EN ISO 14911:1999

Water quality - Determination of dissolved Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ and Ba2+ using ion chromatography - Method for water and waste water (ISO 14911:1998)

Migrated from Progress Sheet (TC Comment) (2000-07-10): E-mail of 980119 to Safoura: as FDIS is almost ready, we can only follow with ++ a UAP but WHEN the ISO will be published (TA/980120) ++ Barz's fax dated 980917: CS requested to launch the UAP at the reception of the ++ German version (TA/980917)

Wasserbeschaffenheit - Bestimmung der gelösten Kationen Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ und Ba2+ mittels Ionenchromatographie - Verfahren für Wasser und Abwasser (ISO 14911:1998)

Diese Internationale Norm legt ein Verfahren zur Bestimmung der gelösten Kationen Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ und Ba2+ in Wasser (z.B. Trinkwasser, Oberflächenwasser und Abwasser) fest. Eine geeignete Vorbehaltung der Probe (z.B. Verdünnung) und die Anwendung eines Leitfähigkeitsdetektors (LD) machen die in Tabelle 1 angegebenen Arbeitsbereiche möglich. Die Anwendbarkeit des Verfahrens für Abwasserproben sollten in jedem Fall geprüft werden.

Qualité de l'eau - Dosage par chromatographie ionique, des ions Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ et Ba2+ dissous - Méthode applicable pour l'eau et les eaux résiduaires (ISO 14911:1998)

La présente Norme internationale spécifie une méthode de dosage des cations Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ et Ba2+ dissous dans l'eau (par exemple eau potable, eaux de surface, eaux résiduaires).  En faisant subir un prétraitement approprié à l'échantillon (par exemple une dilution) et en utilisant un détecteur conductimétrique (CD), il est possible d'obtenir les gammes de travail données dans le tableau 1.  L'applicabilité de cette méthode pour les échantillons d'eaux résiduaires doit être vérifiée au cas par cas.

Določevanje raztopljenih ionov Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ in Ba2+ z ionsko kromatografijo - Metoda za vodo in odpadno vodo (ISO 14911:1998)

General Information

• Status: Published
• Publication Date: 17-Aug-1999
• Withdrawal Date: 28-Feb-2000
• ICS: 13.060.01 - Water quality in general
• Technical Committee: CEN/TC 230 - Water analysis
• Drafting Committee: CEN/TC 230 - Water analysis
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 21-May-2008
• Completion Date: 21-May-2008
• Ref Project: SIST EN ISO 14911:2000 - Water quality - Determination of dissolved Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ and Ba2+ using ion chromatography - Method for water and waste water (ISO 14911:1998)

Standards Content (Sample)

