1、BS EN ISO27587:2009ICS 59.140.30NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDLeather Chemicaltests Determinationof the freeformaldehyde inprocess auxiliaries(ISO 27587:2009)This British Standard was published under the authority of the Standards Policy and St
2、rategy Committee on 31January 2010 BSI 2010ISBN 978 0 580 62288 5Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 27587:2009National forewordThis British Standard is the UK implementation of EN ISO 27587:2009. The UK participation in its preparation was entrusted to TechnicalComm
3、ittee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application. Compliance wi
4、th a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 27587 October 2009 ICS 59.140.30 English Version Leather - Chemical tests - Determination of the free formaldehyde in process auxiliaries (ISO 27587:2009) Cuir - Essais chimiqu
5、es - Dosage du formaldhyde libre dans les auxiliaires de traitement (ISO 27587:2009) Leder - Chemische Prfverfahren - Bestimmung des Gehalts an freiem Formaldehyd in Hilfsmitteln fr die Lederherstellung (ISO 27587:2009) This European Standard was approved by CEN on 26 September 2009. CEN members are
6、 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 be obtained on application to t
7、he CEN 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 the CEN Management Centre has the same
8、 status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Ro
9、mania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reserve
10、d worldwide for CEN national Members. Ref. No. EN ISO 27587:2009: EBS EN ISO 27587:2009EN ISO 27587:2009 (E) 3 Foreword This document (EN ISO 27587:2009) has been prepared by Technical Committee CEN/TC 289 “Leather”, the secretariat of which is held by UNI, in collaboration with the International Un
11、ion of Leather Technologists and Chemists Societies (IULTCS). 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 April 2010, and conflicting national standards shall be withdrawn at the latest by Apr
12、il 2010. 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 shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards org
13、anizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
14、Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN ISO 27587:2009ISO 27587:2009(E) IULTCS/IUC 26:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle. 1 5 Reagents 1 6 Appara
15、tus and materials 2 7 Methods . 3 7.1 Outline of sample preparation system . 3 7.2 Sample preparation 3 8 HPLC conditions (recommendations) 4 9 Calibration . 4 10 Calculation. 4 11 Checking reagents for absence of formaldehyde . 5 12 Control of the procedure 5 13 Determination of formaldehyde in sto
16、ck solutions. 5 14 Test report . 5 Annex A (informative) Reliability of the method . 6 BS EN ISO 27587:2009ISO 27587:2009(E) IULTCS/IUC 26:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (
17、ISO member bodies). The work of preparing 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, go
18、vernmental and non-governmental, in liaison 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/IE
19、C Directives, Part 2. The main task of technical 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 memb
20、er 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. ISO shall not be held responsible for identifying any or all such patent rights. ISO 27587/IUC 26 was prepared by the European Committee for Standardization
21、 (CEN) Technical Committee CEN/TC 289, Leather, in collaboration with the Chemical Tests Commission of the International Union of Leather Technologists and Chemists Societies (IUC Commission, IULTCS), in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement). I
22、ULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to further the advancement of leather science and technology. IULTCS has three Commissions, which are responsible for establishing international methods for the sampling and testing of leather. ISO recog
23、nizes IULTCS as an international standardizing body for the preparation of test methods for leather. BS EN ISO 27587:2009INTERNATIONAL STANDARD ISO 27587:2009(E)IULTCS/IUC 26:2009(E) ISO 2009 All rights reserved 1Leather Chemical tests Determination of the free formaldehyde in process auxiliaries 1
24、Scope This International Standard specifies a method for the determination of free formaldehyde in process auxiliaries for leather. The analytical result obtained according to this procedure is expressed in milligrams per kilogram (mg/kg) sample. The upper limit of quantification of the method is gi
25、ven by the capacity of the cartridge (total carbonyls 6 400 g/cartridge). 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 referenc
26、ed document (including any amendments) applies. ISO 3696, Water for analytical laboratory use Specification and test methods 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 free formaldehyde formaldehyde that is released under dynamic conditi
27、ons when the sample is heated in an inert dry atmosphere 4 Principle The sample is heated in an inert atmosphere for a defined period of time. The released formaldehyde is captured and derivatized using a dinitrophenylhydrazine (DNPH) cartridge. The analyte is eluted with acetonitrile and analysed b
28、y high-performance liquid chromatography (HPLC) using a UV detector. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise stated. 5.1 Sulfuric acid, 3 mol/l. 5.2 Sodium hydroxide, 2 mol/l. 5.3 Sodium thiosulfate, 0,1 mol/l. 5.4 Iodine solution, 0,05 mol/l, i.e. 12,68 g iodin
29、e per litre of water. BS EN ISO 27587:2009ISO 27587:2009(E) IULTCS/IUC 26:2009(E) 2 ISO 2009 All rights reserved5.5 Starch solution, 1 g/100 ml water. 5.6 Formaldehyde hydrazone solution. 5.7 Calibration standards. Prepare solutions by adequate dilution of the formaldehyde hydrazone solution (5.6).
