1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 17226-3:2011Leather Chemical determination of formaldehyde contentPart 3: Determination of formaldehyde emissions from leather (ISO 17226-3:2011)BS EN ISO 17226-3:2011
2、BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 17226-3:2011.The UK participation in its preparation was entrusted to Technical Committee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this committee can be obtained on re
3、quest to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. BSI 2011 ISBN 978 0 580 68694 8 ICS 59.140.30 Compliance with a British Standard cannot confer immunity from legal obligations.This Briti
4、sh Standard was published under the authority of the Standards Policy and Strategy Committee on 30 June 2011.Amendments issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17226-3 May 2011 ICS 59.140.30 English Version Leather - Chemical deter
5、mination of formaldehyde content - Part 3: Determination of formaldehyde emissions from leather (ISO 17226-3:2011) Cuir - Dosage chimique du formaldhyde - Partie 3: Dosage du formaldhyde mis par le cuir (ISO 17226-3:2011) Leder - Chemische Bestimmung des Formaldehydgehalts -Teil 3: Bestimmung der Fo
6、rmaldehydemissionen aus Leder (ISO 17226-3:2011) This European Standard was approved by CEN on 11 May 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 alterat
7、ion. 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 official versions (English, French, German). A version in any other language made b
8、y 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 of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
9、 Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISC
10、HES 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 17226-3:2011: EBS EN ISO 17226-3:2011 EN ISO 17226-3:2011 (E) 3 Foreword This document (EN ISO 172
11、26-3:2011) has been prepared by Technical Committee CEN/TC 289 “Leather”, the secretariat of which is held by UNI, in collaboration with the International Union of Leather Technologists and Chemists Societies. This European Standard shall be given the status of a national standard, either by publica
12、tion of an identical text or by endorsement, at the latest by November 2011, and conflicting national standards shall be withdrawn at the latest by November 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC
13、shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic,
14、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 the United Kingdom. BS EN ISO 17226-3:2011ISO 17226-3:2011(E) IULTCS/IUC 19-3
15、:2011(E) ISO 2011 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Principle .1 4 Reagents 1 4.1 Reagents for the formaldehyde stock solution1 4.2 Reagents for the HPLC method .2 5 Apparatus.2 6 Methods2 6.1 Procedure for the determination of formaldehyde in the st
16、ock solution 2 6.1.1 Preparation of the formaldehyde stock solution .2 6.1.2 Determination 3 6.2 Procedure for the determination of formaldehyde emission by the HPLC method .4 6.2.1 Shipment and storage leather for this method 4 6.2.2 Sampling 4 6.2.3 Determination of volatile matter 4 6.2.4 Determi
17、nation of formaldehyde emission.4 6.2.5 Reaction with DNPH4 6.2.6 HPLC conditions (recommendations).4 6.2.7 Calibration of HPLC.5 6.2.8 Calculation of the formaldehyde content in leather samples.5 7 Expression of results5 8 Test report6 BS EN ISO 17226-3:2011ISO 17226-3:2011(E) IULTCS/IUC 19-3:2011(
18、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 International Standards is normally carried out through ISO technical committees. Each member body int
19、erested 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 liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnic
20、al 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 technical committees is to prepare International Standards. Draft International Standards adopted by the
21、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 drawn to the possibility that some of the elements of this document may be the subject of patent rights.
