1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 14184-1:2011Textiles Determination offormaldehydePart 1: Free and hydrolised formaldehyde(water extraction method) (ISO14184-1:2011)BS EN ISO 14184-1:2011 BRITISH STAND
2、ARDNational forewordThis British Standard is the UK implementation of EN ISO14184-1:2011. It supersedes BS EN ISO 14184-1:1999 which iswithdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee TCI/80, Chemical testing of textiles.A list of organizations represented on thi
3、s committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 69627 5ICS 59.080.01Compliance with a British Standard cannot confer immunity fromle
4、gal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 August 2011.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14184-1 August 2011 ICS 59.080.01 Supersedes EN ISO 14
5、184-1:1998English Version Textiles - Determination of formaldehyde - Part 1: Free and hydrolised formaldehyde (water extraction method) (ISO 14184-1:2011) Textiles - Dosage du formaldhyde - Partie 1: Formaldhyde libre et hydrolys (mthode par extraction deau) (ISO 14184-1:2011) Textilien - Bestimmung
6、 des Gehaltes an Formaldehyd - Teil 1: Freier und hydrolisierter Formaldehyd (Wasser-Extraktions-Verfahren) (ISO 14184-1:2011) This European Standard was approved by CEN on 14 August 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for gi
7、ving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three of
8、ficial versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies
9、of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdo
10、m. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14184-1:2011: EBS
11、 EN ISO 14184-1:2011EN ISO 14184-1:2011 (E) 3 Foreword This document (EN ISO 14184-1:2011) has been prepared by Technical Committee ISO/TC 38 “Textiles“ in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” the secretariat of which is held by BSI. This European Standar
12、d shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2012, and conflicting national standards shall be withdrawn at the latest by February 2012. Attention is drawn to the possibility that some of the elements of t
13、his document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 14184-1:1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following cou
14、ntries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slo
15、venia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 14184-1:2011 has been approved by CEN as a EN ISO 14184-1:2011 without any modification. BS EN ISO 14184-1:2011ISO 14184-1:2011(E) ISO 2011 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normati
16、ve references1 3 Principle1 4 Reagents.1 5 Apparatus.2 6 Preparation of standard solution and calibration 2 7 Preparation and conditioning of test specimens.3 8 Procedure.4 9 Calculation and expression of the results4 10 Test report5 Annex A (normative) Standardization of formaldehyde stock solution
17、6 Annex B (informative) Information on accuracy of the method.8 BS EN ISO 14184-1:2011ISO 14184-1:2011(E) iv ISO 2011 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing
18、 International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liais
19、on with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of te
20、chnical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is dr
21、awn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 14184-1 was prepared by Technical Committee ISO/TC 38, Textiles. This second edition cancels and replaces the fi
22、rst edition (ISO 14184-1:1998), of which it constitutes a minor revision. ISO 14184 consists of the following parts, under the general title Textiles Determination of formaldehyde: Part 1: Free and hydrolysed formaldehyde (water extraction method) Part 2: Released formaldehyde (vapour absorption met
23、hod) BS EN ISO 14184-1:2011INTERNATIONAL STANDARD ISO 14184-1:2011(E) ISO 2011 All rights reserved 1Textiles Determination of formaldehyde Part 1: Free and hydrolysed formaldehyde (water extraction method) WARNING This part of ISO 14184 calls for the use of substances and/or procedures that may be i
24、njurious to health if adequate precautions are not taken. It refers only to technical suitability and does not absolve the user from legal obligations relating to health and safety at any stage. It has been assumed in the drafting of this part of ISO 14184 that the execution of its provisions is ent
25、rusted to appropriately qualified and experienced people. 1 Scope This part of ISO 14184 specifies a method for determining the amount of free formaldehyde and formaldehyde extracted partly through hydrolysis by means of a water extraction method. The method can be applied to the testing of textile
26、samples in any form. The procedure is intended for use in the range of free and hydrolysed formaldehyde on the fabric between 16 mg/kg and 3 500 mg/kg when determined by this method. The lower limit is 16 mg/kg. Below this limit, the result is reported as “not detectable”. A method for determination
27、 of released formaldehyde is given in ISO 14184-2. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including
28、any amendments) applies. ISO 139:2005, Textiles Standard atmospheres for conditioning and testing ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 4793:1980, Laboratory sintered (fritted) filters Porosity grading, classification and designation 3 Principle Formal
29、dehyde is extracted from a textile sample with water at 40 C. The amount of formaldehyde is then determined colorimetrically. 4 Reagents All reagents shall be of analytical reagent quality. 4.1 Distilled water or grade 3 water complying with ISO 3696. BS EN ISO 14184-1:2011ISO 14184-1:2011(E) 2 ISO
30、2011 All rights reserved4.2 Acetylacetone reagent (Nash reagent). Dissolve 150 g of ammonium acetate in about 800 ml of water (4.1), add 3 ml of glacial acetic acid and 2 ml of acetylacetone, transfer into a 1 000 ml volumetric flask and make up to the mark with water (4.1). Store in a brown bottle.
