1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 15320:2011Pulp, paper and board Determination ofpentachlorophenol inan aqueous extract (ISO15320:2011)BS EN ISO 15320:2011 BRITISH STANDARDNational forewordThis British
2、 Standard is the UK implementation of EN ISO15320:2011. It supersedes BS EN ISO 15320:2003 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PAI/11, Methods of test for paper, board and pulps.A list of organizations represented on this committee can beobt
3、ained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 60733 2ICS 85.040; 85.060Compliance with a British Standard cannot confer immunity fromlegal obligations.
4、This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 November 2011.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15320 August 2011 ICS 85.040; 85.060 Supersedes EN ISO 15320:2003Eng
5、lish Version Pulp, paper and board - Determination of pentachlorophenol in an aqueous extract (ISO 15320:2011) Ptes, papiers et cartons - Dosage du pentachlorophnol dans un extrait aqueux (ISO 15320:2011) Zellstoff, Papier und Pappe - Bestimmung von Pentachlorphenol in einem wssrigen Extrakt (ISO 15
6、320:2011) This European Standard was approved by CEN on 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 bibliograp
7、hical 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 by translation under the responsibili
8、ty 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, Finland, France, Germany, Greece, H
9、ungary, 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 EUROPISCHES KOMITEE FR NORMUNG Management Ce
10、ntre: 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 15320:2011: EBS EN ISO 15320:2011EN ISO 15320:2011 (E) 3 Foreword This document (EN ISO 15320:2011) has been prepared by Technical Com
11、mittee ISO/TC 6 “Paper, board and pulps“ in collaboration with Technical Committee CEN/TC 172 “Pulp, paper and board” the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the
12、 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 elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any o
13、r all such patent rights. This document supersedes EN ISO 15320:2003. 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, Denmark
14、, 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. Endorsement notice The text of ISO 15320:2011 has been approved
15、by CEN as a EN ISO 15320:2011 without any modification. BS EN ISO 15320:2011ISO 15320:2011(E) ISO 2011 All rights reserved iiiContents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Principle . 1 4 Apparatus . 2 5 Reagents 2 6 Sampling 3 7 Extraction . 3 7.1 Cold-water extraction 3 7.2 Hot-wa
16、ter extraction 4 8 Procedure . 4 8.1 Preparation . 4 8.2 Solid phase concentration . 4 8.3 Derivatization . 4 9 Calibration 5 10 Gas chromatographic analysis 5 10.1 Gas chromatographic condition 5 10.2 Establishing retention time of pentachlorophenol 5 10.3 Calculation of the area ratio versus mass
17、ratio . 5 10.4 Calibration for mass spectrometer using 13C6labelled pentachlorophenol . 6 11 Calculation . 6 12 Test report 7 Annex A (informative) Precision 8 Bibliography 9 BS EN ISO 15320:2011ISO 15320:2011(E) iv ISO 2011 All rights reservedForeword ISO (the International Organization for Standar
18、dization) 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 interested in a subject for which a technical committee has been established has the right to
19、 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 Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Stan
20、dards 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 technical committees are circulated to the member bodies for voting. Publication as an Int
21、ernational 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. ISO shall not be held responsible for identifying any or all such patent rights. ISO 15320
22、 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps. This second edition cancels and replaces the first edition (ISO 15320:2003), which has been technically revised. BS EN ISO 15320:2011INTERNATIONAL STANDARD ISO 15320:2011(E) ISO 2011 All rights reserved 1Pulp, paper and board Det
