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1、BRITISH STANDARD BS EN ISO 14184-2:1998 Textiles Determination of formaldehyde Part 2: Released formaldehyde (vapour absorption method) The European Standard EN ISO 14184-2:1998 has the status of a British Standard ICS 59.080.01 BS EN ISO 14184-2:1998 This British Standard, having been prepared unde
2、r the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 1998 BSI 02-2000 ISBN 0 580 30743 3 National foreword This British Standard is the English language version of EN ISO 14184-2:1998. I
3、t is identical with ISO 14184-2:1998. Attention is drawn to BS 6806-3:1987 Formaldehyde in textiles Part 3: Method for determination of released formaldehyde, which uses a different methodology from BS EN ISO 14184-2 and is declared obsolescent. The UK participation in its preparation was entrusted
4、to Technical Committee TCI/25, Chemical properties, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related int
5、ernational and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be fou
6、nd in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standard
7、s are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, pages 2 to 9 and a back cover. This sta
8、ndard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No.DateComments BS EN ISO 14184-2:1998 BSI 02-2000i Contents Page National forewordInside front cove
9、r Foreword2 Text of EN ISO 14184-23 ii blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14184-2 August 1998 ICS 59.080.10 Descriptors: Textiles, chemical analysis, determination of content, formaldehyde, quantitative analysis, absorption English version Textiles Determination of formal
10、dehyde Part 2: Released formaldehyde (vapour absorption method) (ISO 14184-2:1998) Textiles Dosage du formaldhyde Partie 2: Formaldhyde dgag (Mthode par absorption de vapeur) (ISO 14184-2:1998) Textilien Bestimmung des Gehaltes an Formaldehyd Teil 2: Freigesetzter Formaldehyd (Wasserdampf-Absorption
11、s-Verfahren) (ISO 14184-2:1998) This European Standard was approved by CEN on 2 May 1998. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date li
12、sts and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the resp
13、onsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Ne
14、therlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any mea
15、ns reserved worldwide for CEN national Members. Ref. No. EN ISO 14184-2:1998 E EN ISO 14184-2:1998 BSI 02-2000 2 Foreword The text of EN ISO 14184-2:1998 has been prepared by Technical Committee CEN/TC 248 “Textiles and textile products”, the secretariat of which is held by BSI, in collaboration wit
16、h Technical Committee ISO/TC 38 “Textiles”. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 1999, and conflicting national standards shall be withdrawn at the latest by January 1999. Accor
17、ding to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal
18、, Spain, Sweden, Switzerland and the United Kingdom. Contents Page Foreword2 1Scope3 2Normative references3 3Principle3 4Reagents3 5Apparatus3 6Preparation of standard solution and calibration4 7Test specimens4 8Procedure5 9Calculation5 10Test report5 Annex A (normative) Standardization of formaldeh
19、yde stock solution7 Annex B (informative) Alternative procedure using chromotropic acid7 Annex C (informative) Information on accuracy of the test8 Figure 1 Wire mesh basket (aluminium) (on left) which is suspended in a sealed jar with one specimen as shown on the right6 Table C.1 Critical differenc
20、es for zero formaldehyde8 Table C.2 Critical differences for low level formaldehyde9 EN ISO 14184-2:1998 BSI 02-20003 WARNING. This standard calls for the use of substances and/or procedures that may be injurious to health if adequate precaution are not taken. It refers only to technical suitability
21、 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 standard that the execution of its provisions is entrusted to appropriately qualified and experienced people. 1 Scope This standard specifies a method for det
22、ermining the amount of formaldehyde released under the conditions of accelerated storage from textiles in any form by means of a vapour absorption method. The procedure is intended for use in the range of releasable formaldehyde on the fabric between 20 mg/kg and 3 500 mg/kg when determined by this
23、method. The lower limit is 20 mg. Below this limit the result is reported as “not-detectable”. A method for determination of free formaldehyde and formaldehyde extracted partly through hydrolysis in aqueous solution is given in ISO 14184-1. 2 Normative references This European Standard incorporates
24、by dated and undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European st
25、andard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. ISO 139, Textiles Standard atmospheres for conditioning and testing. ISO 3696, Water for analytical laboratory use Specification and test methods. 3 Princip
26、le A weighed fabric specimen is suspended over water in a sealed jar. The jar is placed in an incubator at a controlled temperature for a specified length of time. The amount of formaldehyde absorbed by the water is then determined colorimetrically. 4 Reagents All reagents shall be of analytical rea
27、gent quality. 4.1 Distilled water or water complying with grade 3 of ISO 3696. 4.2 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
28、 to the mark with water (4.1). Store in a brown bottle. NOTEThe reagent darkens in colour slightly on standing over the first 12 h. For this reason the reagent should be held 12 h before use. Otherwise, the reagent is usable over a considerable period of time, at least 6 weeks. However, since the se
29、nsitivity may change slightly over a long period of time, it is good practice to run a calibration curve weekly to correct for slight changes in the standard curve. As an alternative the chromotropic acid method described in Annex B may be used. 4.3 Formaldehyde solution, approximately 37 % (W/V or