31、 The reagent darkens in colour slightly on standing over the first 12 h. For this reason, the reagent should be held for 12 h before use. Otherwise, the reagent is usable over a considerable period of time, at least 6 weeks. Since the sensitivity may change slightly over a long period of time, it is
32、 good practice to run a calibration curve weekly to correct for slight changes in the standard curve. 4.3 Formaldehyde solution, approximately 37 % (M/V or M/m). 4.4 Ethanolic solution of dimedone. Prepare by dissolving 1 g of dimedone (dimethyl-dihydro resorcinol or 5,5-dimethyl-cyclohexanedione) i
33、n ethanol and by diluting the solution with ethanol to make 100 ml. Prepare immediately before use. 5 Apparatus 5.1 Stoppered volumetric flasks, 50 ml, 250 ml, 500 ml and 1 000 ml. 5.2 Flask, 250 ml, with a stopper. 5.3 Pipettes, 1 ml, 5 ml, 10 ml and 25 ml and graduated at intervals of 5 ml. NOTE A
34、n automatic pipette system of the same accuracy as manual pipettes can be used. 5.4 Burettes, 10 ml and 50 ml. 5.5 Spectrophotometer, capable of reading absorbance to a minimum of 3 decimal places at a wavelength of 412 nm. 5.6 Test tubes or spectrophotometer tubes. 5.7 Water bath, capable of mainta
35、ining a temperature of (40 2) C. 5.8 Filters, made from heat-resistant glass having a pore size between 40 m and 100 m (pore symbol P100 in accordance with ISO 4793). 5.9 Balance, accurate to 0,2 mg. 6 Preparation of standard solution and calibration 6.1 Preparation Prepare an approximately 1 500 mg
36、/l stock solution of formaldehyde by diluting 3,8 ml of formaldehyde solution (4.3) to 1 litre with water (4.1). Determine the concentration of formaldehyde in the stock solution by the standard method given in Annex A. Record the accurate concentration of this standardized stock solution. This stoc
37、k solution will keep for up to 4 weeks and is used to prepare standard dilutions. BS EN ISO 14184-1:2011ISO 14184-1:2011(E) ISO 2011 All rights reserved 36.2 Dilution The equivalent concentrations of the formaldehyde in the test specimen, based on a mass of 1 g of the test specimen and 100 ml of wat
38、er, will be 100 times the accurate concentration of the standard solutions. 6.2.1 Preparation of the standard solution (S2) Dilute 10 ml of the titrated standard solution (containing 1,5 mg/ml of formaldehyde), prepared in 6.1, with water (4.1) to 200 ml in a volumetric flask. This solution contains
39、 75 mg/l of formaldehyde. 6.2.2 Preparation of the calibration solutions Prepare calibration solutions from the standard solution (S2), by diluting with water (4.1) in 500 ml volumetric flasks, using a minimum of five solutions from the following: 1 ml of S2 to 500 ml, containing 0,15 g CH2O/ml = 15
40、 mg/kg CH2O on the fabric 2 ml of S2 to 500 ml, containing 0,30 g CH2O/ml = 30 mg/kg CH2O on the fabric 5 ml of S2 to 500 ml, containing 0,75 g CH2O/ml = 75 mg/kg CH2O on the fabric 10 ml of S2 to 500 ml, containing 1,50 g CH2O/ml = 150 mg/kg CH2O on the fabric 15 ml of S2 to 500 ml, containing 2,25
41、 g CH2O/ml = 225 mg/kg CH2O on the fabric 20 ml of S2 to 500 ml, containing 3,00 g CH2O/ml = 300 mg/kg CH2O on the fabric 30 ml of S2 to 500 ml, containing 4,50 g CH2O/ml = 450 mg/kg CH2O on the fabric 40 ml of S2 to 500 ml, containing 6,00 g CH2O/ml = 600 mg/kg CH2O on the fabric Calculate the firs
42、t-order regression curve of the type y = a + bx. This regression curve will be used for all measurements. If the test specimens contain a higher amount of formaldehyde than 500 mg/kg, dilute the sample solution. NOTE This double-dilution is necessary to have the same formaldehyde concentrations in t
43、he calibration solutions as in the test solutions of the fabrics. If the fabric contains 20 mg/kg of formaldehyde, a 1,00 g specimen is extracted with 100 ml of water; the solution contains 20 g of formaldehyde and from this it follows that 1 ml of the test solution contains 0,2 g of formaldehyde. 7
44、 Preparation and conditioning of test specimens Do not condition the test specimen because the predrying and humidity in connection with the conditioning may cause changes in the formaldehyde content of the sample. Prior to testing, store the sample in a container. NOTE Storage can be in a polyethyl
45、ene bag and wrapped in aluminium foil. The reason for the storage precaution is that formaldehyde might diffuse through the pores of the bag. In addition, catalysts, or other compounds present in a finished, unwashed fabric, can react with the foil if in direct contact. From the sample, cut two test
46、 specimens into small pieces, and weigh approximately 1 g of the pieces to an accuracy of 10 mg. If the formaldehyde content is low, increase the test specimen mass to 2,5 g in order to achieve a sufficient accuracy. For each test specimen, put the weighed pieces into a 250 ml flask with a stopper (
47、5.2) and add 100 ml of water (4.1). Stopper tightly and place in a water bath at (40 2) C for (60 5) min. Shake the flask at least every 5 min, ensuring that the specimens are entirely wet. Then filter the solution into another flask through a filter (5.8). BS EN ISO 14184-1:2011ISO 14184-1:2011(E)
48、4 ISO 2011 All rights reservedIf it is difficult to obtain completely wet specimens, a mechanical-shaking water bath should be used. In cases of dispute, use a conditioned parallel specimen to calculate a correction coefficient to be used in correcting the mass of the test specimen to be used for th
49、e test. Cut the test specimen from the sample, weigh it immediately and again after conditioning (in accordance with ISO 139). Use these values to calculate the correction coefficient to two integers and use the coefficient to calculate the conditioned mass of the test specimen used for the sample solution. 8 Procedure 8.1 Put 5 ml of the filtered test specimen solution in a tube (5.6) and 5 ml of the standard formaldehyde solutions in further tubes (5.6). Add 5 ml of acetylacetone reagent (4.2) in
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