30、5.8 Formaldehyde solution, approximately 37 % mass fraction. 5.9 Formaldehyde stock solution S1, prepare by pipetting 5 ml of formaldehyde solution (5.8) in a 1 000 ml volumetric flask and fill to the mark with distilled water. 5.10 Formaldehyde solution S2 in an adequate dilution for procedure cont
31、rol e.g. 2,5 ml of the formaldehyde stock solution S1 (5.9) in a 100 ml volumetric flask, fill up with distilled water. The concentration of this solution should be adapted to ensure that the formaldehyde content is in the middle of the calibrated range. 5.11 Distilled water, quality 2 according to
32、ISO 3696. 5.12 2,4-Dinitrophenylhydrazine cartridges (DNPH cartridges), suitable for fixing a total of 6 400 g of carbonyls per cartridge. For lower quantities of free formaldehyde, a smaller capacity cartridge can be used. It is recommended that the cartridge have an excess capacity of at least 20
33、% more than the predicted formaldehyde amount. 5.13 Acetonitrile, HPLC grade. 5.14 Water, HPLC grade. 6 Apparatus and materials Usual laboratory apparatus is required and, in particular, the following. 6.1 Thermostatic oil bath with stirring facilities, capable of maintaining a constant temperature
34、of (90 3) C. The oil bath shall be deep enough to allow the U-tube to be dipped in up to the side tubing. 6.2 Silicone oil, suitable for oil bath (6.1). 6.3 Nitrogen, purity 4,6. 6.4 U-tube, calcium chloride tube, U-shaped, with two stopcocks, leg length 150 mm. 6.5 Flow meter. 6.6 Silicone tubing.
35、6.7 Syringe filters, 0,45 m, regenerated cellulose. 6.8 Sea sand, purified by acid and calcined; quality grade GR for analysis. 6.9 Polytetrafluoroethylene (PTFE) stopcock grease, free of formaldehyde. 6.10 HPLC equipped with a UV detector. 6.11 HPLC column, of the RP-C18 type. 6.12 Hair dryer. BS E
36、N ISO 27587:2009ISO 27587:2009(E) IULTCS/IUC 26:2009(E) ISO 2009 All rights reserved 37 Methods 7.1 Outline of sample preparation system See Figure 1. Key 1 gas tank 2 flow meter 3 DNPH cartridge 4 HPLC Figure 1 Schematic outline of sample preparation system 7.2 Sample preparation Prepare a sample p
37、reparation system as described in 7.1. Initially, the U-tube (6.4) and the DNPH cartridge (5.12) are disconnected from the sampling system. All the parts of the sample preparation system shall be dry prior to use. Purge the system for 15 min with nitrogen (6.3) at a flow rate of 500 ml/min. It is im
38、portant that the analysis be carried out under an inert atmosphere. The purging step may be omitted before further analyses if work is done without interruption. The sampling system is slightly pressurized; therefore, all stopcocks should be secured with joint clamps. Add 3 g to 4 g of sea sand (6.8
39、) to the U-tube (6.4), ensuring that it is not blocked and that the nitrogen flow can be maintained. If this is not possible, use a larger diameter U-tube. Accurately weigh 0,5 g to 2 g of sample to the nearest 0,001 g into the U-tube. It may be necessary to reduce the amount of sample if it is in a
40、 liquid phase in order to diminish the likelihood of condensed water giving erroneous results. Apply a thin layer of stopcock grease (6.9) to the joints of the U-tube. Introduce the U-tube into the system and purge for 5 min with nitrogen (6.3) at a flow rate of 500 ml/min. Reduce the flow rate to b
41、etween 150 ml/min to 350 ml/min. Introduce the DNPH cartridge (5.12) into the system and place the U-tube into the oil bath (6.1) preheated to 90 C. Cover the cartridge and U-tube carefully with aluminum foil. During sampling, it may be necessary to readjust the flow rate. After 30 min, remove the U
42、-tube containing the sample from the oil bath. Remove any condensate from the cartridge side of the tubing and stopcock using a hair dryer (6.12). This step shall be carried out irrespective of whether condensate can be observed visually. BS EN ISO 27587:2009ISO 27587:2009(E) IULTCS/IUC 26:2009(E) 4
43、 ISO 2009 All rights reservedRemove the DNPH cartridge from the system and elute with small portions of acetonitrile (5.13) in a 10 ml volumetric flask. Make up to volume with acetonitrile. Carefully mix the solution by shaking and filter an aliquot for analysis using a syringe filter (6.7). Analyse
44、 the resulting filtrate by HPLC (6.10). It is recommended that the cartridges be removed from the refrigerator immediately prior to use. Experiments have shown that cartridges should be eluted within 3 days. 8 HPLC conditions (recommendations) Separation column: CC 250/4 Nucleosil 100-5 C18 HD1)with
45、 pre-column Flow rate: 0,8 ml/min Mobile phase: Solvent A, water Solvent B, acetonitrile Gradient: 55 % B linear to 95 % B in 20 min Column oven: 30 C UV detection: 360 nm Injection volume: 20 l 9 Calibration Calibration is carried out by means of an external standard in the range of 0,5 g/10 ml to
46、50 g/10 ml. The working range is limited by the capacity of the cartridge. Prepare adequate dilutions (in acetonitrile) of the formaldehyde hydrazone solution (5.6). Calibration shall be done using at least six concentration levels. The calibration is effected through plotting a graph of the formald
47、ehyde derivative peak area versus the concentration (g/10 ml). 10 Calculation Calculate the formaldehyde content (w) expressed in milligrams per kilogram (mg/kg) of sample being tested. Fwm=where is the concentration of formaldehyde obtained from the calibration graph, expressed in g/10 ml; F is the
48、 dilution factor; m is the mass of the sample, expressed in grams (g).1) Nucleosil 100-5 C18 HD is the trade name of a product supplied by Sorbent Technologies. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of the product named.
49、 Equivalent products may be used if they can be shown to lead to the same results. BS EN ISO 27587:2009ISO 27587:2009(E) IULTCS/IUC 26:2009(E) ISO 2009 All rights reserved 511 Checking reagents for absence of formaldehyde Blank analyses should be carried out on a regular basis and at least for each lot of reagents, mobile phase and cartridges or any other change in the system. The formaldehyde content detected in the blank solution should be below 75 % of the lowest calibration level (0,5 g/10 ml). 12 Control of the p
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