1、BRITISH STANDARDBS EN 14719:2005Pulp, paper and board Determination of the Diisopropyl-naphthalene (DIPN) content by solvent extractionThe European Standard EN 14719:2005 has the status of a British StandardICS 85.040; 85.060g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g
2、48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14719:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 December 2005 BSI 30 December 2005ISBN 0 580 47414
3、 3National forewordThis British Standard is the official English language version of EN 14719:2005. The UK participation in its preparation was entrusted to Technical Committee PAI/11, Methods of test for paper, board and pulps, which has the responsibility to: A list of organizations represented on
4、 this committee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by usi
5、ng the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity fr
6、om legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.
7、Summary of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 10, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date Comme
8、ntsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14719August 2005ICS 85.040; 85.060English versionPulp, paper and board - Determination of theDiisopropylnaphthalene (DIPN) content by solvent extractionPtes, papiers et cartons - Dtermination de la teneur endiisopropylnaphtalne (DIPN) par extracti
9、on au solvantFaserstoff, Papier und Karton - Bestimmung des Gehaltesan Diisopropylnaphthalin (DIPN) mittelsLsemittelextraktionThis European Standard was approved by CEN on 27 June 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving
10、 this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (
11、English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, C
12、zech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NOR
13、MALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14719:2005: EEN 14719:2005 (E) 2 Contents Foreword 3 1 Scope .4 2 Principle.4 3 Reage
14、nts4 3.1 General 4 3.2 Standards 4 3.2.1 Diisopropylnaphthalene (DIPN) (technical mixture of isomers) .4 3.2.2 Diethylnaphthalene (DEN), with a purity of 97 % or more4 3.3 Chemicals, Acetone4 3.4 Calibration stock solutions 4 3.5 Internal standard stock solution5 4 Apparatus and auxiliary aids .5 4.
15、1 Gas chromatograph5 4.2 Gas chromatograph analytical capillary column5 4.3 Ultrasonic bath6 4.4 Microsyringes, 100 l, 250 l6 4.5 Graduated pipettes, 1 ml, 2 ml, 10 ml 6 4.6 40 ml screw top vials, with PTFE (polytetrafluorethylene) lined septa .6 5 Sampling6 6 Preparation of test pieces 6 7 Calibrat
16、ion .6 7.1 Calibration standards .6 7.1.1 General 6 7.1.2 Calibration A6 7.1.3 Calibration B6 7.2 Blank value7 7.3 Control standard .7 8 Procedure 7 8.1 GC-MS analysis.7 8.2 Calibration .7 8.3 Test piece analysis .7 8.3.1 Test piece extracts7 8.3.2 Determination of DIPN7 8.4 Evaluation of data .7 8.
17、4.1 Interferences .7 8.4.2 Determination of the DIPN concentration in the test pieces7 8.4.3 Calculation of the DIPN content in the paper8 9 Precision9 10 Test report .9 Bibliography.10 EN 14719:2005 (E) 3 Foreword This European Standard (EN 14719:2005) has been prepared by Technical Committee CEN/T
18、C 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 latest by February 2006, and conflicting national standards shall be withdrawn at the
19、latest by February 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, I
20、reland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 14719:2005 (E) 4 1 Scope This European Standard describes a method for the determination of the content of diisopropylnaphthalene (DIPN) i
21、n paper, board and pulp by solvent extraction. The content of diisopropylnaphthalene (DIPN) is expressed as mg of total diisopropylnaphthalene DIPN isomers per kilogram of paper, board or pulp. This test method is appropriate for the quantitative determination of the content of diisopropylnaphthalen
22、e (DIPN) with a limit of determination of about 0,6 mg/kg. 2 Principle The content of total diisopropylnaphthalene (DIPN) is determined by solvent extraction of the paper, board or pulp sample and analysed by gas chromatography with mass selective detection (GC-MS), using diethylnaphthalene as an in