22、ISO shall not be held responsible for identifying any or all such patent rights. ISO 17226-3 was prepared by the European Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, in collaboration with Chemical Test Commission of the International Union of Leather Technologists an
23、d Chemists Societies (IUC Commission, IULTCS), in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement). IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to further the advancement of leather science and technol
24、ogy. IULTCS has three Commissions, which are responsible for establishing international methods for the sampling and testing of leather. ISO recognizes IULTCS as an international standardizing body for the preparation of test methods for leather. ISO 17226 consists of the following parts, under the
25、general title Leather Chemical determination of formaldehyde content: Part 1: Method using high performance liquid chromatography Part 2: Method using colorimetric analysis Part 3: Determination of formaldehyde emissions from leather BS EN ISO 17226-3:2011INTERNATIONAL STANDARD ISO 17226-3:2011(E)IU
26、LTCS/IUC 19-3:2011(E) ISO 2011 All rights reserved 1Leather Chemical determination of formaldehyde content Part 3: Determination of formaldehyde emissions from leather 1 Scope This part of ISO 17226 specifies a method for determining the emission of formaldehyde from leathers. This method is based o
27、n high performance liquid chromatography (HPLC). It is selective and also allows the emission of other low molecular aldehydes and ketones to be observed. This part of ISO 17226 deals with the release of formaldehyde to the gas phase. Therefore, the obtained results are not comparable with the resul
28、ts of methods described in ISO 17726-1 and ISO 17226-2 which are based on extraction with liquid water. 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
29、latest edition of the referenced document (including any amendments) applies. ISO 2418, Leather Chemical, physical and mechanical and fastness tests Sampling location ISO 2419, Leather Physical and mechanical tests Sample preparation and conditioning ISO 3696:1987, Water for analytical laboratory us
30、e Specification and test methods ISO 4684, Leather Chemical tests Determination of volatile matter 3 Principle A specimen with defined dimensions is held above demineralized water in a sealed bottle and is heated at constant temperature for a specific period. Afterwards, the bottle is cooled and the
31、 formaldehyde absorbed into the water is analysed. The water is mixed with 2,4-dinitrophenylhydrazine, whereby aldehydes and ketones react to give the respective hydrazones. These are separated by means of a reversed-phase HPLC method, detected at 360 nm and quantified. 4 Reagents Use only reagents
32、of recognized analytical grade, unless otherwise stated. The water shall be of grade 3 in accordance with ISO 3696:1987. All solutions are aqueous solutions. 4.1 Reagents for the formaldehyde stock solution 4.1.1 Formaldehyde solution, approximately 37 % (mass fraction). BS EN ISO 17226-3:2011ISO 17
33、226-3:2011(E) IULTCS/IUC 19-3:2011(E) 2 ISO 2011 All rights reserved4.1.2 Iodine solution, 0,05 mol/l, i.e. 12,68 g iodine/l. 4.1.3 Sodium hydroxide solution, 2,0 mol/l. 4.1.4 Sulfuric acid solution, 2,0 mol/l. 4.1.5 Sodium thiosulfate solution, 0,1 mol/l. 4.1.6 Starch solution, 1 %, i.e. 1 g in 100
34、 ml water. 4.2 Reagents for the HPLC method 4.2.1 Dinitrophenylhydrazine (DNPH) solution, consisting of 0,3 g DNPH (2,4-dinitrophenylhydrazine) dissolved in 100 ml concentrated o-phosphoric acid (85 % mass fraction); (DNPH recrystallized from 25 % mass fraction, acetonitrile in water). 4.2.2 Acetoni
35、trile. 5 Apparatus Use usual laboratory equipment and, in particular, the following. 5.1 One (1) l polyethylene bottle with hook implement integrated in the lid (see Figure 1). Hook made of stainless steel with seals, positioned inside the lid of the test bottle. 5.2 Volumetric flasks, of capacities
36、 10 ml, 500 ml and 1 000 ml. 5.3 Erlenmeyer flasks, of capacities 100 ml and 250 ml. 5.4 Pipettes, of capacities 5 ml and 50 ml. 5.5 Oven, capable of being maintained at (60 2) C. 5.6 Analytical balance, weighing to an accuracy of 1 mg. 5.7 HPLC system with UV detection, e.g. 360 nm. 5.8 Press knife
