SIST EN ISO 10304-1:1998
(Main)Water quality - Determination of dissolved fluoride, chloride, nitrite, orthophosphate, bromide, nitrate and sulfate ions, using liquid chromatography of ions - Part 1: Method for water with low contamination (ISO 10304-1:1992)
Water quality - Determination of dissolved fluoride, chloride, nitrite, orthophosphate, bromide, nitrate and sulfate ions, using liquid chromatography of ions - Part 1: Method for water with low contamination (ISO 10304-1:1992)
Migrated from Progress Sheet (TC Comment) (2000-07-10): ISO 10304-1:1992 to be submitted to the UAP
Wasserbeschaffenheit - Bestimmung der gelösten Anionen Fluorid, Chlorid, Nitrit, Orthophosphat, Bromid, Nitrat und Sulfat mittels Ionenchromatographie - Teil 1: Verfahren für gering belastete Wässer (ISO 10304-1:1992)
Dieser Teil der En 30304 beschreibt ein Verfahren zur Bestimmung von Fluorid, Chlorid, Nitrit, Phosphat(ortho-), Bromid, Nitrat und Sulfat in wenig belastete Wässern (wie z.B. Trinkwasser, Niederschlagswasser, Grundwasser und Oberflächenwasser) in den folgenden Massenkonzentrationen: Fluorid (F): 0,01 mg/l bis 10 mg/l; Chlorid (Cl): 0,1 mg/l bis 50 mg/l; Nitrit (NO2): 0,05 mg/l bis 20 mg/l; Orthophosphat: 0,1 mg/l bis 20 mg/l; Bromid (Br) : 0,05 mg/l bis 20 mg/l; Nitrat (NO3): 0,1 mg/l bis 50 mg/l; Sulfat (SO4): 0,1 mg/l bis 100 mg/l.
Qualité de l'eau - Dosage des ions fluorure, chlorure, nitrite, orthophosphate, bromure, nitrate et sulfate dissous, par chromatographie des ions en phase liquide - Partie 1: Méthode applicable pour les eaux faiblement contaminées (ISO 10304-1:1992)
La CEI 62642-6:2011 spécifie les exigences, les critères de performance et les procédures d'essai pour les alimentations destinées à être utilisées comme partie de systèmes d'alarme contre l'intrusion et les hold-up (I&HAS). L'alimentation doit être intégrée à un composant d'un I&HAS ou être un ensemble séparé. Les fonctions de commande de l'alimentation peuvent être intégrées comme partie du dispositif de l'alimentation, ou peuvent être fournies par un autre composant de l'I&HAS, par exemple un équipement de contrôle et de signalisation.
Kakovost vode - Določevanje raztopljenih fluoridnih, kloridnih, nitritnih, ortofosfatnih, bromidnih, nitratnih in sulfatnih ionov z uporabo ionske kromatografije - 1. del: Metoda za malo obremenjene vode (ISO 10304-1:1992)
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 10304-1:1998
01-januar-1998
.DNRYRVWYRGH'RORþHYDQMHUD]WRSOMHQLKIOXRULGQLKNORULGQLKQLWULWQLK
RUWRIRVIDWQLKEURPLGQLKQLWUDWQLKLQVXOIDWQLKLRQRY]XSRUDERLRQVNH
NURPDWRJUDILMHGHO 0HWRGD]DPDORREUHPHQMHQHYRGH ,62
Water quality - Determination of dissolved fluoride, chloride, nitrite, orthophosphate,
bromide, nitrate and sulfate ions, using liquid chromatography of ions - Part 1: Method for
water with low contamination (ISO 10304-1:1992)
Wasserbeschaffenheit - Bestimmung der gelösten Anionen Fluorid, Chlorid, Nitrit,
Orthophosphat, Bromid, Nitrat und Sulfat mittels Ionenchromatographie - Teil 1:
Verfahren für gering belastete Wässer (ISO 10304-1:1992)
Qualité de l'eau - Dosage des ions fluorure, chlorure, nitrite, orthophosphate, bromure,
nitrate et sulfate dissous, par chromatographie des ions en phase liquide - Partie 1:
Méthode applicable pour les eaux faiblement contaminées (ISO 10304-1:1992)
Ta slovenski standard je istoveten z: EN ISO 10304-1:1995
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
SIST EN ISO 10304-1:1998 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 10304-1:1998
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SIST EN ISO 10304-1:1998
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SIST EN ISO 10304-1:1998
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SIST EN ISO 10304-1:1998
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SIST EN ISO 10304-1:1998
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SIST EN ISO 10304-1:1998
INTERNATIONAL
STANDARD
103044
First edition
19924 1-I 5
Water quality - Determination of dissolved
fluoride, chloride, nitrite, orthophosphate,
bromide, nitrate and sulfate ions, using liquid
chromatography of ions -
Part 1:
Method for water with low contamination
Qualite de I’eau - Dosage des ions fluorure, chlorure, nitrite,
orthophosphate, bromure, nitrate et sulfate dissous, par
Chromatographie des ions en Phase liquide -
Partie 1: Methode applicable pour les eaux faiblement contaminees
P--Y--
--.- _~
--
Reference number
--
-----~
---.--~_-_ ISO 10304-1:1992(E)
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SIST EN ISO 10304-1:1998
ISO 10304-1:1992(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
International organizations, govern-
represented on that committee.
mental and non-governmental, in liaison with ISO, also take patt 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 Inter-
national Standard requires approval by at least 75 % of the member
bodies casting a vote.
