1、STDnBSI BS EN IS0 153LB-ENGL 2000 R Lb24bb9 0841092 BTB BRITISH STANDARD Pulp, paper and board - Determination of 7 specified polychlorinated biphenyls (PCB) The European Standard EN IS0 15318:1999 has the status of a British Standard ICs 85.040; 85.060 BS EN IS0 15318:2000 Imqmtiq Corrigendum No. 1
2、 NO COPYING WITROUT BSI PERMISSION EXCEPT AS PERMIITED BY COPYRIGHT LAW STD-BSI BS EN IS0 L53LB-ENGL 2000 H Lb24bb7 0841073 734 BS EN IS0 15318:2000 This British Standard, having been prepared under the direction of the Sector Committee for Materiais and Chemicals, was published under the authority
3、of the Standards Committee and comes into effect on 15 March 2000 O BSI 042000 ISBN O 580 34257 3 National foreword This British Standard is the official English language version of EN IS0 15318 1999. It is identical with IS0 153181999. This British Standard supersedes DD ENV 17981996. The UK partic
4、ipation in its preparation was enkusted to Technical Committee PAV11, Test methods for paper, board and pulps, 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
5、change, and keep the UK interests informed; - monitor related international and European developments and promulgate them in the UK A list of organizations represented on this committee can be obtained on request to its secrem. Cross-references Attention is drawn to the fact that CEN and CENELEC Sta
6、ndards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “I
7、nternational 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 Standards are responsible for their correct application. Compliance with
8、 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, the EN IS0 title page, pages 2 to 12, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates whe
9、n the document was last issued. Sidelining in this document indicates the most recent changes by amendment. Amendments issued since publication Amd. No. 10919 Comgendum No. 1 Date April 2000 Comments Indicated by a sideline STD=BSI BS EN IS0 15316-ENGL 2000 1b24bb9 0841094 670 EUROPEAN STANDARD NORM
10、E EUROPENNE EUROPISCHE NORM EN IS0 15318 October 1999 ICs 67.250; 85.040; 85.060 English version Pulp, paper and board - Determination of 7 specified polychlorinated biphenyls (PCB) (IS0 1531 8: 1999) Pues. papiers et cartons - Dtermination de 7 palychiorobiphnyles (PCB) spcifis (IS0 15318:1999) Zel
11、lstoff, Papier und Pappe - Bestimmung von 7 ausgewhlten Biphenylen (PCB) (IS0 15318:1999) This European Standard was approved by CEN on 25 June 1999. CEN members are bound to comply with the CENKENELEC intemal Regulations which stipulate the conditions for giving this European Standard lhe status of
12、 a national standard without any aiteration. Up-to-date lists and bibiiographical 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 officiai versions (English, French, German). A versio
13、n in any other language made by translation under the responsibility 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
14、, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATION EUROPISCHES KOMITEE FUR NORMUNG Central Secretailet: rue de Ctrirscir2 36 El 050 Brusseh Q 1999 C
15、EN All rights of exploitation in any form and by any means resewed worldwide for CEN national Members. Ref. No. EN IS0 15318:1999 E STD-BSI BS EN IS0 15318-ENGL 2000 = 1624669 OB41095 507 Page 2 EN IS0 15318:1999 Content Page 1 2 3 4 5 6 7 8 9 10 11 12 Annex A Annex B Annex C Foreword . 3 Introducti
16、on 4 Scope 4 Normative references . 4 Principle 4 4 Apparatus and auxiliary aids Reagents . 5 Sampling 6 Procedure . 6 Determination 7 Confirmation . 8 Expression of results . 9 Precision 9 Testreport 9 (informative): Method for the estimation of the total PCB-content 1 0 (informative): Description
17、of the extraction reservoir . 11 (informative): Graphical determination of congener level in paper . 12 - - STDOBSI BS EN IS0 L5318-ENGL 2000 1624669 0841096 443 Page 3 EN IS0 15318:1999 Foreword The text of EN IS0 153183999 has been prepared by Technical Committee CEMC 172 “Pulp, paper and board“,
18、the secretariat of which is held by DIN, in collaboration with Technical Cornmittee ISO/TC 6 “Paper, board and pulps“. This European Standard supersedes ENV 1798:1995. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsemen
19、t, at the latest by March 2000, and conflicting national standards shall be withdrawn at the latest by March 2000. According to the CEWCENELEC Intemal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech R
