DIN EN ISO 14184-1-2011 Textiles - Determination of formaldehyde - Part 1 Free and hydrolysed formaldehyde (water extraction method) (ISO 14184-1 2011) German version EN ISO 14184-.pdf

1、December 2011 Translation by DIN-Sprachendienst.English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 59.080.01!$xNP“1854345www.din.deDDIN EN ISO 14184-1Textiles Determination of formaldehyde Part 1: Free and hydrolysed formaldehyde (water extraction method)(ISO 14184-1:2011)English translation of DIN EN ISO 14184-1:2011-12Textilien Bestimmung des Gehaltes an Formaldehyd Teil 1: Freier und hydroli

3、sierter Formaldehyd (Wasser-Extraktions-Verfahren)(ISO 14184-1:2011)Englische bersetzung von DIN EN ISO 14184-1:2011-12Textiles Dosage du formaldhyde Partie 1: Formaldhyde libre et hydrolys (mthode par extraction deau)(ISO 14184-1:2011)Traduction anglaise de DIN EN ISO 14184-1:2011-12SupersedesDIN E

4、N ISO 14184-1:1999-02www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises pages11.1113DIN EN ISO 14184-1:2011-12 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 38 “Texti

5、les” (Secretariat: SAC, China/JISC, Japan) in collaboration with Technical Committee CEN/TC 248 “Textile and textile products” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), W

6、orking Committee NA 062-05-12 AA Textilchemische Prfver-fahren und Fasertrennung. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 139 DIN EN ISO 139 ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN EN ISO 14184-1:1999-02

7、as follows: a) the lower limit has been reduced to 16 mg/kg (see 1 Scope); b) the standard has been editorially revised. Previous editions DIN 54260: 1988-02 DIN EN ISO 14184-1: 1999-02 National Annex NA (informative) Bibliography DIN EN ISO 139, Textiles Standard atmospheres for conditioning and te

8、sting DIN ISO 3696, Water for analytical laboratory use Specification and test methods 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14184-1 August 2011 ICS 59.080.01 Supersedes EN ISO 14184-1:1998English Version Textiles - Determination of formaldehyde - Part 1: Free and hydrolised for

9、maldehyde (water extraction method) Textiles - Dosage du formaldhyde - Partie 1: Formaldhyde libre et hydrolys (mthode par extraction deau) (ISO 14184-1:2011) Textilien - Bestimmung des Gehaltes an Formaldehyd - Extraktions-Verfahren) (ISO 14184-1:2011) This European Standard was approved by CEN on

10、14 August 2011. 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 lists and bibliographical references concerning such national standards may

11、be obtained on application to the CEN-CENELEC Management Centre 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 responsibility of a CEN member into its own language and notified to

12、 the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxe

13、mbourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. 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

14、. EN ISO 14184-1:2011: E(ISO 14184-1:2011) Teil 1: Freier und hydrolisierter Formaldehyd (Wasser-EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Contents Page Foreword .3 1 Scope4 2 Normative references4 3 Principle4 4 Reagents.4 5 Apparatus.5 6 P

15、reparation of standard solution and calibration 5 7 Preparation and conditioning of test specimens.6 8 Procedure.7 9 Calculation and expression of the results7 10 Test report8 Annex A (normative) Standardization of formaldehyde stock solution9 Annex B (informative) Information on accuracy of the met

16、hod. 2DIN EN ISO 14184-1:2011-12 EN ISO 14184-1:2011 (E) 11Foreword 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 Euro

17、pean Standard 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 e

18、lements of this 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 f

19、ollowing countries 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, S

20、lovakia, Slovenia, 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. 3DIN EN ISO 14184-1:2011-12 EN ISO 14184-1:2011 (E) WARNING This part of ISO 14184 calls for the use of su

21、bstances and/or procedures that may be injurious 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 tha

22、t the execution of its provisions is entrusted 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 c

23、an be applied to the testing of textile 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

24、 detectable”. A method for determination 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 editio

25、n of the referenced document (including 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, classific

26、ation and designation 3 Principle Formaldehyde 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. 4DIN EN

27、ISO 14184-1:2011-12 EN ISO 14184-1:2011 (E) 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 to the mark with water (4.1). Stor

28、e in a brown bottle. 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 p

29、eriod of time, it is 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

30、-cyclohexanedione) in 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 inter

31、vals of 5 ml. NOTE An 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 bat

32、h, capable of maintaining 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 ap

33、proximately 1 500 mg/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

34、 solution. This stock solution will keep for up to 4 weeks and is used to prepare standard dilutions. 5DIN EN ISO 14184-1:2011-12 EN ISO 14184-1:2011 (E) 6.2 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

35、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

36、 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

37、 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

38、 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

39、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

40、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

41、 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

42、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

43、 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 (

44、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). 6DIN EN ISO 14184-1:2011-12 EN ISO 14184-1

45、:2011 (E) If 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 the test. Cut the test

46、 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

47、 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) into each tube and shake them. 8.2 Keep the test tubes first in a water bath at (40 2) C for (30 5) min and then at amb

48、ient temperature for (30 5) min. Take the solution of 5 ml of acetylacetone reagent solution in 5 ml of water having been treated in the same way as the blank reagent. Using a spectrophotometer (5.5), measure the absorbances in a 10 mm absorption cell at a wavelength of 412 nm against water (4.1). 8

49、.3 If it is anticipated that the fabrics have formaldehyde extraction levels of more than 500 mg/kg, or if the calculated levels from the test using a 5:5 ratio are more than 500 mg/kg, dilute the extract to give an absorbance in the range of the calibration curve (the dilution factor shall be taken into account when calculating the results). 8.4 To account for the effect of any impurities or discoloration in the test specimen solution, put 5 ml of the sample solution in a separate test tube, add 5 ml of