International Standard ISO 10304-1 was prepared by Technical Commit-
tee ISO/TC 147, Water quality, Sub-Committee SC 2, Physical, Chemical,
biochemical methods.
ISO 10304 consists of the following Parts, under the general title Water
quality - of dissolved fluoride, chloride, nitrite,
Determination
orthophosphate, bromide, nitrate and sulfate ions, using liquid chro-
matography of ions:
- Part 1: Method for water with low contamination
- Part 2: Method for waste water
- Part 3: Determination of chromate, thiocyanate and thiosulfate
Annex A of this part of ISO 10304 is for information only.
0 ISO 1992
All rights reserved. No part of this publication may be reproduced or utilized in any form
or by any means, electronie or mechanical, inciuding photocopying and microfilm, without
Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-121 1 Geneve 20 l Switzerland
Printed in Switzerland
ii
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SIST EN ISO 10304-1:1998
ISO 1030401:1992(E)
Introduction
Many different ion-exchange chromatography Systems tan be consid-
ered. It is therefore not appropriate to indicate the type of column, mo-
bile Phase, detector type etc. that is to be used. Thus detailed
information is not given at any Stage during the method, although guid-
ante is provided. However, the quality Parameters which should be met
by the chromatography conditions Chosen are defined.
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SIST EN ISO 10304-1:1998
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SIST EN ISO 10304-1:1998
INTERNATIONAL STANDARD ISO 10304-1:1992(E)
- Determination of dissolved fluoride, chloride,
Water quality
nitrite, orthophosphate, bromide, nitrate and sulfate ions,
using liquid chromatography of ions -
Part 1:
Method for water with low contamination
1.2.2 The determination of fluoride in particular is
1 Scope
subject to interference by formic acid, acetic acid
and carbonate, even at low concentrations.
1 .l General
1.2.3 Cross sensitivity (lack of resolution) may oc-
This part of ISO 10304 specifies a method for the
cur in the case of large differentes in concentration
determination of fluoride, chloride, nitrite,
between the anions determined (F, Cl, NO,, PO,, Br,
orthophosphate, bromide, nitrate and sulfate in wa-
NO,, SO,).
ter with low contamination (e.g. drinking water, rain
water, ground water and surface water) in the fol-
1.2.4 The bromide and Phosphate anions do not
lowing ranges:
interfere in the working range specified, unless oth-
erwise stated.
Fluoride (F): 0,Ol mg/1 to IO mg/l
0,l mg/l to 50 mg/l
Chloride (Cl):
1.2.5 In a buffered eluent (e.g. carbonate/hydro-
gencarbonate), the determination will not be influ-
0,05 mg/l to 20 mg/l
Nitrite (NO,):
enced by the Sample pH in the range of pH 2 to
Orthophosphate (PO,): 0,l mg/l to 20 mg/1
pH 9.
Bromide (Br): 0,05 mg/l to 20 mg/l
Nitrate (NO,): 0,l mg/l to 50 mg/1 1.2.6 The concentration ratios given in table 1 were
checked experimentally for various representative
0,l mg/1 to 100 mg/1
Sulfate (SO,):
No interferences could be observed
conditions.
when 50 ~1 of Sample volume was used for the
used without charges
NOTE 1 Anion Symbols are
chromatographic analysis.
throughout the text.
In certain cases, the range of application may be 1.2.7 The information in 1.2.4 to 1.2.6 is valid only
changed by variations in the working conditions (e.g. as long as the quality requirements of the separat-
Sample volume, dilution, separating columns, pre- ing column are fulfilled (see clause 6) and the elec-
concentration techniques, sensitivity ranges of de- trical conductivity of the Sample is less than
tectors, etc.). 1 000 pS/cm (except fluoride: c 500 pS/cm). For na-
tural samples, the peak resolution (n> needs to be
better than 1,3 (see figure 3).
1.2 Interferences
3.2.8 Solid material and organic cornpounds (e.g.
mineral oils, detergents and humic acids) shorten
1.2.1 Some organic acids, such as malonic acid,
the Iife-time of the separating column. They should
malcic acid and malic acid, may interfere in the de-
therefore be removed from the Sample Prior to
termination of inorganic anions if they are present
analysis (see clause 7).
in high concentrations.
