SLOVENSKI STANDARD

SIST ISO 7150-1:1996

01-junij-1996

.DNRYRVWYRGH'RORþDQMHDPRQLMDGHO5RþQDVSHNWURIRWRPHWULMVNDPHWRGD

Water quality -- Determination of ammonium -- Part 1: Manual spectrometric method

Qualité de l'eau -- Dosage de l'ammonium -- Partie 1: Méthode spectrométrique

manuelle
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Ta slovenski standard je istoveten SIST z: ISOISO 7150-1:1984
7150-1:1996
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ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances

SIST ISO 7150-1:1996 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
 SIST ISO 7150-1:1996

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 SIST ISO 7150-1:1996

International Standard
INTERNATIONAL ORGANIZATION FOR STANDARDlZATIONWvlEX~YHAPO~HAR OPI-AHM3AUMR fl0 CTAH~APTM3A~MM~ORGANISATlON INTERNATIONALE DE NORMALISATION

Water quality - Determination of ammonium -

Part 1 : Manual spectrometric method
Qualitb de l’eau - Dosage de l’ammonium - Partie I : AMhode spectrombtrique manuelle

First edition - 1984-06-01

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UDC 543.342 : 543.42 Ref. No. ISO 7150/1-1984 (E)

Descriptors : water, quality, Chemical analysis, determination of content, ammoniacal nitrogen, ammonium ion, spectrophotometric analysis,
water pollution.

Price based on 7 pages

 SIST ISO 7150-1:1996

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards bodies (ISO member bodies). The work of developing International
Standards is carried out through ISO technical committees. Every member body
interested in a subject for which a technical committee has been authorized 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.

Draft International Standards adopted by the technical committees are circulated to

the member bodies for approval before their acceptance as International Standards by
the ISO Council.
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International Standard ISO 7150/1 was developed by Technical Committee
(standards.iteh.ai)
ISO/TC 147, Water guality, and was circulated to the member bodies in February 1983.

lt has been approved by the member bodies of the following

SISTcountries :
ISO 7150-1:1996
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Australia Hungary Norway
feb520e40890/sist-iso-7150-1-1996
Austria India Poland
Belgium Iran Romania
Canada Iraq South Africa, Rep. of
Chile Italy Spain
Czechoslovakia Korea, Dem. P. Rep. of Sweden
Denmark Korea, Rep. of Switzerland
Finland Mexico Thailand
France Netherlands United Kingdom
Germany, F. R. New Zealand USSR

The member body of the following country expressed disapproval of the document on
technical grounds :

Japan

@ International Organkation for Standardkation, 1984 0

Printed in Switzerland
 SIST ISO 7150-1:1996

INTERNATIONAL STANDARD ISO 7150/1-1984 (E)

Water quality - Determination of ammonium -

Part 1 : Manual spectrometric method

1 Scope and field of application 3 Principle

1 .l Substance determined Spectrometric measurement at about 655 nm of the blue

compound formed by reaction of ammonium with salicylate
This part of ISO 7150 specifies a manual spectrometric method and hypochlorite ions in the presence of sodium nitrosopenta-
for the determination of ammonium in water. cyanoferrate(lll) (sodium nitroprusside).

NOTE - An automated spectrometric method for the determination of Hypochlorite ions are generated in situ by the alkaline
ammonium will form the subject of ISO 7150/2. hydrolysis of N, AI’-dichloro-1,3,5-triazine-2,4,6 (1 H, 3H,
5H)-trione, sodium salt (sodium dichloroisocyanurate). Reac-
1.2 Type of Sample iTeh STANDARD PREVIEW tion of the Chloramine with sodium salicylate takes place at
pH 12,6 in the presence of sodium nitroprusside. Any
(standards.iteh.ai)
The method is applicable to the analysis of potable water, and
most raw and waste waters. Application to excessively coloured
chloramines present in the Sample are quantitatively de-
termined as a consequence. Sodium citrate is incorporated in
or Saline waters shall be preceded by distillation (sec clause 10). the reagent to mask interference from cations, notably Calcium
SIST ISO 7150-1:1996
and magnesium.
For interferences, see clause https://standards.iteh.ai/catalog/standards/sist/5b65be87-65ff-412c-9dfb-
9.
feb520e40890/sist-iso-7150-1-1996
1.3 Range
4 Reagents
An ammonium nitrogen concentration, QN of up to 1 mg/I,
using the maximum test Portion of 40 ml, tan be determined. During the analysis, use only reagents of recognized analytical
Much higher concentrations tan be determined by taking grade and only water prepared as described in 4.1.
smaller test portions.

