SLOVENSKI STANDARD

SIST ISO 9297:1996

01-junij-1996

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Water quality -- Determination of chloride -- Silver nitrate titration with chromate indicator
(Mohr's method)
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Qualité de l'eau -- Dosage des chlorures -- Titrage au nitrate d'argent avec du chromate
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comme indicateur (Méthode de Mohr)

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Ta slovenski standard je istoveten z: ISO 9297:1989

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ICS:
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13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for

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VQRYL chemical substances

SIST ISO 9297:1996 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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 INTERNATIONAL
STANDARD
First edition
1989-l l-1 5

Water quality - Determination of chloride -

Silver nitrate titration with chromate indicator
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(Mohr’s method)
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de l’eau - D osage des chiorures - Titragle au nitrate d’argent

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Qualit
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avec du ch romate co lmme indic mafew (Methode de Mohr)

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Reference number
IS0 9297: 1989(E)
IS0 9297:1989(E)

Foreword

IS0 (the International Organization for Standardization) is a worldwide

federation of national standards bodies (IS0 member bodies). The work
of preparing International Standards is normally carried out through IS0
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, govern-
mental and non-governmental, in liaison with ISO, also take part in the
work. IS0 collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
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Draft International Standards adopted by the technical committees are

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circulated to the member bodies for approval before their acceptance
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as International Standards by the IS0 Council. They are approved in

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accordance with IS0 procedures requiring at least 75 % approval by the

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member bodies voting.

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International Standard IS0 9297 was prepared by Technical Committee

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ISO/TC 147, Water quality.

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0 IS0 1989
All rights reserved. No part of this publication may be reproduced or utilized in any form
or by any means, electronic or mechanical, including photocopying and microfilm, without
permission in writing from the publisher.
International Organization for Standard ization
Case Postale 56 l CH-1211 Gerkve 20 l Switzerl and
Printed in Switzerland

ii
 IS0 9297:1989(E)

Introduction

Nearly all natural waters, as well as rain water and many waste waters,
contain chloride ions. Concentrations can vary widely from a few milli-
grams per litre in some natural waters to very high concentrations in
polluted waste water, marine water and saline ground water.

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INTERNATIONAL STANDARD IS0 9297:1989(E)

Water quality - Determination of chloride - Silver nitrate

titration with chromate indicator (Mohr’s method)

1 scope
Table 1 - Interferences
Amount interfering
Substance
1 .l Application range mg/l
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This International Standard specifies a titration Br- 3

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method for the determination of dissolved chloride 19 f2 I-

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in water. The method is applicable to the direct de-

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termination of dissolved chloride in concentrations

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CN-- 1
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between 5 mg/l and 150 mg/l. The working range

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may be extended to 400 mg/l by using a burette of Fe(CN)6 4- 2

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larger capacity or by sample dilution. Due to many Fe( CN)6 3--- 2

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interferences the method is not applicable to heavily

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NH4 -t- 100

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polluted waters of low chloride content.

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s* 03 2-- 200
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SCN-- 3
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1.2 Interferences Cr04 2-- 1000

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PO4 3- 25
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Normal concentrations of common constituents of

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ground water, surface water and potable water do

not interfere with the determination. Table 1 gives a summary of the concentrations of
interfering compounds, in milligrams per litre, that
The following substances interfere with the method give an increase of approximately 2 % in the result
when in the presence of 70 mg/l of chloride.
- Substances forming insoluble silver compounds,
such as bromides, iodides, sulfides, cyanides,
hexacyanoferrates(lI) and hexacyanoferrates(lll).
If necessary, bromide and iodide ions shall be
determined separately, and the result of the
chloride determination corrected accordingly.
2 Normative references
- Compounds forming complexes with silver ions,
such as ammonium and thiosulfate ions. The following standards contain provisions which,
through reference in this text, constitute provisions
- Compounds which will reduce chromate ions, of this International Standard. At the time of publi-
including iron and sulfite ions. cation, the editions indicated were valid. All stand-
ards are subject to revision, and parties to
The interferences mentioned above will lead to high agreements based on this International Standard
chloride values. are encouraged to investigate the possibility of ap-
plying the most recent editions of the standards in-
Highly coloured or turbid solutions may obscure the
dicated below. Members of IEC and IS0 maintain
end point, for example hydrated iron oxide.
registers of currently valid International Standards.
IS0 9297:1989(E)

IS0 385,1:1984, Laboratory glassware - Burettes - 4.4 Nitric acid, c(HN0,) z 0,l mol/l.
Part 1: General requirements.
Stored in a glass bottle, the solution is stable indef-
IS0 5667-l :1980, Water quality - Sampling - initely.
Part 1: Guidance on the design of sampling pro-
grammes. 4.5 Sodium hydroxide, solution, c(NaOH) 3
0,l mol/l.
IS0 5667.211982, Water quality - Sampling -
Part 2: Guidance on sampling techniques.
4.6 Reagent, for improvement of the buffer capac-
IS0 5667-3:1985, Water quality - Sampling - ity.
Part 3: Guidance on the preservation and handling
of samples. Calcium carbonate (CaCO,) or sodium hydrogen
carbonate (NaHCO,) in powder form.
IS0 572511986, Precision of test methods - Determi-
nation of repeatability and reproducibility for a
standard test method by inter-laboratory tests. 5 Apparatus

Ordinary laboratory equipment and

3 Principle

Reaction of chloride with added silver ions to form 5.1 Burette, of capacity 25 ml, complying with
insoluble silver chloride which precipitates IS0 385-l.
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quantitatively. Addition of a small excess of silver

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ions to form a red brown silver chromate with
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chromate ions that have been added as an indicator. 6 Procedure 19 f2

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This reaction is used for indicating the end-point.