20、epublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. With regard to ENV 1798 : 1995-07 the following changes have been made: a) extension of the scope to “pulp“; b) addition of detai
21、led information on precision“; c) transformation from a European Prestandard (ENV) to a European Standard (EN); d) editorial updating. Page 4 EN IS0 15318:1999 Introduction CEWC 172 has decided to publish this test method as a European Standard (EN) because the validation of the test method on the l
22、evel of the existing limit for PCB (2 ppm) was until now impossible due to the fact that there was no reference material with this level of PCB and all samples tested have a PCB content on the level of aie deteciion limit (about 5 pgkg of the congeners). Prior to discontinuance of its use in 1971 a
23、commercial PCB had been an ingredient in carbonless copy paper. The presence of these copy papers in waste paper can lead to contamination of recycled pulp, paper and board products with PCB. The PCB contaminant has the same congener pattern as the PCB used earlier in carbonless copy papers and this
24、 identifies the source of PCB contamination. In this method, seven specified PCB congeners (numbers 18, 28, 52, 101, 138, 153 and 180) are determined individually. Because the source of the PCB contamination can be identified from the congener pattern, the total PCB content of the paper may be estim
25、ated from these seven congeners. For routine analyses, the spiking procedure of 5.10.5 and 7.4.4 may be omitted, provided that the result obtained from the analysis is less than 50 % of any present limit. This will require modification of clause 8 to take account of these changes. The use of this mo
26、dification shall be stated in the test report. In the event of any dispute the full method shall be used. Warnina: The use of this European Standard may involve hazardous materials, operations and equipment. It does not address all the safety problems associated with its use. It is the responsibilit
27、y of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of safety regulations prior to use. 1 scope This European Standard gives guidance on a test method which permits the determination of seven specified PCBs in pulp, paper and b
28、oard. Annex A gives a procedure for estimating the total content of PCB from the congener content. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text
29、and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this Standard only when incoroporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. EN IS0
30、186 EN 27213 Paper and board - Sampling to determine average quality (IS0 186 : 1994) Pulps - Sampling for testing (IS0 7213 : 1981) 3 Principle The test material is extracted with boiling ethanolic or methanolic potassium hydroxide solution. An aliquot of the extract is mixed with water and subject
31、ed to liquid-solid partitioning on a disposable C, solid phase extraction cartridge followed by elution with hexane or ISO-octane. The PCBs contained in the hexane phase are quantified by capillary gas chromatography using an electron capture detector (ECD) or a mass selective detector (MSD). The pa
32、ttern of the seven congener peaks is compared with the pattern of a technical PCB. If the patterns correspond, the level of total PCB can be estimated from the congener content by application of an appropriate factor. STD-BSI BS EN IS0 15318-ENGL 2000 W Lb24bb9 0843098 23b W Page 5 EN IS0 15318:1999
33、 4 Apparatus and auxiliary aids 4.1 Ordinary laboratory apparatus 4.2 Extractor reservoir An example is given in Annex B, where the reservoir comprises a glass tube approximately 200 mm long with an internal diameter of 30 mm. The tube is tapered twice at the lower end to ensure that the connection
34、to the disposable cartridge (4.3) is gas-tight and to allow drops to build up on the tip. 4.3 Disposable solid-phase extraction cartridge with a C, bonded phase (3,O ml size and 200 mg). 4.4 Gas chromatograph with an electron capture detector (ECD) or a mass selective detector (MSD). 4.5 Capillary c
35、olumn suitable for the determination of PCB in accordance with the specification laid down in 8.1. 5 Reagents Unless otherwise specified, reagents of a grade suitable for residue analysis shall be used. Water should be doubledistilled or of equivalent quality. Methanol can be used in place of ethano