23、ternal standard. NOTE It may be worthwhile to state that diisopropylnaphthalene (DIPN) can be present as a contaminant in pulp, paper and board. For the time being it cannot be avoided that diisopropylnaphthalene (DIPN) is present when using recovered fibres. It may be present as either adsorbed ont
24、o the test piece or present in an encapsulated form. Acetone is an effective solvent for complete extraction of both physical forms of diisopropylnaphthalene (DIPN). 3 Reagents 3.1 General All reagents shall be of recognised analytical quality unless otherwise stated. 3.2 Standards 3.2.1 Diisopropyl
25、naphthalene 1)(DIPN) (technical mixture of isomers) The purity shall be given by the supplier or 2,6-Diisopropylnaphthalene. 3.2.2 Diethylnaphthalene (DEN), with a purity of 97 % or more 3.3 Chemicals, Acetone 3.4 Calibration stock solutions 3.4.1 Stock solution of diisopropylnaphthalene (DIPN) in a
26、cetone with an accurately known concentration of approximately 1 200 mg/l Weigh accurately about 30 mg of diisopropylnaphthalene (DIPN) (3.2.1) into a 25 ml volumetric flask. Fill the volumetric flask to approximately half the volume with acetone (3.3), shake to dissolve and dilute to the mark with
27、acetone. Calculate the concentration of diisopropylnaphthalene (DIPN) in mg/l, by using the exact mass taken and the purity. 1) Diisopropylnaphthalene is a name of a product supplied by Fisher. This information is given for the convenience of users of this European Standard and does not constitute a
28、n endorsement by CEN of the product. Equivalent products from other manufacturers may be used if they can be shown to lead to the same results. EN 14719:2005 (E) 5 3.4.2 Standard stock solution (A) with an accurately known concentration of approximately 12 mg/l Transfer 1 ml of the 1 200 mg/l stock
29、solution (3.4.1) into a 100 ml volumetric flask and dilute to the mark with acetone. 3.4.3 Standard stock solution (B) with an accurately known concentration of approximately 120 mg/l Transfer 10 ml of the 1 200 mg/l stock solution (3.4.1) into a 100 ml volumetric flask and dilute to the mark with a
30、cetone. 3.5 Internal standard stock solution Stock solution of diethylnaphthalene (DEN) (3.2.2) in acetone with a concentration of approximately 1 000 mg/l. Weigh accurately approximately 50 mg of diethylnaphthalene (DEN) (3.2.2) into a 50 ml volumetric flask and dilute to the mark with acetone. 4 A
31、pparatus and auxiliary aids NOTE An instrument or item of apparatus is listed only if it is special, or made to a particular specification, usual laboratory glassware and equipment being assumed to be available. 4.1 Gas chromatograph Equipped with a mass selective detector. 4.2 Gas chromatograph ana
32、lytical capillary column Appropriate operating conditions shall be established for the specific equipment used for the determination. An example of suitable chromatographic conditions is given below: Column 5 % phenylmethyl siloxane 30 m x 0,25 mm ID 0,25 m film thickness Carrier gas: Helium, 1 ml/m
33、in Temperature program: isothermal at 70 C for 2 min, from 70 C to 250 C at 10 C/min isothermal at 250 C for 15 min Injector: Splitless, 240 C Transferline: 280 C Detection: MSD (Mass Selective Detector) Ions, diisopropylnaphthalene (DIPN) m/z 155, 197, 212 diethylnaphthalene (DEN) m/z 169 The follo
34、wing retention times have been observed under these conditions: diisopropylnaphthalene (DIPN) 6 major isomers 15,5 min to 16,1 min; diethylnaphthalene (DEN) 14,8 min. A separation of diisopropylnaphthalene (DIPN) into 7 isomers was observed with other columns, which did not influence the result. EN
35、14719:2005 (E) 6 4.3 Ultrasonic bath 4.4 Microsyringes, 100 l, 250 l 4.5 Graduated pipettes, 1 ml, 2 ml, 10 ml 4.6 40 ml screw top vials, with PTFE (polytetrafluorethylene) lined septa 5 Sampling Wrap test pieces for test individually in aluminium foil. Avoid direct contact to plastic films. Use the
36、 test pieces without humidity-conditioning or drying. 6 Preparation of test pieces Carry out the test in duplicate. Cut (avoiding edges) a piece (approx. 5 g) of the paper, board or pulp test piece into test pieces with an area of approximately 2 cm2. At the same time weigh a specimen for determinat
