1、CGSB CAN/CGSB-4=2 N0=73*4-M71 * 1874650 0011731 7BT M C ANICGSB-4.2 NATIONAL STANDARD OF CANADA Nom 73m49M9lI IS0 2916:1975 Textile Test Methods Wool - Determination of Alkali Content this remains the continuing responsibility of the accredited standards-writing organization. Those who have a need t
2、o apply standards are encouraged to use National Siandards of Canada whenever practicable. These standards are subject to periodic review; therefore, users are cautioned to obtain the latest edition from the organization preparing the standard. The responsibility for approving National Standards of
3、Canada rests with the: Standards luncil of Canada 350 Sparks Street Ottawa, Ontario K1P 6N7 4ow to order -3 Publications: by Telephone - (819) 956-0425 or - (819) 956-0426 by Fax - (819) 956-5644 by Mail - CGSB, Sales Unit Ottawa, Canada K1A 1G6 11 Laurier Seet Hull, Quebec in Person - Place du Port
4、age ii, 9C1 Copyright Canadian General Standards Board Provided by IHS under license with CGSBNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-NATIONAL STANDARD OF CANADA C AN/CGSB-4.2 NO. 73.4-M91/ IS0 2916:1975 TEXTILE TEST METHODS WOOL - DETERMINATION OF ALKALI C
5、ONTENT Prepared by the International Organization for Standardization Reviewed by the Canadian General Standards Board es Approved by the Standards Council of Canada Published June 1991 by the Canadian General Standards Board Ottawa, Canada K1A 1G6 Minister of Supply and Services Canada - 1991 No pa
6、rt of this publication may be reproduced in any form without the prior permission of the publisher. Copyright Canadian General Standards Board Provided by IHS under license with CGSBNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-CGSB CAN/CGSB-4.2 N0.73.4-M9L * L87
7、4b50 OOLL934 b99 CANADIAN GENERAL STANDARDS BOARD COMMITTEE ON TEXTILE TEST METHODS Crown, Dr. E.M. Chairperson Biron, C. Cadieux, J. Carrick, Mrs. D. Clarke, Mrs. N. Cosman, Ms. V. Demers, A. Dolhan, Mrs. P. Duhamel, Ms. D. Edwards, D.S. Farnworth, Dr. B. Graham, M. Grgoire, Miss M. Hurley, Ms. M.
8、Kasem, Dr. M.A. King, Dr. M. Klimes, A. Mitton, Miss M.T. Monk, W.B. Mortimer, R.A. Muniak, Ms. E. Patel, A. Rashid, M.A. Ronsyn, Dr. C. Routhier, D. Scrafton, Ms. K. Randall, Mrs. J. Secretary (Membership at date of approval) University of Alberta Celanese Canada Inc. Royal Canadian Mounted Police
9、Department of National Defence Du Pont Canada Inc. Department of Consumer and Corporate Affairs Professional Association of Cleaners and Launderers of Quebec Department of National Defence Textile Technology Centre Canadian Carpet Institute Mustang Industries Inc. The Wool Bureau of Canada Ltd. Domi
10、nion Fabrics Inc. Department of National Revenue (Customs and Excise) Department of Consumer and Corporate Affairs University of Manitoba Dominion Textile Inc. Consultant Consultant ORTECH International The T. Eaton Company Canada Ltd. Sears Canada Inc. Department of Public Works, Alberta Department
11、 of Supply and Services Consoltex Inc. The Retail Research Foundation of Canada Canadian General Standards Board Acknowledgment is made for the French translation of this National Standard of Canaa by the Translation Bureau of the Department of the Secretary of State. CANKGSB-4.2 NO. 73.4-M91/ IS0 2
12、916:1975 Copyright Canadian General Standards Board Provided by IHS under license with CGSBNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-National Standard of Canada I Ottawa Canada KiA lG6 TEXTILE TEST METHODS NO. 73.4-M91/ IS0 2916:1975 Preface to the National S
13、tandard of Canada I CAN/CGSB-4.2 This National Standard of Canada has been prepared by the CGSB Committee on Textile Test Methods. It is identical in content and in layout with the International Standard IS0 2916, Wool - Determination of alkali content, published 1975-07-01 by the International Orga
14、nization for Standardization QSO). The international standard was reviewed by the CGSB committee to determine its suitability for Canadian use. It was agreed to use it in total, without editorial changes. A Canadian Note has been added to correct an apparent typographical error in the Annex to the S
15、tandard. Throughout this standard, the words ?National Standard of Canada? are to be understood as replacing the words ?International Standard? wherever they appear. e Some terminology and conventions are not identical to those used in other test methods within CAN/CGSB-4.2-M - Textile Test Methods.