SLOVENSKI STANDARD
01-februar-2000
'RORþHYDQMHUD]WRSOMHQLKLRQRY/L1D1+.0Q&D0J6ULQ
%D]LRQVNRNURPDWRJUDILMR0HWRGD]DYRGRLQRGSDGQRYRGR,62
Water quality - Determination of dissolved Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+
and Ba2+ using ion chromatography - Method for water and waste water (ISO
14911:1998)
Wasserbeschaffenheit - Bestimmung der gelösten Kationen Li+, Na+, NH4+, K+, Mn2+,
Ca2+, Mg2+, Sr2+ und Ba2+ mittels Ionenchromatographie - Verfahren für Wasser und
Abwasser (ISO 14911:1998)
Qualité de l'eau - Dosage par chromatographie ionique, des ions Li+, Na+, NH4+, K+,
Mn2+, Ca2+, Mg2+, Sr2+ et Ba2+ dissous - Méthode applicable pour l'eau et les eaux
résiduaires (ISO 14911:1998)
Ta slovenski standard je istoveten z: EN ISO 14911:1999
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL ISO
STANDARD 14911
First edition
1998-10-01
Water quality — Determination of dissolved
+ + + + 2+ 2+ 2+ 2+
Li , Na , NH , K , Mn , Ca , Mg , Sr and
2+
Ba using ion chromatography — Method
for water and waste water
+ +
Qualité de l'eau — Dosage, par chromatographie ionique, des ions Li , Na ,
+ + 2+ 2+ 2+ 2+ 2+
NH , K , Mn , Ca , Mg , Sr et Ba dissous — Méthode applicable
pour l'eau et les eaux résiduaires
A
Reference number
ISO 14911:1998(E)
ISO 14911:1998(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.
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.
International Standard ISO 14911 was prepared by Technical Committee
TC 147, Water quality, Subcommittee SC 2, Physical, chemical,
biochemical methods.
Annexes A and B of this International Standard are for information only.
©  ISO 1998
All rights reserved. Unless otherwise specified, 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 Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
Printed in Switzerland
ii
©
ISO ISO 14911:1998(E)
Introduction
The essential minimum requirements of an ion chromatographic system
applied within the scope of this International Standard are given in
clause 5.
The diversity of the appropriate and suitable assemblies and the procedural
steps depending on them permit a general description only.
Further information on the analytical technique is given in the normative
references (see clause 2) and the bibliography.
iii
INTERNATIONAL STANDARD  © ISO ISO 14911:1998(E)
+ + + + 2+
Water quality — Determination of dissolved Li , Na , NH , K , Mn ,
2+ 2+ 2+ 2+
Ca , Mg , Sr and Ba using ion chromatography — Method for
water and waste water
1 Scope
+ + + +
This International Standard specifies a method for the determination of the dissolved cations Li , Na , NH , K ,
2+ 2+ 2+ 2+ 2+
Mn , Ca , Mg , Sr and Ba in water (e.g. drinking water, surface water, waste water).
An appropriate pretreatment of the sample (e.g. dilution) and the application of a conductivity detector (CD) make
the working ranges given in table 1 feasible.
The applicability of the method for waste water samples should be proved in each case.
Table 1 — Working ranges of the analytical method
Cation Typical working range with 10 μl loop
1)
mg/l
Lithium 0,01 to  1
Sodium 0,1 to 10
Ammonium 0,1 to 10
Potassium 0,1 to 10
Manganese 0,5 to 50
Calcium 0,5 to 50
Magnesium 0,5 to 50
Strontium 0,5 to 50
Barium 1  to 100
1) The working range is limited by the ion-exchange capacity of the separator column.
If necessary, the sample shall be diluted to meet the working range, or use a 100 μl loop
for lower working ranges.
2 Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
© ISO
ISO 14911:1998(E)
ISO 5667-1:1980, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes.
ISO 5667-2:1991, Water quality — Sampling — Part 2: Guidance on sampling techniques.
ISO 5667-3:1994, Water quality — Sampling — Part 3: Guidance on the preservation and handling of samples.
ISO 6058:1984, Water quality — Determination of calcium content — EDTA titrimetric method.
ISO 6059:1984, Water quality — Determination of the sum of calcium and magnesium — EDTA titrimetric method
ISO 6333:1986, Water quality — Determination of manganese — Formaldoxime spectrometric method.
ISO 7980:1986, Water quality — Determination of calcium and magnesium — Atomic absorption spectrometric
method.
ISO 8466-1:1990, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 1: Statistical evaluation of the linear calibration function.
ISO 8466-2:1993, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 2: Calibration strategy for non-linear second order calibration functions.
3 Interferences
3.1  Organics such as amino acids and aliphatic amines can interfere with the determination of inorganic cations.
3.2  If a strong complexing agent such as pyridine-2,6-dicarboxylic acid (PDA) is not present in the mobile phase,
2+ 2+ 2+
and if the suppressor technique is not used, cross interferences from other cations like Zn , Ni , Cd etc. can
occur.
3.3  Cross-sensitivities with other cations, e.g. manganese, are dependent on the selectivity of the separator
column used. If the quality requirements in clause 8 are not achieved, the sample shall be diluted.
+ +
3.4  Cross-sensitivities in the determination of NH and Na can occur when there are large differences in
concentration.
3.5  Solid material and organic compounds (such as mineral oils, detergents and humic acids) shorten the lifetime
of the separator column. They are therefore eliminated from the sample (9.3).
4 Principle
+ + + + 2+ 2+ 2+ 2+ 2+
Liquid chromatographic separation of Li , Na , NH , K , Mn , Ca , Mg , Sr and Ba by means of a separator
column. A low-capacity cation exchanger is used as the stationary phase, and usually, aqueous solutions of mono-
and dibasic acids as mobile phases (eluent, see 6.16).
These cations are detected by conductivity. It is essential that the eluents have a sufficiently low conductivity. For
this reason, a conductivity detector (CD) is often combined with a suppressor device (e.g. an anion exchanger)