1.4 Limit of detection 1) 4.1 Water, ammonium-free, prepared by one of the follow-
ing methods.
When using cells of Optical path length 40 mm and a 40 ml test
Portion, the limit of detection lies within the range @N = 0,003
to 0,008 mg/l. 4.1.1 Ion exchange method

Pass distilled water through a column of strongly acidic cation

1.5 Sensitivity 1)
exchange resin (in the hydrogen ferm) and collect the eluate in
Using a 40 ml test Portion and a cell of Optical path length a glass bottle provided with a weil-fitting glass stopper. Add
about 10 g of the same resin to each litre of collected eluate for
40 mm, @N = 0,200 mg/l gives an absorbance of about
0,69 units. storage purposes.

Using a 40 ml test Portion and a cell of Optical path length

4.1.2 Distillation method
lo mm, @N = 0,750 mg/l gives an absorbance of about
0,65 units.
Add 0,lO + 0,Ol ml of sulfuric acid (Q = 1,84 g/ml) to
1 000 & 10 ml of distilled water and redistil in an all glass
2 Reference apparatus. Discard the first 50 ml of distillate, and then collect
the distillate in a glass bottle provided with a weil-fitting glass
ISO 5664, Water guality - Determination of ammonium - stopper. Add about 10 g of strongly acidic cation exchange
Dis tilla tion and titra tion me tho d. resin (in the hydrogen form) to each litre of collected distillate.

1) Data from a United Kingdom interlaboratory exercise involving five participants.

1
 SIST ISO 7150-1:1996

ISO 7150/1-1984 (EI

4.2 Colour reagent. 4.7 Cleaning solution.

Dissolve 130 + 1 g of sodium salicylate (C7HGOsNa) and Dissolve 100 + 2 g of potassium hydroxide in 100 + 2 ml of
130 Ifr 1 g of trisodium citrate dihydrate (C6H507Na3m2H20) water. Cool the Solution and add 900 + 50 ml of 95 % (V/ V)
in water (4.1) in a 1000 ml one-mark volumetric flask. ethanol.
Add sufficient water to give a total liquid volume of about
Store the Solution in a polyethylene bettle.
950 ml and then add 0,970 + 0,005 g of sodium nitroso-
pentacyanoferrate(III) dihydrate { sodium nitroprusside,
[Fe(CN)5NOINa2.2H20}. D issolve the solid and then dilute to 5 Apparatus
the mark with water.
Ordinary laboratory apparatus and
Stored in an amber glass bottle, this reagent is stable for at
least 2 weeks. 5.1 Spectrometer, capable of operating at a wavelength of
655 nm with cells of Optical path length between 10 and
4.3 Sodium dichloroisocyanurate, Solution. 50 mm.

Dissolve 32,0 + 0,l g of sodium hydroxide in 500 If: 50 ml 5.2 Water-bath or incubator, capable of being maintained
of water (4.1). Cool the Solution to room temperature and at 25 * 1 OC.
add 2,00 ?I 0,02 g sodium dichloroisocyanurate dihydrate
K3N303CI,Na -2H,O) to the Solution. Dissolve the solid and NOTE ON CLEANING OF GLASSWARE
transfer the Solution quantitatively to a 1 000 ml one-mark All glassware shall be carefully cleaned using the cleaning Solution (4.7)
volumetric flask. Dilute to the mark with water. followed by thorough rinsing with water (4.1).