23、ermination of pentachlorophenol in an aqueous extract WARNING The use of this International Standard may involve hazardous materials, e.g. methanol and pentachlorophenol, which are toxic substances, as well as acetic anhydride, which is corrosive. This International Standard does not address all the
24、 safety and environmental problems associated with its use. It is the responsibility of the user of this International Standard to establish appropriate safety, health and environmental practices and determine the applicability of safety regulations prior to use. 1 Scope This International Standard
25、specifies a test method for the determination of pentachlorophenol (PCP) in an aqueous extract of pulp, paper and board. Although it was developed for paper and board intended to come into contact with foodstuffs, it is applicable to all kinds of pulp, paper and board. The working range for acetylat
26、ion is 0,05 mg/kg to 0,5 mg/kg. NOTE The upper limit of the working range could be increased if the aqueous extract is diluted. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For
27、undated references, the latest edition of the referenced document (including any amendments) applies. ISO 186, Paper and board Sampling to determine average quality ISO 536, Paper and board Determination of grammage ISO 638, Paper, board and pulps Determination of dry matter content Oven-drying meth
28、od ISO 7213, Pulps Sampling for testing ISO 3696, Water for analytical laboratory use Specification and test methods 3 Principle A specimen of the material to be tested is extracted with either cold or hot water. The pentachlorophenol extract is concentrated by adsorption onto a phenyl silica column
29、 using solid-phase extraction. The pentachlorophenol is then eluted from the phenyl silica column with n-hexane and an acetylated derivative formed with acetic anhydride. The amount of pentachlorophenol present is then determined using gas chromatography employing an electron-capture detector (ECD)
30、or mass spectrometer (MS) detector. The result is expressed as milligrams per kilogram of material. BS EN ISO 15320:2011ISO 15320:2011(E) 2 ISO 2011 All rights reserved4 Apparatus 4.1 Conical flask, 500 ml, wide necked with a ground-glass stopper with tap (see ISO 1773). 4.2 Filtration equipment, fr
31、itted-glass filter of porosity 4 (nominal size 90 m) with a filter flask of 500 ml (see ISO 6556). 4.3 Marked volumetric flask, 250 ml (see ISO 1042). 4.4 Solid-phase extraction (SPE) system and SPE columns, phenyl silica columns, 500 mg/3 ml. 4.5 Gas chromatograph, a conventional split/splitless in
32、jector gives suitable sensitivity when used in the splitless mode. Alternatively, an on-column injection mode may be used. 4.6 Capillary column, suitable for determination of acetylated derivates of pentachlorophenol. A column with the following features is given as an example: stationary phase: pol
33、ydimethyl-siloxan with 5 % phenyl groups; film thickness: 0,25 m; length: 30 m; internal diameter: 0,32 mm. 4.7 Detector, electron-capture detector (ECD) or mass spectrometer (MS) suitable for carrying out the measurement. The following features are given as an example: a) ionization: EI 70 eV (elec
34、tron impact); b) resolution: 1 amu (atomic mass unit); c) runnability: SIM mode (selected ion monitoring). NOTE SIM is called SIR (selected ion recording) for some instruments. 5 Reagents All reagents shall be of a grade “pro analysis” (p.a.) or equivalent quality. 5.1 Water, grade 2 in accordance w
35、ith ISO 3696. 5.2 Methanol, CH3OH. 5.3 Hydrochloric acid, HCl (0,1 mol/l). 5.4 n-Hexane, C6H14. 5.5 Sulfuric acid, H2SO4 (diluted 1+1). 5.6 Acetic anhydride, C4H6O3(99 %). 5.7 Potassium carbonate solution, K2CO3(0,1 mol/l). Weigh 13,8 g of potassium carbonate with an accuracy of 0,1 g into a beaker
36、and dissolve it in a small amount of water. Transfer the solution to a 1 000 ml volumetric flask and dilute to volume with water. BS EN ISO 15320:2011ISO 15320:2011(E) ISO 2011 All rights reserved 35.8 Sodium sulfate, anhydrous, Na2SO4. 5.9 Reference standard solutions 5.9.1 Pentachlorophenol refere
