INTERNATIONAL ISO

STANDARD 9964-2
First edition
1993-05-01

Water quality - Determination of sodium

and potassium -
Part 2:
iTeh STANDARD
Determination PREVIEW
of potassium by atomic
absorption spectrometry
(standards.iteh.ai)
ISO 9964-2:1993
Quakt6 de I’eau - Dosage du sodium et du potassium -
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56f91f83dc04/iso-9964-2-1993
Partie 2: Dosage du potassium par spectromhtrie d’absorption atomique

Reference number
ISO 99642:1993(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. Esch 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
(1EC) on all matters of electrotechnical standardization.

Draft International Standards adopted by the technical committees are

circulated to the member bodies for voting. Publication as an International
iTeh STANDARD PREVIEW
Standard requires approval by at least 75 % of the member bodies casting
a vote.

International Standard
(standards.iteh.ai)
ISO 9964-2 was prepared by Technical Committee
ISO/TC 147, Water quality, Sub-Committee SC 2, Physical, Chemical,
biochemical methods. ISO 9964-2:1993
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ISO 9964 consists of the following Parts, under 56f91f83dc04/iso-9964-2-1993
the general title Water
quality - Determination o f sodium and potassium:

- Part 1: Determination of sodium by atomic absorption spectrometry

- Part 2: Determination of potassium by atomic absorption spec-

trome try

- Part 3: Determination of sodium and po tassium bY flame emission

spectrometry

0 ISO 1993
Al9 rights reserved. No part 0%this publication may be reproduced or utilized in any ferm or
by any means, electronie or mechanical, including photocopying and microfilm, without per-
mission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 l Switzerland
Printed in Switzerland

ii
INTERNATIONAL STANDARD ISO 9964=2:1993(E]

Water quality - Determination of sodium and

potassium -

Part 2:
Determination of potassium by atomic absorption
spectrometry

1 Scope ISO 5667-1: 1980, Water quality - Sampling -

Part 1: Guidance on the design of sampling pro-
iTeh STANDARD PREVIEW grammes.
1.1 Field of application
(standards.iteh.ai)
ISO 5667-2: 1991, Water quality -
Part 2: Guidance on sampling techniques.
Sampling -
This International Standard specifies a method for the
determination of dissolved potassium by flame atomic ISO 9964-2:1993
absorption spectrometry (AAS). lt is intended for the
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analysis of raw and drinking waters.
3 Principle
56f91f83dc04/iso-9964-2-1993
The method is applicable to water samples with a Addition of caesium chloride Solution to the Sample
mass concentration of potassium in the range from as an ionization suppressant. Aspiration of the Sample
5 mg/1 to 50 mg/l. This range tan be extended to directly into the airlacetylene flame of an atomic ab-
lower or higher limits if dilution factors are Chosen sorption spectrometer. Measurement of the
which are different from the factor specified in absorbance at a wavelength of 766,5 nm.
clause 8.
4 Reagents
1.2 Interferences
During the analysis, use only reagents of recognized
The ions normally present in raw and drinking waters analytical grade and only deionized water or water of
do not interfere with the determination of potassium equivalent purity.
by atomic absorption spectrometry.
4.1 Hydrochlorit acid, c(HCI) x 11 mol/l,
p = 1,18 g/ml.
2 Normative references
4.2 Nitrit acid, c(HNO$ N 16 mol/l, p = 1,41 g/ml.
The following Standards contain provisions which,
through reference in this text, constitute provisions 4.3 Caesium chloride, (CsCI), solution.
of this part of ISO 9964. At the time of publication, the
editions indicated were valid. All Standards are subject Dissolve 25 g of caesium chloride in a Solution of
to revision, and Parties to agreements based on this 50 ml of hydrochloric acid (4.1) and 450 ml of water,
part of ISO 9964 are encouraged to investigate the and dilute to 1 litre with water in a one-mark
possibility of applying the most recent editions of the volumetric flask.
Standards indicated below. Members of IEC and ISO
maintain registers of currently valid International One litre of this Solution contains approximately 20 g
Standards. of Cs.

1
NOTE 1 Nitrit acid (4.2) may be used instead of 7 Procedure
hydrochloric acid (4.1).

7.1 Preparation of test samples for

4.4 Potassium, stock solution. presentation to the spectrometer
In a 1 000 ml one-mark volumetric flask, dissolve 7.1.1 Filter samples containing particulate matter
1,907 g -f: 0,005 g of potassium chloride (previously through an acid-washed filter of pore size 0,45 km to
dried for at least 1 h at 140 “C & 10 “C) in water and prevent clogging of the nebulizer and burner Systems.
make up to the mark. (The acid used for washing the filter should have the
Store the Solution, which is stable for at least same concentration and be of the same type as the
6 months, in a polyethylene bottle. acid used in the Sample preparation.)

One litre of this Solution contains 1 000 mg of K. NOTE 3 Instead of filtration, the particulate matter may
be removed from Suspension by using a centrifuge.
Alternatively, use a commercially available, ready-
made Solution. 7.1.2 Take a number of 100 ml one-mark volumetric
flasks according to the number of samples being an-
alysed. To each of these flasks, add 10 ml of the
4.5 Potassium, Standard solution. caesium chloride Solution (4.3).