37、ion of the dry content. Accurately weigh (2,00 0,01) g of the prepared test piece into a 40 ml screw top vial, add 100 l of internal standard stock solution (3.5) and allow it to soak in. Then add by measuring cylinder 25 ml acetone. Cap the vial and leave to stand for about 16 h at room temperature
38、 and then put the vials to the ultrasonic bath for 15 min. Remove a small portion of the extract for analysis by GC-MS (Gas Chromatography Mass Spectrometry). 7 Calibration 7.1 Calibration standards 7.1.1 General Prepare two sets of calibration standards in the ranges of 0,05 mg/l to 1,0 mg/l (calib
39、ration A) and 1 mg/l to 10 mg/l (calibration B). NOTE There are two calibration standards for two different values. 7.1.2 Calibration A Add 0,1 ml, 0,2 ml, 0,5 ml, 1,0 ml and 2,0 ml of standard stock solution A (3.4.2) and 100 l internal standard stock solution (3.5) into five 25 ml volumetric flask
40、s by syringe or pipette. Dilute to the mark with acetone to give calibration standard solutions nominally containing 1,2 g, 2,4 g, 6 g, 12 g and 24 g of diisopropylnaphthalene (DIPN). 7.1.3 Calibration B Add 0,2 ml, 0,5 ml, 1,0 ml and 2,0 ml of standard stock solution B (3.4.3) and 100 l internal st
41、andard stock solution (3.5) into four 25 ml volumetric flasks by syringe or pipette. Dilute to the mark with acetone to give calibration standard solutions nominally containing 24 g, 60 g, 120 g and 240 g of diisopropylnaphthalene (DIPN). Calculate the exact amounts of diisopropylnaphthalene (DIPN)
42、added to the calibration standard solutions. NOTE The calibration standard solutions can be stored in a refrigerator up to 3 month. EN 14719:2005 (E) 7 7.2 Blank value Follow the procedure described in Clause 6 but without addition of the test piece. 7.3 Control standard Prepare a control standard f
43、rom the standard stock solution A (3.4.2) by adding 2 ml into a 25 ml volumetric flask and 100 l internal standard stock solution (3.5) and diluting to the mark with acetone. Calculate the amount of diisopropylnaphthalene (DIPN) added in g. 8 Procedure 8.1 GC-MS analysis Maintain the same operating
44、conditions of the GC-MS system throughout the measurements of all solutions prepared in Clauses 6 to 7.3. 8.2 Calibration Inject the calibration standards prepared in 7.1 together with the control standard (7.3) for GC-MS analysis. Obtain the integrated peak areas of the DIPN and DEN peaks. Construc
45、t the calibration line by plotting the total peak area ratio of DIPN/DEN versus the mass of DIPN (g) added to the calibration solutions. NOTE The correlation coefficients of the calibration lines should be 0,996 or better. The control standard should give a result from the calibration graph within 8
46、 % of the true value. If the correlation coefficients are less than 0,996 then fresh intermediate standard stock solutions and calibration solutions should be prepared from the original stock solutions. 8.3 Test piece analysis 8.3.1 Test piece extracts Inject the test piece extracts and blank as pre
47、pared in Clauses 6 and 7.2 for GC-MS analysis. 8.3.2 Determination of DIPN Identify the six DIPN peaks on the basis of the retention time and measure the total peak areas. Also measure the DEN peak area and calculate the DIPN/DEN area ratio. 8.4 Evaluation of data 8.4.1 Interferences No interference
48、s with the DIPN or DEN peaks arising from the extraction procedure have so far been observed using the method and the GC-MS conditions specified in (4.2). NOTE If DIPN is found in the blank (7.2) it is recommended to check for the source of contamination. 8.4.2 Determination of the DIPN concentratio
49、n in the test pieces 8.4.2.1 Graphical determination Read from the calibration graph (see Clause 8) the quantity of DIPN in g in the test piece extract by interpolation of the total peak area ratios DIPN/DEN to the x-axis. EN 14719:2005 (E) 8 8.4.2.2 Calculation from the regression parameters Calculate the regression line equation according to formula (1): bay += x (1) where y is the regression line (peak area ratio); a is the slope of the regression line in g-1; x is the concentration DIPN in micrograms; b is the intercept of the regressi
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