37、nce stock standard solution, 100 g/ml. This solution is commercially available. 5.9.2 Pentachlorophenol dilute reference stock standard solution, 5 g/ml. Pipette 1 ml of the stock solution (5.9.1) into a 20 ml volumetric flask and dilute to volume with methanol (5.2).This solution is stable for at l
38、east 6 months when stored in a refrigerator at 4 C. 5.9.3 Pentachlorophenol reference standard solution, 0,5 g/ml. Pipette 1 ml of the dilute stock solution (5.9.2) into a 10 ml volumetric flask and dilute to volume with methanol (5.2). This solution is stable for at least 6 months when stored in a
39、refrigerator at 4 C. 5.10 Internal standard solutions for ECD 5.10.1 2,3,6-Trichlorophenol internal standard stock solution, 10 g/ml. This solution is commercially available. 5.10.2 2,3,6-Trichlorophenol internal standard solution, 2 g/ml. Pipette 2 ml of the internal standard stock solution (5.10.1
40、) into a 10 ml volumetric flask and dilute to volume with methanol (5.2). This solution is stable for at least 3 months when stored in a refrigerator at 4 C. 5.11 Internal standard solutions for MS 5.11.1 13C6labelled pentachlorophenol (labelled at all six carbons) internal standard stock solution,
41、10 g/ml. This solution is commercially available. It is an alternative to the 2,3,6-trichlorophenol solution mentioned in 5.10.1 and can be employed only when a mass spectrometer is used as a detector. 5.11.2 13C6labelled pentachlorophenol internal standard solution, 1 g/ml. Pipette 1 ml of the inte
42、rnal standard stock solution (5.11.1) into a 10 ml volumetric flask and dilute to volume with methanol (5.2). This solution is stable for at least 6 months when stored in a refrigerator at 4 C. 6 Sampling If the analysis is being made to evaluate a lot of paper, board or pulp, the sample shall be se
43、lected in accordance with ISO 186 or ISO 7213, as relevant. If the analysis is made on another type of sample, report the source of the sample, and, if possible, the sampling procedure. Select the specimens so that they are representative of the sample received. Do not touch the test area of the sam
44、ple or test specimen with fingers; use protective gloves. A minimum of 10 g of sample is required. Take a separate sample for the determination of the dry matter content in accordance with ISO 638. 7 Extraction Determine the dry matter content of the sample in accordance with ISO 638. 7.1 Cold-water
45、 extraction Using protective gloves, tear or cut the sample as taken into pieces of approximately 1 cm2to 2 cm2. BS EN ISO 15320:2011ISO 15320:2011(E) 4 ISO 2011 All rights reservedWeigh (10 0,1) g (oven-dried) of the test pieces to an accuracy of 0,01 g, put them into the conical flask (4.1), add 2
46、00 ml of water and stopper the flask. Leave this preparation to stand for 24 h at (23 2) C, shaking occasionally. Decant the solution and wash the test pieces remaining in the flask twice. If necessary, filter the preparation (see 4.2). Transfer the extract and washings or the filtrate to a marked v
47、olumetric flask (4.3) and fill up to the mark with water. Use the contents of the flask for the PCP measurement. 7.2 Hot-water extraction Using protective gloves, tear or cut the sample as taken into pieces of approximately 1 cm2to 2 cm2. Weigh (10 0,1) g (oven-dried) of the test pieces to an accura
48、cy of 0,01 g, put them in the conical flask (4.1), add 200 ml of boiling water and stopper the flask. Leave this preparation to stand for 2 h 5 min in a water bath of temperature (80 2) C, shaking occasionally. Decant the solution and wash the test pieces in the flask twice with water at 80 C. If ne
49、cessary filter the hot preparation (see 4.2). Cool to (23 2) C, then transfer the extract and washings or the filtrate to a marked volumetric flask (4.3), and fill up to the mark with water. Use the contents of the flask for the PCP measurement. 8 Procedure Analyse the water extract received from 7.1 or 7.2 as described below. Carry out duplicate determinations. 8.1 Preparation Sample 50 ml of the water extract. Add 200 l of the internal standard solution (5.10.2 or 5.11.2) and acidify with 1 ml of sul