16、 For example, the comma is used throughout this standard as a decimal marker rather than the point. The testing and evaluation of a product against this method may require the use of materials and/or equipment that could be hazardous. This document does not purport to address all the safety aspects
17、associated with its use. Anyone using this method has the responsibility to consult the appropriate authorities and to establish appropriate health and safety practices in conjunction with any existing applicable regulatory requirements prior to its use. The referenced international standard may be
18、obtained from the Standards Council of Canada, Standards Sales Branch, 350 Sparks Street, Suite 1200, Ottawa, Ontario K1P 6N7. Copyright Canadian General Standards Board Provided by IHS under license with CGSBNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- INTERNA
19、TIONAL STANDARD IS0 2916-1975 (E) . Wool - Determination of alkali content O INTRODUCTION This International Standard is based on the IWO test method 21-69 drawn up by the International Wool Textile Organization. 1 SCOPE AND FIELD OF APPLICATION This International Standard specifies a method for the
20、 determination of the alkali content of wool. The method is applicable to undyed wool in any form; for example, loose fibres, card sliver, tops, yarn or fabric. It can be used with dyed wool if the amount of dye extracted in the course of the test does not affect the determination of the end-point o
21、f the titration. 2 PRINCIPLE Extraction of the alkali from a weighed quantity of wool by immersion in dilute boric acid solution. Determination of the amount of alkali extracted, by titration with a standard volumetric solution of hydrochloric acid. 3 REAGENTS 3.1 Boric acid solution. Dissolve 10 g
22、of boric acid (analytical reagent grade) in 1 I of distilled water. 3.2 Hydrochloric acid, N120 solution. Standardize this solution by titration with freshly standardized sodium hydroxide solution. 3.3 Mathyl red - Methylene blue indicator : a) A 1 gll solution of methyl red in absolute ethanol. b)
23、4 ml of a 10 g/l aqueous solution of methylene blue mixed with 96 ml of ethanol with warming. 4 APPARATUS 4.1 qonical flasks with glass stoppers, capacity 250 ml. 4.2 Erlenmeyer flasks, capacity 250 ml. 4.3 Microburette.2 ml. 4.4 Pipettes, 50 and 100 ml. 4.5 Weighing bottle with lid. 4.6 Sintered-gl
24、ass crucible, with pore diameter between 100 and 160 wm. 4.7 Analytical balance, accurate to 0,000 5 g. 4.8 Desiccator. 4.9 Oven for drying samples at 105 * 2 “C. 4.10 Mechanical shaking device (optional). 5 SAMPLING AND PREPARATION OF TEST SPECIMENS Take a representative sample of mass not less tha
25、n 10 g from the material to be tested. If the dichloromethane extract of the sample is greater than 1 %, degrease with dichloromethane as follows : Extract the sample with dichloromethane for 1 h in a Soxhlet apparatus, at the minimum rate of 6 cycles per hour. Evaporate the dichloromethane from the
26、 cleaned sample and remove all vegetable matter and foreign substances from the wool. If the sample is yarn or cloth, dissect into short lengths of yarn (approximately 1 cm) and leave to attain equilibrium with the laboratory atmosphere. Felted materials that cannot be dissected into yarn must first
27、 be cut up into small pieces. Ne. 7S4M91 1 Copyright Canadian General Standards Board Provided by IHS under license with CGSBNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 2916-1975 (E) Take from the cleaned, or uncleaned, sample, as the case may be, at least
28、two representative test specimens each of mass 2 i 0,001 g and one representative test specimen of mass 1 f 0,001 g for determining the dry mass. 6 TEST PROCEDURE 6.1 Determination of dry mass Transfer the test specimen of mass 1 f 0.001 g to the weighing bottle (4.5) and dry it in the drying oven (
29、49) at 105 * 2 OC. Stopper the bottle, allow it to cool in the desiccator (4.8). remove and determine its mass. Repeat these drying and mass determination operations until constant mass has been attained.” Remove the test specimen, determine the mass of the weighing bottle and hence determine the dr
30、y mass of the test specimen. hlculate by proportion the dry mass of the other test specimens. 6.2 Determination of alkali content Place each of the other test specimens in a conical flask (4.1) and add by pipette (4.4) 100 ml of boric acid solution (3.1). Stopper the flasks and either shake for 2 h