36、l for all solutions if required and ISO-octane can be used in place of hexane. 5.1 Ethanol (C,H,OH 99,s %) 5.2 Methanol 5.3 n-Hexane (C,H, 98,O %) 5.4 Sulphuric acid, concentrated (d= 1,84) 5.5 Reference substances (CHaOH 99,8 Yo) Ballschmit Nomenclature 5.5.1 2,2,5-Trichlorobiphenyl 5.5.2 2,4,4-Tri
37、chlorobiphenyl 5.5.3 2,2,5,5-Tetrachlorbiphenyl 5.5.4 2,2,4,5,5-Pentachlorobiphenyl 5.5.5 2,2,3,4,4,5-Hexachlorobiphenyl 5.5.6 2,2,4,4,5,5-Hexachlorobiphenyl 5.5.7 2,2,3,4,4,5,5-Heptachlorobiphenyl 18 28 52 1 o1 138 153 180 5.6 Comparison sample Technical mixture of, for example, ChIophen) A 30 to A
38、 6003 or AmchIo+) 1242 to 1260. 5.7 Gas-Chromatography (GC) resolution sample 5.7.1 2,4,5-Tnchlorobiphenyl (TCBP, PCB 31) 5.8 Internal standards 5.8.1 2.4,6-Tnchlorobiphenyl (TCBP, PCB 30) 5.8.2 2,4,6-Tribromobiphenyl (TBBP) I Chlophen is the trade-name of a product supplied by Bayer. This informati
39、on is given for the convenience of users of this Standard and does not constitute an endorsement by CEN of the product named. Equivalent products may be used if they can be shown to lead to the same results. Arochlor is an example of a suitable product available commercially. This information is giv
40、en for the convenience of users of this Standard and does not constitute an endorsement by CEN of this product. Page 6 EN IS0 15318:1999 5.9 Ethanolic potassium hydroxide solution (2 % Mv) Dissolve 30,O g of potassium hydroxide in a solution 19:l 14vethanoVwater (1500 mi). Allow to stand for 24 h, d
41、ecant, and retain the clear solution. 5.10 Combined standard solutions Prepare the following standard solutions using volumetric glassware throughout: 5.10.1 Intermediate standard solutions A (200 pglml) Take approximately 10,O mg (to an accuracy of 0,l mg) of reference congener substance 18 (5.5.1)
42、. transfer quantitatively to a 50,O ml volumetric flask and make up to the mark with hexane. Shake to dissolve. NOTE: Mixtures corresponding to 5.1 O. 1 to 5.10.4 are commercially available. Repeat for congeners 28, 52, 101, 138, 153 and 180 (5.5), GC resolution sample 31 (5.7) and for TCBP or TBBP
43、(5.8). 5.10.2 Intermediate standard solutions B (20 pgiml) Take 5,O ml of solution A for congener 18 (5.10.1) and dilute to 50,O ml using hexane. Repeat for congeners 28, 52, 101, 138, 153 and 180, GC resolution sample 31, and for TCBP or TBBP (5.8). 5.10.3 Individual standard solutions for GC (0,l
44、pglml) Take 1,OO rnl of solution B for congener 18 (5.10.2) and dilute to 200,O ml wiih hexane. Repeat for congeners 28, 52, 101, 138, 153 and 180, GC resolution sample 31, and for TCBP or TBBP (5.8). 5.10.4 Combined standard solutions for GC (01 pgimi) Take 1 ,O0 ml of solution B for each congener
45、18, 28, 52, 101, 138, 153 and 180, GC resolution sample 31, and TCBP or TBBP (5.8) , and dilute to 200,O ml with hexane. 5.10.5 Spiking solution (0,l pgCm1) Take approximately 10,O mg (to an accuracy of 0,l mg) of congener substances 18,28,52,101,138,153 and 180 (5.5), transfer quantitatively to a 1
46、00,O ml volumetric flask and make up to the mark with ethanol. Shake to dissolve. Take 5,OO ml of this solution and dilute to 100,O ml with ethanol. Take 540 ml of this second solution and dilute to 250,O ml with ethanolic potassium hydroxide solution (5.9). 5.10.6 Internal standard solution (0,l pg
47、mi) Take approximately 10,O mg (to an accuracy of 0,l mg) of intemal standard substance TCBP or TBBP (5.8), transfer quantitatively to a 100,O ml volumetric flask and make up to the mark with ethanol. Shake to dissolve. Take 5,OO ml of this solution and dilute to 100.0 ml with ethanol. Take 500 ml o
48、f this second solution and dilute to 250,O ml with ehanolic potassium hydroxide solution (5.9). 6 Sampling Sampling shall be camed out in accordance with EN IS0 186 or EN 27213. The sample shall be wrapped in aluminium foil between acquisition and testing, to prevent any change before the test. 7 Pr
49、ocedure 7.1 Suitable safety measures shall be taken when the work laid down in this test method is canid out. 7.2 Attach the solid-phase disposable cartridge (4.3) to the extractor resetvoir (4.2) to give a gas-tight seal and condition with two charges of methanol (5.2) (typically 2 x 3,O mi) followed by water (typically 2 x 3,O mi) in accordance with the manufacturers instructions. 7.3 Take a representative sample of the pulp, paper or board sample (about 100 g as received), cut into pieces of about 1 cm2 and randomise by shaking in a large glass
