1、BRITISH STANDARD BS ISO 9198:2001 Paper, board and pulp Determination of water-soluble sulfates ICS 85.060; 85.040; 71.040.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 9198:2001 This British Standard, having been prepared under the direction of the Sector Committee
2、 for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 September 2001 BSI 08-2001 ISBN 0 580 38340 7 National foreword This British Standard reproduces verbatim ISO 9198:2001 and implements it as the UK national standard. It supersedes
3、BS 2924-3:1990 which is withdrawn. 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 this committee can be obtained on request to its secretary. Cros
4、s-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electroni
5、c 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 a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand
6、the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a fr
7、ont cover, an inside front cover, the ISO title page, pages ii and iii, a blank page, pages 1 to 4, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsReferenc
8、e number ISO 9198:2001(E) INTERNATIONAL STANDARD ISO 9198 Second edition 2001-06-01 Paper, board and pulp Determination of water-soluble sulfates Papier, carton et pte Dtermination des sulfates solubles dans leauISO 9198:2001(E) DPF dlcsiremia ihTs PDF file mya ctnoain emdeddeb tyfepcaes. In acccnad
9、roe with Aebods licnesign lopic,y this file may be pirntde ro ivwede tub slahl ton eb ideted lnuess teh tyfepacse which aer emdeddeb era licnesed to dna intslaled on teh computre freporming teh idetign. In wodlnidaogn this f,eli trapies accept tniereh teh sersnoptilibiy of ton nifrgnigni Asebod lics
10、negni ilopcy. ehT ISO tneClar Secteraairt accepts no lilibaity ni this .aera Aebod is a tedarmakr fo Aebod Stsyems Icntaropro.de teDails fo the sfotwera pcudorts sude to crtaee tihs PFD file can be fdnuo in the Glarene Info leratiev to the fil;e the Pc-FDaertion arapmteres were tpoimizde for pirtnin
11、g. Evyre cera sah neeb taken to enseru taht teh file is suitlbae fro sue by ISO memreb idob.se In teh lnuikley etnev ttah a plborem leratign to it is f,dnuo lpsaee ifnrom teh tneClar Sceterairat at the sserdda givne lebwo. ISO 1002 All rhgits rsevre.de elnUss towrehise scepfidei, on trap of tihs cil
12、buptanoi mya eb cudorperde ro utzilide ni yna form ro yb yna snaem, eelctinorc ro mecinahcal, inclidugn tohpociypong dna micrfoilm, wittuoh repmissino in writing form eitreh ISO at teh erddass lebwo ro ISOs memreb ydob in the ctnuoyr of the rtseuqee.r ISO cirypothg fofice saCe tsopale 65 1121-HC ave
13、neG 20 leT. + 41 22 947 10 11 xaF + 14 22 947 90 74 E-mail cirypothgiso.ch eWb www.iso.ch ii ISO 1002 All irhgts seredevrISO 9198:2001(E) ISO 1002 All rights rsedevre iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO mem
14、ber 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, governmen
15、tal 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/IEC Direc
16、tives, Part 3. 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 member bodies casting a vote. Attention is drawn to the possibility that some of the ele
17、ments of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 9198 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps. This second edition cancels and replaces th
18、e first edition (ISO 9198:1989), of which it constitutes a technical revision. There are two major differences between this and the previous edition of ISO 9198. a) The extraction is now done at 23 C, whereas boiling water was used in the previous edition. b) Ion chromatography, a technique now wide
19、ly used for the determination of anions because of its high sensitivity and selectivity, replaces the conductometric titration using barium chloride and lithium sulfate solutions in the former edition.INTERNATIONAL STANDARD ISO 9198:2001(E) ISO 1002 All rights rsedevre 1 Paper, board and pulp Determ
20、ination of water-soluble sulfates 1 Scope This International Standard specifies a method for the determination of water-soluble sulfates in all types of pulp, paper and board. The lower limit of the determination is 20 mg of sulfate ion per kilogram of dry sample. 2 Normative references The followin
21、g normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International St
22、andard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International S
23、tandards. ISO 186:1994, Paper and board Sampling to determine average quality. ISO 287:1985, Paper and board Determination of moisture content Oven-drying method. ISO 638:1978, Pulps Determination of dry matter content. ISO 7213:1981, Pulps Sampling for testing. 3 Term and definition For the purpose
24、s of this International Standard, the following term and definition applies. 3.1 water-soluble sulfates in pulp, paper and board amount of sulfate ion that is extracted with water at 23 C and determined under the conditions specified 4P r i n c i p l e Pieces of the sample are extracted with water a
25、t 23 C in a disintegrator. An aliquot of the resulting suspension is used for determination of the sulfate ion content by ion chromatography. 5 Reagents Use only reagents of recognized analytical quality and only water as specified in 5.1. 5.1 Distilled water or deionized water, of conductivity less
26、 than 0,1 mS/m at 25 C.ISO 9198:2001(E) 2 ISO 1002 All rights rsedevre 5.2 Sulfate stock solution, (SO 4 2 ) = 1 000 mg/l. Dry a portion of potassium sulfate (K 2 SO 4 )a t1 4 0 C. Transfer 181,5 mg 2 mg thereof to a 100 ml volumetric flask, dissolve the salt and make up to the mark with water (5.1)
27、. Commercially available standard solutions can be used. 5.3 Sulfate matching solution Dilute the sulfate stock solution (5.2) with water (5.1) to a sulfate ion concentration of, for example, (SO 4 2 )= 10 mg/l. Do not use sulfate matching solutions that are more than 1 week old. 5.4 Other solutions