30、W/W). 5 Apparatus 5.1 Glass preserving jars, 0,95 l to 1,0 l with gas tight sealing caps (see Figure 1). 5.2 Small wire mesh baskets (or other suitable means for suspending the test specimen above the water level inside the jars. As an alternative to the wire mesh baskets, a double strand of sewing
31、thread may be used to make a loop in the test specimen that has been folded in half twice, suspended above the water level. The two double-thread ends are draped over the top of the jar and held securely by the jar cap. NOTEA simple support for insertion in the preserving jars can be constructed as
32、follows: A piece of aluminium wire screening 15,2 cm 14,0 cm is bent around a length of wood 3,8 cm square and fastened together to form a rectangular, open-ended cage. One side is cut at the corners about halfway up the side and the cut section folded inward and fastened. This folded piece forms th
33、e bottom of the wire basket while the other three sides form the support legs. Fastening can be accomplished by twisting short lengths of wire through or around the appropriate part. EN ISO 14184-2:1998 4 BSI 02-2000 5.3 Incubator, thermostatically controlled at (49 2) C. 5.4 Stoppered volumetric fl
34、asks, 50 ml, 250 ml, 500 ml and 1 000 ml. 5.5 Pipettes, 1 ml, 5 ml, 10 ml, 15 ml, 20 ml, 25 ml, 30 ml and 50 ml volumetric and 5 ml graduated. NOTEAn automatic pipette system of the same accuracy as manual pipettes may be used. 5.6 Burettes, 10 ml and 50 ml. 5.7 Photoelectric colorimeter or spectrom
35、eter (wavelength 412 nm). 5.8 test tubes, colorimeter tubes, or spectrometer tubes. 5.9 Water bath at (40 2) C. 5.10 Balance, accurate to 0,2 mg. 6 Preparation of standard solution and calibration 6.1 Preparation Prepare an approximately 1 500 mg/l stock solution of formaldehyde by diluting 3.8 ml o
36、f formaldehyde solution (4.3) to one litre with water (4.1). Determine the concentration of formaldehyde in the stock solution by the method given in Annex A. Record the accurate concentration of this standardized stock solution. This stock solution will keep for up to four weeks and is used to prep
37、are standard dilutions. 6.2 Dilution The equivalent concentrations of the formaldehyde in the test specimen, based on the mass of 1 g of the test specimen and 50 ml of water, will be 50 times the accurate concentrations of the standard solutions. 6.2.1 Preparation of the standard-solution (S2) Dilut
38、e 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 75 mg/l of formaldehyde. 6.2.2 Preparation of the calibration-solutions Dilute calibration solutions from the standard solution
39、(S2), by diluting with water (4.1) in 500 ml volumetric flasks, using a minimum of five solutions from the following: Calculate the first order regression curve of the type y = a + bx. This regression curve will be used for all measurements. If the test specimens contains a higher amount of formalde
40、hyde than 500 mg/kg dilute the sample solution. NOTEThis double-dilution is necessary to have the same formaldehyde concentrations in the calibration solutions as in the test solutions of the fabrics. If the fabric contains 20 mg/kg formaldehyde, a 1,00 g specimen is extracted with 50 ml water; the
41、solution contains 20 4g formaldehyde and from this follows, 1 ml of the test solution contains 0,4 4g of formaldehyde. 7 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 sampl
42、e Prior to test store the sample sealed in a container. From the sample cut at least two specimens into small pieces and weigh approximately one gram of the pieces to an accuracy of 10 mg. 1 ml S2 to 500 ml, containing 0,15 4g CH2O/ml N7,5 mg/kg CH2O on the fabric 2 ml S2 to 500 ml, containing 0,30
43、4g CH2O/ml N 15 mg/kg CH2O on the fabric 5 ml S2 to 500 ml, containing 0,75 4g CH2O/ml N 37,5 mg/kg CH2O on the fabric 10 ml S2 to 500 ml, containing 1,50 4g CH2O/ml N 75 mg/kg CH2O on the fabric 15 ml S2 to 500 ml, containing 2,25 4g CH2O/ml N112,5 mg/kg CH2O on the fabric 20 ml S2 to 500 ml, conta
44、ining 3,00 4g CH2O/ml N150 mg/kg CH2O on the fabric 30 ml S2 to 500 ml, containing 4,50 4g CH2O/ml N225 mg/kg CH2O on the fabric 40 ml S2 to 500 ml, containing 6,00 4g CH2O/ml N300 mg/kg CH2O on the fabric EN ISO 14184-2:1998 BSI 02-20005 NOTEStorage maybe in a polyethylene bag and wrapped in alumin
45、ium foil. The reason for the storage precaution is that formaldehyde may diffuse through the pores of the bag. In addition, catalysts, or other compounds present in a finished, unwashed fabric may react with the foil if in direct contact. 8 Procedure Place 50 ml of water (4.1) in the bottom of each
46、jar. Suspend one specimen above the water in each jar, using a wire mesh basket or other means. Seal the jars and place them in the incubator (5.3) at (49 2) C for 20 h 15 min. Remove and cool the jars for (30 5) min and remove the specimen and baskets, or other support, from the jars. Recap the jar
47、s and shake them to mix any condensation formed on the jar sides. Pipette 5 ml of acetylacetone reagent (4.2) into a suitable number of tubes (5.8), and pipette 5 ml of the acetylacetone reagent into at least one additional tube for a reagent blank. Add 5 ml aliquots from each of the sample preservi
48、ng jars to the tubes and 5 ml of water (4.1) to the tube which is used as a reagent blank. Mix and place the tubes in a water bath (5.8) at (40 2) C for (30 5) min. Cool and read the absorbance in the colorimeter or spectrometer against the reagent blank using a wavelength of 412 nm in a 10 mm absor
49、ption cell. Determine the 4g/ml formaldehyde in the sample solutions using the prepared calibration curve. If it is anticipated that the fabrics have formaldehyde release levels of more than 500 mg/kg, or if the calculated levels from the test using the 5 : 5 ratio are more that 500 mg/kg dilute the extract to give absorbance in the range of the calibration curve (the dilution factor shall be taken into account when calculating the results). CAUTION. Exposure of the developed yellow colour to direct sunlight for a p