which will reduce the conductivity of the eluent and transform the separated cations into their corresponding bases.
In the conductivity detection without chemical suppression, the difference between the ion equivalent conductivities
is measured directly after the column. This difference should be as high as possible and the detector cell
temperature should be stabilized within ± 0,1 °C.
The concentration of the respective cations is determined by a calibration of the overall procedure. Particular cases
can require calibration by means of standard addition (spiking).
© ISO
ISO 14911:1998(E)
5 Essential minimum requirements
The essential minimum requirements of an ion chromatographic system applied within the scope of this
International Standard are the following:
a) Resolution power (R) of the column: For the cation to be determined it is essential that the peak
resolution does not fall below R = 1,3 (see clause 8, figure 3).
b) Method of detection: Measurement of the electrical conductivity with or without
suppressor device.
c) Applicability of the method: Working ranges according to table 1.
d) Calibration (10.2): Calibration and determination of the linear (see ISO 8466-1) or
quadratic (see ISO 8466-2) working range. Use of the method
of standard addition to special cases of application (see 10.3).
e) Guaranteeing the analytical quality (10.3.2): Validity check of the calibration function. Replicate
determinations, if necessary.
6 Reagents
Use only reagents of recognized analytical grade. Carry out weighing with an accuracy of ±1 % of the nominal
mass. The water shall have an electrical conductivity of < 0,01 mS/m and shall not contain particulate matter of a
particle size > 0,45 μm.
6.1  DL-2,3-Diaminopropionic acid monohydrochloride (DAP), C H N O �HCI.
3 8 2 2
6.2  Hydrochloric acid solution, c(HCl) = 7,7 mol/l.
6.3  Methanesulfonic acid, CH O S (≥ 99%).
4 3
6.4  Pyridine 2,6-dicarboxylic acid (PDA), C H NO
.
7 5 4
6.5  Tartaric acid, C H O
.
4 6 6
6.6  Nitric acid solution, c(HNO = 1 mol/l.
)
6.7  Lithium nitrate, LiNO .
6.8  Sodium nitrate, NaNO .
6.9  Ammonium chloride, NH Cl.
6.10  Potassium nitrate, KNO .
6.11  Manganese nitrate tetrahydrate, Mn(NO ) �4H O.
3 2 2
6.12  Calcium nitrate tetrahydrate, Ca(NO ) �4H O.
3 2 2
6.13  Magnesium nitrate hexahydrate, Mg(NO ) �6H O.
3 2 2
6.14  Strontium nitrate, Sr(NO )
.
3 2
6.15  Barium nitrate, Ba(NO )
.
3 2
© ISO
ISO 14911:1998(E)
6.16  Eluents, their choice depending on the type of separator column and detector.
Follow the column manufacturer´s instructions for the exact composition of the eluent. The eluent compositions
described in 6.16.1.1, 6.16.1.2, 6.16.2.1.1 and 6.16.2.2 are examples only.
A selection of reagents for preparing common eluents is presented in 6.1 to 6.6.
Degas all eluents or prepare eluents using degassed water. Avoid any renewed gas pick-up during operation (e.g.
by helium sparging). Store the eluents in the dark and renew as required.
6.16.1  Examples of eluents for ion chromatography using the suppressor technique
For the application of the suppressor technique, solutions containing strong acids like hydrochloric acid or
methanesulfonic acid or mixtures of these acids with DAP (6.1) can be used. Eluent concentrates are not
recommended, but can be used.
6.16.1.1  Hydrochloric acid / DAP eluent
+ + + + 2+ 2+ 2+ 2+ 2+
The following eluent is applicable for the determination of Li , Na , NH , K , Mn , Ca , Mg , Sr and Ba :
Place 5,2 ml of a hydrochloric acid solution (6.2) and 0,562 g ± 0,006 g of DAP (6.1) into a 1000 ml volumetric flask
and dilute to volume with degassed water.
The solution contains 0,04 mol/l of hydrochloric acid and 0,004 mol/l DAP (6.1). Store the solution at 4 °C to 6 °C,
renew it every 7 d.
6.16.1.2  Methanesulfonic acid eluent
+ + + + 2+ 2+ 2+ 2+ 2+
The following eluent is applicable for the determination of Li , Na , NH , K , Mn , Ca , Mg , Sr and Ba :
Place 1,3 ml of methanesulfonic acid-solution (6.3) into a 1000 ml volumetric flask and dilute to volume with
degassed water.
The solution contains 0,02 mol/l of methanesulfonic acid. Renew the eluent every 3 d.
6.16.2  Examples of eluents for ion chromatography without using the suppressor technique
For ion chromatography techniques without suppressor devices, acids like nitric, tartaric, oxalic etc. are used. The
solutions can contain various additions, e.g. alcohols. The concentration of the acids is usually in the range of
0,001 mol/l to 0,01 mol/l. Concentrate and eluent solutions are prepared as described in 6.16.
6.16.2.1  Tartaric acid/PDA concentrate
The eluent concentrate has proved to be successful for the eluent preparation (6.16.2.1.1):
Place 1,671 g ± 0,017 g of PDA (6.4) in a beaker of capacity 1000 ml, add approximately 500 ml of water (clause 6).
Stir and dissolve by heating (60 °C to 80 °C). After cooling add 6,003 g ± 0,060 g tartaric acid (6.5) and transfer the
cool solution into a 1000 ml volumetric flask and dilute to volume with water.
The solution contains 0,01 mol/l PDA and 0,04 mol/l tartaric acid and is stable for one month if stored at 4 °C to
6 °C.
6.16.2.1.1  Tartaric acid/PDA eluent
+ + + + 2+ 2+ 2+ 2+ 2+
For the determination of Li , Na , NH , K , Mn , Ca , Mg , Sr and Ba , the following eluent has proved to be
successful:
Place 100 ml of the concentrate (6.16.2.1) into a 1000 ml volumetric flask and dilute to volume with water (clause 6).
© ISO
ISO 14911:1998(E)
The solution contains 0,001 mol/l PDA and 0,004 mol/l tartaric acid. The eluent pH is 2,8. Renew the eluent every
3 d.
6.16.2.2  Nitric acid eluent
+ + + + 2+ 2+ 2+ 2+ 2+
For the determination of Li , Na , NH , K , Mn , Ca , Mg , Sr and Ba , the following eluent has proved to be
successful:
Place 500 ml of water (clause 6) into a 1000 ml volumetric flask, add 20 ml of the nitric acid solution (6.6) and dilute
to volume with water.
The solution contains 0,02 mol/l nitric acid. Renew the eluent every 3 d.
6.17  Stock solutions
+ + + + 2+ 2
...