Stored in an amber glass bottle, this reagent is stable for at

least 2 weeks. 6 Sampling and samples

4.4 Ammonium nitrogen, iTeh STANDARD

Standard Solution, PREVIEW
Laboratory samples shall be collected in polyethylene or glass
bottles. They should be analysed as quickly as possible, or else
&$J = 1 000 mg/l.
(standards.iteh.ai)
stored at between 2 and 5 OC until analysed. Acidification with
pH < 2 may also be used as an aid to preser-
sulfuric acid to
Dissolve 3,819 + 0,004 g of ammonium chloride (dried at
vation, provided that possible contamination of the acidified
105 OC for at least 2 h) in about 800 ml of water (4.1) SIST in a ISO 7150-1:1996
Sample by absorption of any atmospheric ammonia is avoided.
1 000 ml one-mark volumetric flask.https://standards.iteh.ai/catalog/standards/sist/5b65be87-65ff-412c-9dfb-
Dilute to the mark with
water.
feb520e40890/sist-iso-7150-1-1996
7 Procedure
1 ml of this Standard Solution contains 1 mg of ammonium
nitrogen.
7.1 Test Portion
Stored in a stoppered glass bottle, this Solution is stable for at
The maximum test Portion volume is 40 ml, which tan be used
least 1 month.
for the determination of ammonium nitrogen concentrations up
to @N = 1 mgll.
4.5 Ammonium nitrogen, Standard Solution,
QN = 100 mg/l. Smaller test portions may be used as appropriate in Order to
accommodate much higher ammonium nitrogen concentra-
Pipette 100 ml of ammonium nitrogen Standard Solution (4.4) tions. Laboratory samples containing suspended matter should
into a 1 000 ml one-mark volumetric flask. Dilute to the mark be allowed to settle, or filtered by gravity through a pre-rinsed
with water. glass fibre Paper before taking the test Portion. Alternatively,
Prior distillation of the Sample may be used (sec clause 10).
1 ml of this Standard Solution contains 0,l mg of ammonium
nitrogen. 7.2 Preparation of test solution
Stored in a stoppered glass bottle, this solution is stable for Pipette the test Portion (7.1) into a 50 ml one-mark volumetric
1 week. flask, and, if necessary, dilute to 40 + 1 ml with water (4.1).

4.6 Ammonium nitrogen, Standard Solution, 7.3 Determination

&J = 1 mg/l.
7.3.1 Formation of the absorbing compound
Pipette 1 ml of ammonium nitrogen Standard Solution (4.5) into
a 100 ml one-mark volumetric flask. Dilute to the mark with Add 4,00 t 0,05 ml of colour reagent (4.2) and mix weil. Then
water. add 4,00 & 0,05 ml of sodium dichloroisocyanurate Solution
(4.3) and mix weil.
1 ml of this Standard Solution contains 1 pg of ammonium
nitrogen. NOTE - After this addition the pH of the Solution should be
12,6 + 0,l. Extremes of acidity or alkalinity in the Sample may Cause
Prepare this Solution immediately before use. deviation.

2
 SIST ISO 7150-1:1996

ISO 7150/1-1984 (El

Dilute to the mark with water (4.1). Shake the flask thoroughly 7.5.4 Plotting the calibration graph
and place it in the water-bath (5.2) maintained at 25 * 1 OC.
Subtract the absorbance of the zero member from the ab-
NOTE - Other water-bath temperatures may be used, but all deter- sorbances obtained from the other calibration solutions. Plot a
minations and calibrations should be carried out at the same graph of absorbance against mass of ammonium nitrogen, r??N,
temperature (within + 1 K). for each cell path length. This graph should be linear and
should pass through the origin.
7.3.2 Spectrometric measurements

After at least 60 min, remove the flask from the water-bath and 8 Expression of results
measure the absorbance of the Solution at the wavelength of
maximum absorbance, approximately 655 nm, in a cell of
8.1 Method of calculation
suitable path length against water (4.1) in the reference cell.
The absorbance due to ammonium in the test Portion, A,, is
NOTE - The wavelength of maximum absorbance should be checked
when this method is first used, and should be used in all subsequent
given by the equation
determinations.
A, = A, - A,

7.4 Blank test where

Proceed as described in 7.2 and 7.3, but using 40 + 1 ml of
A, is the absorbance of the test Solution (7.3.2);
water (4.1) in place of the test Portion.