28、, as specified in the instructions for the ion chromatograph. 6 Apparatus 6.1 Wet disintegrator, a high-speed mixer, capable of disintegrating the sample completely. 6.2 Ion chromatograph, having a pump, an injector loop of known volume, a column system suitable for the determination of sulfates and
29、 a conductivity detector. 6.3 Syringe, of a quality suitable for ion chromatography, of capacity 5 ml and having a filter of about 0,2 m pore width. 6.4 Tea strainer or similar device with a fine mesh screen, of stainless steel, to prevent fibres from clogging the syringe. 7 Sampling and preparation
30、 of sample The procedure to be followed when sampling depends on the particular circumstances in each case. If the analysis is being made to evaluate a lot or a consignment of pulp, paper or board, the sample shall be taken in accordance with ISO 7213 or ISO 186, as relevant. If the analysis is made
31、 on another type of sample, report the origin of the sample and, if possible, the sampling procedure. Since the amount of sulfates in the sample can be very low, take care not to contaminate it during sampling. Wear clean gloves at all times when handling the sample. Keep the sample protected, wrapp
32、ed in aluminium foil or in plastic bags, until required for analysis. Select the sample portion for the analysis so that it is representative of the sample received. 8 Procedure Carry out the procedure in duplicate. A blank shall also be carried through the entire procedure. Weigh, to the nearest 0,
33、01 g, a test portion, generally of between 2 g and 5 g. Split thick board and pulp sheets into thinner pieces to facilitate soaking. The size of the test portion should be selected so that the sulfate ion content of the extract is within the optimum range of the ion chromatograph. At the same time,
34、determine the dry matter content on a separate portion using the procedure specified in ISO 287 or ISO 638, as relevant.ISO 9198:2001(E) ISO 1002 All rights rsedevre 3 Transfer the weighed test portion to the disintegrator (6.1) and add 250 ml 2 ml of water (5.1) at 23 C 2 C. Disintegrate the sample
35、 portion until it is completely disintegrated, but no longer. After disintegration, let the sample portion soak for about 2 h. Withdraw an aliquot for analysis of the suspension, using the syringe (6.3). If this operation is hampered by the presence of fibres or fibre bundles, use the tea strainer o
36、r similar device (6.4) to prevent fibrous material from clogging the syringe. Place the device over the fibres and withdraw the aliquot from the solution above this device. It is essential that the withdrawn aliquot be free from suspended material. Since the operation of the ion chromatograph (6.2)
37、depends on its design, no detailed instructions can be given in this International Standard. Operate the apparatus as instructed by the manufacturer. For calibration, prepare from the sulfate matching solution (5.3) a series of five calibration solutions, covering about one decade of concentrations,
38、 for example, from 1 mg/l to 10 mg/l. Run the calibration solutions and the sample solution (the aliquot) on the chromatograph as instructed by the manufacturer of the apparatus. Plot the readings for the calibration solutions against their sulfate ion concentrations. The five points for the calibra
39、tion solutions should fall on a straight line. If they fail to do so, repeat the calibration with another set of calibration solutions, covering a lower concentration range. However, the range of calibration solutions shall always bracket the sulfate concentration obtained from the aliquot. Check th
40、e calibration daily and whenever a new set of calibration solutions is taken into use. Read the sulfate peak of the extract (the aliquot). From the calibration graph, read the sulfate ion concentration of the extract, , and of the blank, 0 . 9 Calculation Calculate the mass fraction of water-soluble
41、 sulfates in the sample from the expression 0 d () 100 V m where is the mass fraction of sulfate ions in the sample, in milligrams per kilogram; is the sulfate ion concentration of the filtered extract, in milligrams per litre; 0 is the sulfate ion concentration of the blank solution, in milligrams
42、per litre; V is the volume of water (5.1) used in the disintegration (the volume specified is 250 ml); m is the mass of sample taken, in grams; d is the dry matter content of the sample, expressed as a percentage. Calculate the mean and report the result to the nearest 10 mg/kg. Report values below
43、20 mg/kg as “less than 20 mg/kg“.ISO 9198:2001(E) 4 ISO 1002 All rights rsedevre 10 Precision Five pulp and paper samples were extracted several times in a laboratory. From every extract, two aliquots were analysed. The results are shown in Table 1. Table 1 Results obtained when five samples were an
44、alysed several times, mg/kg Bleached pulp, soft wood Unbleached wrapping paper Writing paper Bleached pulp, hard wood Paper (40 g/m 2 ) 1st extraction 36,5 37,0 65,5 68,2 155,0 155,3 335,5 336,0 840 833 2nd extraction 38,2 38,4 60,8 61,1 153,3 154,3 323,2 320,0 824 830 3rd extraction 36,9 37,8 69,6
45、67,1 Mean value 37,5 65,4 154,5 328,7 832,0 Coefficient of variation (% of all values) 2,1 5,6 0,9 2,5 6,3 11 Test report The test report shall include the following information: a) reference to this International Standard; b) date and place of testing; c) complete identification of the sample teste
46、d; d) the result, expressed as indicated in clause 9; e) any departure from the procedure described in this International Standard or any other circumstances which may have affected the result.BS ISO 9198:2001 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the inde
47、pendent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that th
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