31、on the mechanical shaker (4.10) or allow to stand overnight after first shaking by hand to wet out the wool. Decant the liquid from the wool and filter through the sinteredglass crucible (4.6) in order to remove fibre fragments. Transfer by pipette (4.4) 50 ml of the filtered liquid to an Erlenmeyer
32、 flask (4.2) and titrate with the N120 hydrochloric acid solution (3.2). using 3 drops of methyl red and 3 drops of methylene blue solutions (3.3) as indicator. Carry out a titration on each extract and obtain the mean volume of N/20 hydrbchloric acid solution used in the two titrations. 7 EXPRESSIO
33、N OF RESULTS The mass of the alkali present in the wool, expressed as a percentage of the dry mass of the wool, is given by the formula : % TxVxk Alkali content =- m where i is the normality of the hydrochloric acid solution used; V is the volume, in millilitres, of the hydrochloric acid solution us
34、ed (mean of two titrations); k is a constant; m is the dry mass, in grams, of the dried test specimen. The value of k depends on the form ir1 which the alkali content is to be expressed; it is 5,3 if the alkali content is expressed as sodium carbonate; 4.0 if the alkali content is expressed as sodiu
35、m hydroxide; 3.1 if the alkali content is expressed as sodium oxide. 8 TESTREPORT The test report shall include the following particulars : a) that the procedure was conducted in accordance with this International Standard; b) the results for each test specimen obtained using the formula in clause 7
36、 and the method of expression used; c) any unusual features noted during the determi- nation; d) any operation not included in this International Standard, or regarded as optional. No. 73.4-M91 2 1) Constant mass IS reached when the mass of a sample does not change by more than 1 mg after repeated d
37、rying for at least 30 min. Copyright Canadian General Standards Board Provided by IHS under license with CGSBNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-CGSB CANICGSB-4-2 N0-73-4-flqL tf 1874650 0011938 234 = 0,019 IS0 2916-1975 (E) 0,018 0,023 ANNEX ACCURACY O
38、F THE METHOD content An interlaboratory trial was carried out by a Working Group using three wools of different alkali contents. Nine laboratories participated. The statistical evaluation of the resulting 3 X 9 X 2 values (each laboratory carried out a double test on each wool) produced the values s
39、ummarized in the following table. I I Wwl A I Wool B I Wool C I 0.23 I 0.35 1 0.60 I Mean alkali Content of the r rested wool, % Estimated values for the interlaboratory component of variation sL, % alkali content Estimated values for the I I I I interlaboratory component I 0,003ol 0.004 i I 0.00681
40、 I of variation SR, % alkali These data enable an estimation to be made of the confidence limits to be expected in a determination of alkali content according to the method specified. A.l CONFIDENCE LIMITS FOR THE RESULTS OF ONE LABORATORY If the interlaboratory variance is not taken into considerat
41、ion (cornparison within one laboratory), the confidence limits, Ti, of the mean for the laboratory are calculated with 95 % statistical significance (5 % probability of error) using the formula : SR Ti = * 2-% alkali content Jk where k is the number of tests from which the mean was calculated. An es
42、timated numerical value for SR in relation to the mean alkali content, taken from the above table by approximate interpolation if necessary, is inserted in the above formula. A.2 CONFIDENCE LIMITS TAKING INTO ACCOUNT THE VARIATION BETWEEN LABORATORIES If the variance between laboratories is taken in
43、to account (comparison between different laboratories), then the confidence limits, TL, of the mean are calculated with 95 % statistical significance (5 % probability of error) using the formula : 22 i ixk -+ SL - SR % alkali content in which the participating i laboratories each carried out k tests
44、. When i = 1, the confidence limits for individual laboratories with interlaboratory variance taken into account are obtained. Approximate numerical values for SL and SR are obtained from the above table. *Canadian Note: For the word “interlaboratory” read “intraiaboratory.” NO. 73.4-M91 3 Copyright Canadian General Standards Board Provided by IHS under license with CGSBNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