A, is the absorbance of the blank test Solution (7.4).

7.5 Calibration

7.51 Preparation
iTeh STANDARD PREVIEW
of the set of calibration solutions
NOTE - A, and A, must be measured
for a particular Sample.
in cells of the same path length

(standards.iteh.ai)
To a series of nine 50 ml one-mark volumetric flasks add, by The ammOniUm nitrogen COntent, @N, in milligrams per litt-e, is
means of a burette, the volumes of ammonium nitrogen stan- given by the formula
dard Solution (4.6) shown in table 1. SIST ISO 7150-1:1996
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mN
Add water (4.1) to give a volume of 40 + 1 ml if necessary.
feb520e40890/sist-iso-7150-1-1996
V

7.5.2 Formation of the absorbing compound where

See 7.3.1. mN is the mass, in micrograms, of ammonium nitrogen,

determined from A, and the calibration graph (7.5.4) for the
appropriate cell path length;
7.5.3 Spectrometric measurements
V is the test Portion volume, in millilitres.
Proceed according to 7.3.2 using the cell path length(s)
specified in table 1 for absorbance measurements.
See table 2 fOr COnVWSiOn Of eN t0 ammonia and ammonium
concentrations.
Table 1 - Volumes of Standard solution for use
in the calibration series
Table 2 - Conversion table
Volume of Mass of
Standard ammonium Gell path length QN @NH, c(NH;)
solution (4.6) nitrogen, mN
ml mm .
wl/l I mg/1 mg/1 pmol/l
w
0,oo * 0 10 and 40”” @N = 1 mg/1 1 1,216 1,288 71,4
2,00 2 40
4,00 4 40 @NH, = 1 mg!1 0,823 1 1,059 5817
6,00 6 40
8,00 @NH,+ = 1 mg/1 0,777 0,944 1 55,4
8 40
IO,00 10 10
dNH,+) = 1 ~mol/l 0,014 0,017 0,018 1
20,OO 20 IO
30,oo 30 IO
40,oo 40 10 Example :
* The zero member.
An ammonium ion concentration, QNH+, of I mg/I cor-
** 50 mm path length cells may be used. responds to a nitrogen concentration of 0377 mg/l.

3
 SIST ISO 7150-1:1996

ISO 7150/1-1984 (EI

8.2 Precision tion of ammonium nitrogen in the test Sample. The concentra-
tion in the original Sample is given by the formula
Repeatability and reproducibility Standard deviations have been
determined as shown in table 3.

9 lnterferences where
A range of substances often encountered in water samples has is the result on the test Sample;
@Nl
been tested for possible interference with this method. Full
details are given in annex A. The only serious inter-ferences VI and V2 are as defined above.
which have been encountered are those from aniline and
ethanolamine, and represent the interference to be expected
from primary amines in general. However, such substances are 11 Notes on procedure
seldom encountered at appreciable concentrations in water
samples.
11.1 General
Extremes of acidity or alkalinity will interfere with the formation
of the absorbing compound, as will the presence of any The determination of low concentrations of ammonium is par-
substance causing reduction of hypochlorite ions, although ticularly susceptible to bias caused by the presence of traces of
these circumstances are unlikely to arise in most water ammonium in the analytical environment. While careful
samples. The procedure referred to in clause 10 should be attention to all the instructions given in this part of ISO 7150
adopted in such circumstances. should minimize this susceptibility, the possibility of biased
results remains. Two methods for obtaining an indication of
In Saline samples, interference from magnesium precipitation possible bias are now presented.
arises when the complexing capacity of the citrate in the

necessary (sec clause IO).