Pipette 10 ml of the potassium stock Solution (4.4) 7.1.3 Pipette, 10 ml of the Sample into each of these
into a 1 000 ml one-mark volumetric flask. Make up caesium chloride solutions, and make up to the mark
to the mark with water. with water. If the concentration of the test Solution is
The Solution shall be prepared freshly when required. not in the Optimum range of 0,l mg/1 to 1,O mg/1 of
K, adjust the volume of the Sample appropriately.
iTeh STANDARD PREVIEW
1 ml of this Standard Solution contains 10 pg of K.
(standards.iteh.ai)
7.2 Preparation of the set
solutions
of calibration

5 Apparatus ISO 9964-2:1993

Add 10 ml of caesium chloride Solution to each of a
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series of 100 ml one-mark volumetric flasks. Pipette
Ordinary laboratory apparatus and 56f91f83dc04/iso-9964-2-1993
0 ml; 1,O ml; 2,0 ml; 4,0 ml; 6,0 ml and 10,O ml of the
potassium Standard Solution (4.5) into the series flasks
and make up each flask to the mark with water.
5.1 Atomic absorption spectrometer, set up and
operated according to the manufacturer’s instructions, The calibration solutions will have the concentrations
it is equipped with a burner for an airlacetylene flame, 0 mg/l; 0,l mg/l; 0,2 mg/l; 0,4 mg/l; 0,6 mg/1 and
a hollow cathode lamp for potassium determination, 1,O mg/1 of K, respectively.
and a compatible red-sensitive photomultiplier.

A spectral bandwith of < 0,3 nm is recommended. 7.3 Calibration and determination

All glassware shall be of borosilicate glass. 7.3.1 Set up the spectrometer according to the
manufacturer’s instructions by aspirating a calibration
Clean both glass and polyethylene ware by soaking in
Solution (7.2). Optimize the aspiration and flame con-
an aqueous Solution of 10 % (VW) of nitric acid (4.2)
ditions (aspiration rate, nature of the flame, Position
followed by thorough rinsing with water. The appar-
of the Optical beam in the flame). Adjust the response
atus should only be used for this method.
of the instrument to zero absorbance with water.

7.3.2 Aspirate the calibration solutions (7.2) with an

6 Sampling aspiration of water between each. Measure the
absorbance at 766,5 nm. Prepare a calibration graph
Collect samples in clean polyethylene bottles (see by plotting the respective absorbance readings on the
ISO 5667-1 and ISO 5667-2). Sample preservation by Ordinate against the mass concentrations of potass-
acidification is not generally necessary. ium on the abscissa.

NOTE 2 If other metal analyses are to be carried out on Calculate from the graph the slope, b, in litres per
the samples, the samples tan be preserved by addition of milligram.
hydrochloric acid (4.1) or nitric acid (4.2) to give a pH of ap-
proximately 1. All samples, Standards and blanks should NOTE 4 The calibration graph is normally linear for the
contain the same concentration and the same type of acid. concentration range 0,l mg/1 to 1,O mg/l.

2
 ISO 9964-2: 1993( EI

7.3.3 Aspirate the test samples (7.1), with an aspir- where

ation of water between each, and determine the
absorbance. A is the absorbance of the Sample;

AO is the absorbance of the blank;

7.3.4 Carry out a blank determination with each
batch of samples by applying the same procedure and hl is the volume, in millilitres, of the test
using water instead of the Sample. portion (normally 10 ml);
NOTE 5 lt is good practice to check the slope of the vP is the volume, in millilitres, of the
calibration graph at regular intervals (e.g. every 10 samples). volumetric flask (i 00 ml);
& is the slope of the calibration curve, in li-
8 Calculation and expression of results tres per milligram.

8.1 Use of calibration graph If required, ca culate the amount-of-substance con-

centration, cK', in millimoles per litre, using the
Read the concentrations of potassium in the test sol- equation
utions from the calibration graph (see 7.3.2). From
these values, calculate the potassium concentration PK
CK’
=- . . . (2)
of the test Sample, taking into account the volume of 39,1
test Sample taken (normally 10 ml) and the total vol-
ume of the volumetric flask (100 ml). If the calibration curve is not linear, proceed as de-
scribed in 8.1.
8.2 Method of calculation
If the calibration graph is linear, calculate the mass
concentration of potassium, &, in the Sample, in 8.3 Precision
milligrams per litre, using the equation iTeh STANDARD PREVIEW
An interlaboratory trial, carried out in autumn 1991,
PK=
(A - Ao>‘vm
v .b
(standards.iteh.ai)
...0 using this method, produced the results given in
P table 1.
ISO 9964-2:1993
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56f91f83dc04/iso-9964-2-1993
Table 1 - Precision data
x
Sampld) I n
% w/l YO %
A 1
A 10 27 10 0,99 0,058 1 59
59 0,041 1 42
4,2
B 10 30 0 5,72
572 0,227 9 4,O 0,096 1 lt7
C 10 30 0 6,71 0,239 7 3,6 0,138 7 Zl
2,l

I is the number of laboratories 5 is the repeatability Standard deviation

n is the number of values VC, is the repeatability Variation coefficient
n, is the percentage of outliers OR is the reproducibility Standard deviation
x is the mean value VCR is the reproducibility Variation coefficient
I
1) A: drinking water

B: surface water

C: waste water
9 Test report c) the results and the method of expression used, in
accordance with clause 8;
The test report shall include the following information:
d) any deviation from this method or any other cir-
a) a reference to this International Standard; cumstances which may have influenced the re-
sults.
b) precise identification of the water Sample;

iTeh STANDARD PREVIEW

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ISO 9964-2:1993
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ISO 9964-2:1993
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ISO 9964-2: 1993(E)

iTeh STANDARD PREVIEW

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ISO 9964-2:1993
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56f91f83dc04/iso-9964-2-1993

UDC 614.777:556.114:543.42:546.32
Descriptors: water, quality, water tests, Chemical anaiysis, determlnation of content, potasslum, atomic absorption spectrometric
method.

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