1.3 In the case of fabrics where there is a definite repetition in the pattern, the sample should include all yarns in a com- plete pattern (see 17.6). 7.1.4 In the case of yarns, n
36、ot less than a 2-meter length should be taken. Test Methods 8. Moisture Content 8.1 Procedure. Place not less than 1 g of the textile to be tested in a previously tared weighing bottle and immediately replace the cover. Weigh to the nearest 0.1 mg using the analytical balance and record the weight.
37、Place the uncovered weighing bottle containing the specimen in an oven maintained at 105-110C for 1.5 h. At the end of the time period, re- move the bottle from the oven, immedi- ately replace the cover and put it in the desiccator. When the bottle and contents have cooled to room temperature, remov
38、e them from the desiccator and reweigh. Repeat the heating and reweighing pro- cess for periods of 30 min until the weight is constant to within 0.001 g and record the constant weight. 8.2 Calculations. 8.2.1 Calculate the moisture content of the specimen as follows: where: M = moisture content, per
39、cent. A = weight of sample before drying + bottle. B = weight of sample after drying + bottle. T = tare weight of weighing bottle. 9. Nonfibrous MaterialClean Fiber Content 9.1 Procedure. Take a specimen of not less than 5 g, dry it to constant weight in an oven at 105-110C (see 8.1), record the ove
40、n-dry weight to the nearest 0.1 mg using an analytical balance and then sub- ject it to one, or more, of the following treatments, as appropriate. When specific type of nonfibrous content is known, only that specific treatment, or treatments, need be performed; otherwise, all treat- ments must be ap
41、plied. 9.1.1 Hydrochlorofluorocarbon Treat- ment (for removal of oils, fats, waxes, certain thermoplastic resins, etc.). Extract the dried specimen with hydrochlorofluo- rocarbon in a soxhlet extractor, siphoning over a minimum of six times. Air dry, and then dry at 105-110C to constant weight. For
42、an alternative to soxhlet ex- tractor, see 17.19. 9.1.2 Alcohol Treatment (for removal of soaps, cationic finishes, etc.). Extract the dried specimen with ethyl alcohol in a soxhlet extractor, siphoning over a mini- mum of six times. Air dry, and then dry at 105-110C to constant weight. For an al- t
43、ernative to soxhlet extractor, see 17.19. 9.1.3 Aqueous Treatment (for removal of water soluble materials). Immerse the dried specimen for 30 min in water at 50C using a 100:1 liquid to fabric ratio. Stir occasionally or use a mechanical shaker. Rinse 3 times in fresh portions of water and dry at 10
44、5-110C to constant weight. 9.1.4 Enzyme Treatment (for removal of starch, etc.). Immerse the dried speci- men in aqueous solution of the enzyme preparation following the manufacturers recommendations as to concentration, liquid to fabric ratio and temperature and time of immersion. Rinse thoroughly
45、with hot water and dry at 105-110C to constant weight. 9.1.5 Acid Treatment (for removal of amino resins). Immerse the dried speci- men in 100 times its weight of 0.1N HCl at 80C for 25 min, stirring occasionally. Rinse thoroughly with hot water and dry at 105-110C to constant weight. 9.2 Calculatio
46、ns. M AB AT - -=100 Copyright 2005 American Association of Textile Chemists and Colorists AATCC Technical Manual/2006TM 20A-200559 9.2.1 Calculate the nonfibrous content of the specimen as follows: where: N = nonfibrous materials, percent. C = dry weight, specimen, before treatment. D = dry weight,
47、specimen, after treat- ment. 9.2.2 Calculate the clean fiber content of the specimen as follows: where: F = clean fiber content, percent; other terms as in 9.2.1 10. Mechanical Separation 10.1 Procedure. Remove the non- fibrous materials using the appropriate treatment (see 9.1). Separate the compo-
48、 nent yarns by mechanical dissection; combine those yarns, or plies, having the same fiber composition and determine N CD C - -100= F D C - -100= the oven-dry weight of each generic type present. 10.2 Calculation. Calculate the content of each generic fiber as follows: where: Xi= content of fiber i,
49、 percent. Wi= oven-dry weight of fiber i, after separation. E = weight of clean, oven-dry speci- men taken for analysis. 11. Chemical AnalysisGeneral 11.1 Specimen Preparation. Before analyses are undertaken, the laboratory test sample should be disintegrated, ho- mogenized and a portion of the homoge- nate taken for the chemical treatment(s). In the case of a fabric, one should un- ravel it into its individual yarns, cut the yarns into lengths not greater than 3 mm, thoroughly mix the cut pieces a