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The pH is maintained in the range of 5 to 9,5 For sampling and preservation of samples refer to
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throughout the titration in order to allow precipi-

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IS0 5667-1, IS0 5667-2 and IS0 5667-3.

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tation.
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6.1 Titration
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4 Reagents
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Pipette a test portion of 100 ml, or a smaller volume

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NOTE 1 All silver compounds and solutions are sensi- of the sample diluted to 100 ml (volume V,), into ei-
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tive to light. Silver salts temporarily stain the skin brown.

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ther a white porcelain basin, or a conical flask or a

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beaker held against a white background.

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Use only reagents of recognized analytical grade

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and only distilled water or water of equivalent purity. If the pH of the sample is outside the range of 5 to
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9,5, adjust the pH using nitric acid (4.4) or sodium

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hydroxide (4.5) as appropriate, and note the volume

4.1 Silver nitrate, standard volumetric solution,
B 0,02 mol/l. required.
QWO,)
If ammonium ions are present in the sample in con-
Dissolve 3,3974 g of silver nitrate (AgNO,), previ-
ously dried at 105 “C in water and dilute to 1000 ml centrations exceeding 10 mg/l, adjust the pH to be-
in a one-mark volumetric flask. tween 6,5 and 7.

If stored in the dark in a brown glass bottle with Adjust the pH in one aliquot, then take another and,
this time without measuring the pH, add the same
glass stoppers, the solution is stable for several
amounts of acid/hydroxide solution.
months. The solution is standardized against 10 ml
sodium chloride standard reference solution (diluted
NOTE 2 If the pH is less than 5, pH-adjustment with
to 100 ml) using the procedure given in 6.1, however, calcium carbonate or sodium hydrogen carbonate (4.6) is
there is no need for pH adjustment. preferable. This will also improve the buffer capacity. The
amount added should be chosen so that a carbonate res-
idue is left in the sample even after titration.
4.2 Potassium chromate, indicator, 100 g/l solution.
Dissolve 10 g of potassium chromate (K,CrO,) in
water and dilute to 100 ml. Add 1 ml of potassium chromate indicator solution
(4.2). Titrate the solution by dropwise addition of sil-
ver nitrate solution until the colour of the solution
4.3 Sodium chloride, standard reference solution, just changes to a reddish brown (volume VJ.
c(NaCI) = 0,02 mol/l. Dissolve I,1688 g of sodium
chloride (NaCI), previously dried at 105 OC, in water After addition of one drop of sodium chloride sol-
and dilute to 1000 ml in a one-mark volumetric flask. ution (4.3), the colour should disappear.

2
 IS0 9297:1989(E)

Use the titrated sample treated with sodium chloride VS is the volume, in millilitres, of the silver
solution for comparison with the next titrations. nitrate solution (4.1) used for the titration
of the sample;
Where the titrant volume exceeds 25 ml, repeat the
determination using a larger capacity burette or a c is the actual concentration, expressed in
smaller test portion volume. moles of AgNO, per litre, of the silver
nitrate solution;
6.2 Blank test
s is the conversion factor,
Titrate a blank solution as described in 6.1, using
f = 35453mg/mol.
100 ml of water instead of the test sample. Report the result to the nearest 1 mg/l, giving three
significant figures only.
The blank value should not exceed 0,2 ml of 4.1.
Otherwise check the purity of the water.

7.2 Precision
7 Expression of results
The precision of the method is given in table 2.*)
7.1 Calculation

The chloride content, pcl, in milligrams per litre, is

given by the formula 8 Test report
(vs- v&$ The test report shall include the following informa-
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tion:

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where a) a reference 19 f2 to this International Standard;

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PCI is the concentration, in milligrams per li-

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b) all information neces sary for a complete identifi-

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tre, of chloride;
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cation of the sample;

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is the volume, in millilitres, of the test

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c) the results and the method of expression used;

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sample (maximum 100 ml; dilutions must

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be taken into account);

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d) details of any operations not included in this

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T/ b is the volume, in millilitres, of the silver International Standard or regarded as optional,

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nitrate solution used for the titration of together with any circumstances that may have
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the blank; affected the results.

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*) Values taken from an interlaboratory trial carried out in Germany, F.R., in 1983 in accordance with IS0 5725, except that
the method to reject outliers was different.