37、, in accordance with ISO 2419, suitable for cutting specimens of (100 40) mm. 5.9 Hole punch for holes of 3 mm to 4 mm in diameter. 5.10 Membrane filter, polyamide, 0,45 m. 6 Methods 6.1 Procedure for the determination of formaldehyde in the stock solution 6.1.1 Preparation of the formaldehyde stock
38、 solution Pipette 5 ml of the formaldehyde solution (4.1.1) into a 1 000 ml volumetric flask (5.2) which contains approximately 100 ml water, then fill the flask with demineralized water up to the mark. This solution is the formaldehyde stock solution. BS EN ISO 17226-3:2011ISO 17226-3:2011(E) IULTC
39、S/IUC 19-3:2011(E) ISO 2011 All rights reserved 3Dimensions in millimetres Key 1 polyethylene bottle 2 sample 3 water Figure 1 Polyethylene bottle with specimen and water 6.1.2 Determination Pipette 10 ml from this solution into a 250 ml Erlenmeyer flask (5.3) and mix with the 50 ml iodine solution
40、(4.1.2). Add sodium hydroxide (4.1.3) until it turns yellow. Allow it to react for 15 min 1 min at a temperature between 18 C and 26 C, then add 15 ml of sulfuric acid (4.1.4) while swirling. After adding 2 ml of starch solution (4.1.6), titrate the excess iodine with sodium thiosulfate (4.1.5) unti
41、l the colour changes. Make three individual determinations. Titrate at least two blank solutions in the same manner. 011 FAFA()2VV cM= (1) where FAis the concentration of the formaldehyde stock solution, in milligrams per 10 ml (mg/10 ml); V0is the volume of the thiosulfate solution for the blank so
42、lution, in millilitres (ml); V1is the volume of the thiosulfate solution for the sample solution, in millilitres (ml); MFAis the relative molecular mass of formaldehyde, 30,02 g/mol; c1is the concentration of the thiosulfate solution, in moles per litre (mol/l). BS EN ISO 17226-3:2011ISO 17226-3:201
43、1(E) IULTCS/IUC 19-3:2011(E) 4 ISO 2011 All rights reserved6.2 Procedure for the determination of formaldehyde emission by the HPLC method 6.2.1 Shipment and storage leather for this method To avoid cross-contamination and loss of formaldehyde during shipment and storage, the leather samples should
44、be sealed in an inert gastight plastic bag. NOTE Multiple-layer polyethylene bags with a metal layer inside are appropriate. 6.2.2 Sampling Sample six specimens of (100 40) mm, selecting them in accordance with ISO 2418 and applying the press knife (5.8) in accordance with ISO 2419. Use five of thes
45、e specimens for the determination of formaldehyde emission. Use the sixth specimen for the determination of volatile matter. To fasten specimens 1 to 5, punch a hole of 3 mm to 4 mm near the centre and 10 mm from the upper edge in each one. 6.2.3 Determination of volatile matter If requested to calc
46、ulate the result on the basis of dry substance, use the sixth specimen to determine the volatile matter in accordance with ISO 4684. Do not grind or cut the specimen. 6.2.4 Determination of formaldehyde emission Weigh five of the specimens to 0,01 g. Pipette 50 ml aliquots of demineralized water int
47、o each of the 1 l polyethylene bottles which have to be clean and dry. Attach a specimen to each hook and seal the 5 bottles. Pipette 50 ml aliquots of demineralized water into an additional clean 1 l polyethylene bottle. Seal the bottle without a specimen. Use this bottle for a blank test. As soon
48、as the bottles have been sealed, store them for (180 15) min in a heated oven at (60 2) C. Remove the bottles from the oven and allow them to cool at room temperature for approximately 1 h. Then remove the leather specimens from the bottles and immediately analyse the formaldehyde absorbed in the wa
49、ter as described in 6.2.5. 6.2.5 Reaction with DNPH Pipette 4,0 ml of acetonitrile (4.2.2), a 5,0 ml aliquot of water from the polyethylene bottle (5.1) and 0,5 ml of DNPH solution (4.2.1) into a 10 ml volumetric flask (5.2). Fill the volumetric flask with demineralized water up to the mark and shake it briefly by hand to mix the components. Allow it to stand at least 60 min, but not more than 180 min. After filtering through a membrane filter (5.10), analyse the sample using HPLC. If the concentration is
