1、November 2011 Translation by DIN-Sprachendienst.English price group 10No 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).I
2、CS 85.040; 85.060!$vT5“1834918www.din.deDDIN EN ISO 15320Pulp, paper and board Determination of pentachlorophenol in an aqueous extract(ISO 15320:2011)English translation of DIN EN ISO 15320:2011-11Zellstoff, Papier und Pappe Bestimmung von Pentachlorphenol in einem wssrigen Extrakt (ISO 15320:2011)
3、Englische bersetzung von DIN EN ISO 15320:2011-11Ptes, papiers et cartons Dosage du pentachlorophnol dans un extrait aqueux (ISO 15320:2011)Traduction anglaise de DIN EN ISO 15320:2011-11SupersedesDIN EN ISO 15320:2004-03www.beuth.deIn case of doubt, the German-language original shall be considered
4、authoritative.Document comprises 16 pages11.11 DIN EN ISO 15320:2011-11 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 6 “Paper, board and pulps” in collaboration with Technical Committee CEN/TC 172 “Pulp, paper and board” (Se
5、cretariat: DIN, Germany), Working Group WG 3 “Analytical methods for the assessment of paper and board in contact with foodstuffs” (Secretariat: ASI, Austria). The responsible German body involved in its preparation was the Normenausschuss Papier, Pappe und Faserstoff (Paper, Board and Pulps Standar
6、ds Committee), Working Committee NA 074-02-01 AA Chemisch-technische Prfverfahren fr Papier, Pappe, Faserstoff und Chemiezellstoff. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 186 DIN EN ISO 186 ISO 536 DIN EN ISO 536 ISO 638 DIN EN
7、 ISO 638 ISO 3696 DIN EN ISO 3696 ISO 7213 DIN EN 27213 Amendments This standard differs from DIN EN ISO 15320:2004-03 as follows: a) in Clause 1 “Scope”, it has been specified that the working range for acetylation is 0,05 mg/kg to 0,5 mg/kg; b) Subclause 8.3 “Derivatization” has been added; c) Ann
8、ex A “Precision” has been supplemented by new results of an international round-robin relating to repeatability and reproducibility; d) the standard has been editorially revised. Previous editions DIN EN ISO 15320: 2004-03 DIN EN ISO 15320-2:2011-10 3 National Annex NA (informative) Bibliography DIN
9、 EN 27213, Pulps Sampling for testing DIN EN ISO 186, Paper and board Sampling to determine average quality DIN EN ISO 536, Paper and board Determination of grammage DIN EN ISO 638, Paper, board and pulps Determination of dry matter content Oven-drying method DIN EN ISO 3696, Water for analytical la
10、boratory use Specification and test methods DIN EN ISO 15320:2011-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15320 August 2011 ICS 85.040; 85.060 Supersedes EN ISO 15320:2003English Version Pulp, paper and board - Determination of pentachlorophenol
11、 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 15320:2011) This European Standard was approved by CEN on 14 August 2011.
12、 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 be obtained on
13、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 the CEN-CENELE
14、C 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, Luxembourg, Malta,
15、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 Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploita
16、tion in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15320:2011: EEN ISO 15320:2011 (E) 2 Contents PageForeword31 Scope 42 Normative references 43 Principle44 Apparatus .55 Reagents.56 Sampling.67 Extraction .67.1 Cold-water extraction 67.2 Hot-water extract
17、ion 78 Procedure .78.1 Preparation .78.2 Solid phase concentration78.3 Derivatization .79 Calibration 810 Gas chromatographic analysis 810.1 Gas chromatographic condition 810.2 Establishing retention time of pentachlorophenol.810.3 Calculation of the area ratio versus mass ratio810.4 Calibration for
18、 mass spectrometer using 13C6labelled pentachlorophenol911 Calculation912 Test report 10Annex A (informative) Precision 11A.1 General11A.2 Repeatability.11A.3 Reproducibility.11Bibliography 12DIN EN ISO 15320:2011-11 EN ISO 15320:2011 (E) 3 Foreword This document (EN ISO 15320:2011) has been prepare
19、d by Technical Committee 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 e
20、ndorsement, 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 elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for
21、 identifying any or 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
22、 Republic, 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. Endorsement notice The text of ISO 15320:2011
23、has been approved by CEN as a EN ISO 15320:2011 without any modification. DIN EN ISO 15320:2011-11 EN ISO 15320:2011 (E) 4 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, whi
24、ch is corrosive. This International Standard does not address all the 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
25、safety regulations prior to use. 1 Scope This International Standard 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
26、to all kinds of pulp, paper and board. The working range for acetylation 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
27、 document. For dated references, only the edition cited applies. For 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,
28、 board and pulps Determination of dry matter content Oven-drying method 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 pentachlorophe
29、nol extract is concentrated by adsorption onto a phenyl silica column 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 u
30、sing gas chromatography employing an electron-capture detector (ECD) or mass spectrometer (MS) detector. The result is expressed as milligrams per kilogram of material. DIN EN ISO 15320:2011-11 EN ISO 15320:2011 (E) 5 4 Apparatus 4.1 Conical flask, 500 ml, wide necked with a ground-glass stopper wit
31、h tap (see ISO 1773). 4.2 Filtration equipment, fritted-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 Ga
32、s chromatograph, a conventional split/splitless injector 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 feat
33、ures is given as an example: stationary phase: polydimethyl-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
34、given as an example: a) ionization: EI 70 eV (electron 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 equi
35、valent quality. 5.1 Water, grade 2 in accordance with 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
36、carbonate with an accuracy of 0,1 g into a beaker 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. DIN EN ISO 15320:2011-11 EN ISO 15320:2011 (E) 6 5.8 Sodium sulfate, anhydrous, Na2SO4. 5.9 Reference standard solutions
37、 5.9.1 Pentachlorophenol reference 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).T
38、his solution is stable for at least 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 l
39、east 6 months when stored in a 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
40、standard stock solution (5.10.1) 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) int
41、ernal standard stock solution, 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
42、 g/ml. Pipette 1 ml of the internal 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
43、or pulp, the sample shall be selected 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
44、 touch the test area of the sample 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 accordan
45、ce with ISO 638. 7.1 Cold-water extraction Using protective gloves, tear or cut the sample as taken into pieces of approximately 1 cm2to 2 cm2. DIN EN ISO 15320:2011-11 EN ISO 15320:2011 (E) 7 Weigh (10 0,1) g (oven-dried) of the test pieces to an accuracy of 0,01 g, put them into the conical flask
46、(4.1), add 200 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 t
47、o a marked volumetric 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
48、to an accuracy 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
49、 80 C. If necessary 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