iTeh STANDARD
reagents is exceeded. For this reason, preliminary distillation is 11.2 PREVIEW
Monitoring of blank and calibration Standard
absorbance values
(standards.iteh.ai)
The actual absorbance values (measured against water in the
10 Special cases
reference cell) obtained for the blank test Solution and the
SIST ISO 7150-1:1996
calibration series shall be recorded on each occasion the
If samples are excessively coloured or https://standards.iteh.ai/catalog/standards/sist/5b65be87-65ff-412c-9dfb-
Saline such that errors are
method is used. This record of values will enable any deviation
likely in the absorbance measurements or suchfeb520e40890/sist-iso-7150-1-1996
that in-
to be recognized. Such deviation may be caused by contami-
tet-ference from high concentrations of magnesium or chloride
nation of the blank test Solution or calibration series with
is likely, a test Sample shall be prepared by distillation. The pro-
ammonium, or by a deficiency in one or more of the reagents.
cedure given in ISO 5664 shall be followed, but note that col-
In either case, remedial measures shall be taken. Annex B
lection of the distillate shall be made in 1 % (V/ V) hydrochloric
quotes typical values obtained in an interlaboratory exercise.
acid. The distillate shall then be neutralized and made up to a
measured volume, V2, in millilitres. The volume of Sample taken
for distillation, VI, in millilitres, shall also be noted. 11.3 Checking the accuracy of analytical results

The test Sample thus prepared tan then be analysed as de- When this method is first used, an estimate of the total stan-
scribed in clause 7. However, the result will be the concentra- dard deviation (with at least 9 degrees of freedom) should be

Table 3 - Repeatability and reproducibility Standard deviations”

Ammonium
Standard deviation, s
nitrogen Cell
Sample** concentration path length
Repeatability Reproducibility
QN

ma/l mm mo/I mg/1

Standard Solution 0,150 40 0,002”“” -
Standard Solution l,oo 10 0,005 to 0,025t 0,015 to 0,038t
Standard Solution 5,00 10 0,036”“” -
Weil water 0,217 40 0,002 t 0,004 to 0,OlO”r
Sewage effluent 0,877 IO 0,007 to 0,027? 0,009 to 0,027-f

* Data from the United Kingdom.

** All test Portion volumes were 40 ml except for the 5,00 mg/1 Standard Solution, for which it was 5 ml.

*** Result from one laboratory; 9 degrees of freedom.

t The lowest and highest values from an interlaboratory exercise involving five participants. All values have
9 degrees of freedom.

4
 SIST ISO 7150-1:1996

ISO 7150/1-1984 (El

obtained on the determination of a control Standard ammonium After at least 20 more determinations of this control Standard
nitrogen Solution with a concentration of approximately 50 % Solution have been made, with all values complying with the
of that of the most concentrated calibration Solution. criterion above, those values shall be used to recalculate the
value of s1 for subsequent use.
This control Standard Solution shall not be used for calibration
purposes.
12 Test report
One Portion of this control Standard Solution should be
analysed with every subsequent batch of determinations; The test report shall include the following information :
calibration shall be performed with the calibration series. The
determined concentration of this control Standard Solution shall a) a reference to this part of ISO 7150;
lie within the concentration range
b) all information necessary for complete identification of
@N2+ SS, the Sample;

c) details of the storage and preservation of the laboratory

Sample before analysis;
eN2 is the concentration of the Solution;
d) a Statement of the repeatability achieved;
s1 is the predetermined Standard deviation for the control
Standard solution. e) the results and the method of expression used;

If this criterion is not attained in any batch of analyses, the f) details of any operations not included in this part of
reasons for the bias thus revealed shall be investigated, and the ISO 7150, or regarded as optional, together with any
batch of analyses shall then be repeated. circumstance that may have affected the results.

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