2021-12-18; J, Vaithiyanathan; SMS DX, SHS POC R&D OPS UCD PRL

INTERNATIONAL ISO
STANDARD 9198

Third edition
2020-09

Paper, board and pulp —

Determination of water-soluble
sulfates
Papier, carton et pâte — Détermination des sulfates solubles dans l'eau

Reference number
ISO 9198:2020(E)
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ISO 9198:2020(E)


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ISO 9198:2020(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Principle......................................................................................................................................................................................................................... 1
5 Reagents......................................................................................................................................................................................................................... 1
6 Apparatus...................................................................................................................................................................................................................... 2
7 Sampling and preparation of sample............................................................................................................................................... 2
8 Procedure..................................................................................................................................................................................................................... 2
9 Calculation................................................................................................................................................................................................................... 3
10 Precision........................................................................................................................................................................................................................ 3
11 Test report.................................................................................................................................................................................................................... 4
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ISO 9198:2020(E)


Foreword
ISO (the International Organization for Standardization) 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 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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/​directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/​patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www​.iso​.org/​
iso/​foreword​.html.
This document was prepared by Technical Committee ISO/TC 6, Paper, board and pulps.
This third edition cancels and replaces the second edition (ISO 9198:2001), which has been technically
revised. The main changes compared to the previous edition are as follows:
— In 6.4, the addition of the option of filtering the suspension through a medium coarseness filter
paper prior to withdrawing an aliquot with a syringe.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www​.iso​.org/​members​.html.
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INTERNATIONAL STANDARD ISO 9198:2020(E)

Paper, board and pulp — Determination of water-soluble

sulfates

1 Scope
This document 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 following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this 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 287, Paper and board — Determination of moisture content of a lot — Oven-drying method
ISO 638, Paper, board and pulps — Determination of dry matter content — Oven-drying method
ISO 7213, Pulps — Sampling for testing

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://​w ww​.iso​.org/​obp
— IEC Electropedia: available at http://​w ww​.electropedia​.org/​
3.1
water-soluble sulfates
in pulp, paper and board, the amount of sulfate ion that is extracted with water at 23 °C and determined
under the conditions specified

4 Principle
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.

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 than 0,1 mS/m at 25 °C.

5.2 Sulfate stock solution, r(SO4–2) = 1 000 mg/l.

Dry a portion of potassium sulfate (K 2SO4) at 140 °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).
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ISO 9198:2020(E)


Commercially available standard solutions can be used.

5.3 Sulfate intermediate solution

Dilute the sulfate stock solution (5.2) with water (5.1) to a sulfate ion concentration of, for example,
r(SO4 –2) = 10 mg/l. Do not use sulfate intermediate solutions that are more than 1 week old.

5.4 Other solutions, 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 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 μm pore diameter.

6.4 Tea strainer or similar device with a fine mesh screen, of stainless steel, to prevent fibres from
clogging the syringe. Alternatively, the suspension can be filtered through a medium coarseness filter
paper prior to withdrawing an aliquot with a syringe.

7 Sampling 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, as 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 sample.
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.

8 Procedure
Carry out the procedure in duplicate. A blank shall also be carried through the entire procedure.
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 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.
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 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 or similar device (6.4) to prevent fibrous
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ISO 9198:2020(E)


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) depends on its design, no detailed instructions can
be given in this document. Operate the apparatus as instructed by the manufacturer.
For calibration, prepare from the sulfate intermediate solution (5.3) a series of five calibration solutions,
covering about 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 concentrations. 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 obtained 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, r, and of the blank, r0.

9 Calculation
Calculate the mass fraction of water-soluble sulfates in the sample from the expression
( ρ − ρ0 )V
ω = 100
mωd
where

ω is the mass fraction of sulfate ions in the sample, in milligrams per kilogram;

ρ is the sulfate ion concentration of the filtered extract, in milligrams per litre;

ρ0 is the sulfate ion concentration of the blank solution, in milligrams 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;

ωd 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 20 mg/kg as
"less than 20 mg/kg".

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.
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ISO 9198:2020(E)


Table 1 — Results obtained when five samples were analysed several times, mg/kg

Bleached pulp, Unbleached Bleached pulp, Paper

Writing paper
soft wood wrapping paper hard wood (40 g/m2)
36,5 65,5 155,0 335,5 840
1st extraction
37,0 68,2 155,3 336,0 833
38,2 60,8 153,3 323,2 824
2nd extraction
38,4 61,1 154,3 320,0 830
36,9 69,6 — — —
3rd extraction
37,8 67,1 — — —
Mean value 37,5 65,4 154,5 328,7 832,0
Coef f icient of
variation 2,1 5,6 0,9 2,5 6,3
(% of all values)

11 Test report
The test report shall include the following information:
a) reference to this document, i.e. ISO 9198:2020;
b) date and place of testing;
c) complete 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.
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ISO 9198:2020(E)


ICS 85.060; 85.040

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