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1、Reference number ISO 9198:2001(E) ISO 2001 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 leau ISO 9198:2001(E) PDF disclaimer This PDF file may contain embedded typ
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6、ale 56 ? CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2001 All rights reserved -,-,- ISO 9198:2001(E) ISO 2001 All rights reservediii Foreword ISO (the International Organization for Standardization) is a worldwide
7、 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 be represented on that
8、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 Standards are drafted in acc
9、ordance with the rules given in the ISO/IEC Directives, 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
10、 is drawn to the possibility that some of the elements 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 p
11、ulps. This second edition cancels and replaces the 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 edit
12、ion. b)Ion chromatography, a technique now widely 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 STANDARDISO 9198:2001(E)
13、ISO 2001 All rights reserved1 Paper, board and pulp Determination of water-soluble sulfates 1Scope 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 ki
14、logram of dry sample. 2Normative references The following 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. Howev
15、er, parties to agreements based on this International Standard 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 I
16、EC maintain registers of currently valid International Standards. 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 Sam
17、pling for testing. 3Term and definition For the purposes 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 4Principle
18、 Pieces of the sample are extracted with water at 23 C in a disintegrator. An aliquot of the resulting suspension is used for determination of the sulfate ion content by ion chromatography. 5Reagents Use only reagents of recognized analytical quality and only water as specified in 5.1. 5.1Distilled
19、water or deionized water, of conductivity less than 0,1 mS/m at 25 C. -,-,- ISO 9198:2001(E) 2 ISO 2001 All rights reserved 5.2Sulfate stock solution,?(SO42) = 1 000 mg/l. Dry a portion of potassium sulfate (K2SO4) at 140 C. Transfer 181,5 mg?2 mg thereof to a 100 ml volumetric flask, dissolve the s
20、alt and make up to the mark with water (5.1). Commercially available standard solutions can be used. 5.3Sulfate matching solution Dilute the sulfate stock solution (5.2) with water (5.1) to a sulfate ion concentration of, for example,?(SO42) = 10 mg/l. Do not use sulfate matching solutions that are
21、more than 1 week old. 5.4Other solutions, as specified in the instructions for the ion chromatograph. 6Apparatus 6.1Wet disintegrator, a high-speed mixer, capable of disintegrating the sample completely. 6.2Ion chromatograph, having a pump, an injector loop of known volume, a column system suitable
22、for the determination of sulfates and a conductivity detector. 6.3Syringe, of a quality suitable for ion chromatography, of capacity 5 ml and having a filter of about 0,2 ?m pore width. 6.4Tea strainer or similar device with a fine mesh screen, of stainless steel, to prevent fibres from clogging the
23、 syringe. 7Sampling and preparation 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, a
24、s relevant. If the analysis is made 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 sampl
25、e. Keep the sample protected, wrapped 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. 8Procedure Carry out the procedure in duplicate. A blank shall also be carried through the entire p
26、rocedure. Weigh, to the nearest 0,01 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
27、 chromatograph. At the same time, 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 2001 All rights reserved3 Transfer the weighed test portion to the disintegrator (6.1) and add 250 ml?2 ml of water (5.1) at
28、 23 C?2 C. Disintegrate the sample 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 fib
29、re bundles, use the tea strainer or 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 operati
30、on of the ion chromatograph (6.2) 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 a
31、bout one decade of concentrations, 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 concentration
32、s. The five points for the calibration 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 o
33、btained from the aliquot. Check the 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. 9Calculation Calculate th
34、e mass fraction of water-soluble 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; ?0is the sulfate ion concent
35、ration of the blank solution, in milligrams per litre; Vis the volume of water (5.1) used in the disintegration (the volume specified is 250 ml); mis the mass of sample taken, in grams; ?dis the dry matter content of the sample, expressed as a percentage. Calculate the mean and report the result to
36、the nearest 10 mg/kg. Report values below 20 mg/kg as “less than 20 mg/kg“. -,-,- ISO 9198:2001(E) 4 ISO 2001 All rights reserved 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. T
37、able 1 Results obtained when five samples were analysed several times, mg/kg Bleached pulp, soft wood Unbleached wrapping paper Writing paper Bleached pulp, hard wood Paper (40 g/m2) 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
38、,2 320,0 824 830 3rd extraction 36,9 37,8 69,6 67,1 Mean value37,565,4154,5328,7832,0 Coefficient of variation (% of all values) 2,15,60,92,56,3 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
39、 identification of the sample tested; 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. ISO 9198:2001(E) ICS 85.040; 85.060 Price based on 4 pages ISO 2001 All rights reserved -,-,-