1
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SIST EN ISO 10304-1:1998
ISO 10304~1:1992(E)
1.2.9 Inorganic acids, such as fluoroborate acid or ISO 5667-2:1991, Wafer quality - Sampling -
chlorite, may interfere with the determination. Part 2: Guidance on sampling techniques.
ISO 5667-3:-‘), Water quality - Sampling - Part 3:
Table 1 - Cross sensitivity of anions
Guidance on the preservafion and handling of sam-
ples.
Maximum tolerable absolute
Ratio of the mass
concentration of interfering
concentrations
ions
ISO 8466~1:1990, Water quality - Calibration and
solutelinterfering ion
evaluation of analyticai methods and estimation of
mg/l
performante characteristics - Part 1: Statistical
F/CI 1500 Sum of all ions 400
evaluation of the linear caiibrafion function.
5
CI/NO, 150 NO2
3 Principle
500
CI/NO, 1500 NO3
1500 so4 500
CI/SO,
Liquid chromatographical Separation of ions by
means of a separating column. Use of a low capacity
100
NO,/CI 1:250 Cl
anion exchanger as the stationary Phase, and usu-
20
N”2/Po4 1:50 po4
ally aqueous solutions of salts of weak monobasic
500
N”2/No3 1:500 NO3 and dibasic acids as mobile phases (eluent,
500 see 4.11). Detection by a conductivity detector (most
N02/so4 1500 so4
widely used); sometimes employed in combination
500 with a suppressor device (e-g. a cation exchanger)
PO,/CI 1:500 Cl
which decreases the conductivity of the eluent and
PO,/NO, 1:500 NO3 400
converts the separated anions into their corre-
PO,/Br 1:lOO Br 100
sponding acids.
1:lOO
100
P”4/No,
NO2
500
po4/so, 1:500 so4
NOTE 2 If no suppressor device is used, the conductiv-
ity of the eluent must be as low as possible. References
Br/CI 1:500 Cl 500 covering this analytical techniques are summarized in
annex A.
Br/PO, 1:lOO 100
po4
100
Br/NO, 1:50 NO3
so4 500 4 Reagents
Br/S04 1:500
1:500 Cl 500 Use only reagents of recognized analytical grade.
NO,/CI
The water shall have an electrical conductivity of
NO,/Br 1:lOO Br 100
< 0,l @/cm and shall be free of particulate matter
N03/SO, 1:500 so4 500
with diameter > 0,45 pm. The increase of the elec-
trical conductivity due to an uptake of carbon dioxide
SO&I 1:500 Cl 500
does not interfere with the determination.
1:500 NO3 400
SO4P03
4.1 Sodium hydrogencarbonate (NaHCO,).
4.2 Sodium carbonate (Na,CO,).
2 Normative references
4.3 Potassium hydrogenphthalate (C,H,O,K).
The following Standards contain provisions which,
through reference in this text, constitute provisions
4.4 Sodium fluoride (NaF).
of this part of ISO 10304. At the time of publication,
the editions indicated were valid. All Standards are
4.5 Sodium chloride (NaCI).
subject to revision, and Parties to agreements based
on this part of ISO 10304 are encouraged to investi-
gate the possibility of applying the most recent edi-
4.6 Sodium nitrite (NaNO,).
tions of the Standards indicated below. Members of
IEC and ISO maintain registers of currently valid
4.7 Potassium dihydrogenphosphate (KH,PO,).
International Standards.
4.8 Sodium bromide (NaBr).
ISO 5667-1:1980, Water quality - Sampling -
Part 1: Guidance on the design of sampling pro-
grammes.
4.9 Sodium nitrate (NaNO,).
1) To be published. (Revision of ISO 5667.3:1985)
2
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SIST EN ISO 10304-1:1998
ISO 10304~1:1992(E)
4.11.2 Examples of eluents for ion chromatography
4.10 Sodium sulfate (Na,SO,).
without using the suppressor technique.
For ion chromatography techniques which do not
4.11 Eluents.
utilize suppressor devices, salt solutions (e.g. pot-
Different eluents are used, their choice depending
assium hydrogenphthalate, p-hydroxybenzoic acid,
on the type of separating column and detector.
sodium borate/gluconate and sodium benzoate) are
Therefore, follow the column manufacturer’s in-
used. The concentration of the salts is usually in the
structions for the exact composition of the eluent.
range of 0,000 5 mol/1 to 0,Ol mol/l. Concentrate and
The eluent compositions described in 4.11.1.1 and
eluent solutions are prepared as described in
4.11.2.2 are examples only.
4.11.2.1. Note that some alkaline concentrate sol-
utions of the cited salts are not stable. Adjust the pH
Prepare the eluents using degassed water. Avoid
of the eluent after the dilution of the concentrate.
any renewed gas pick-up during Operation (e.g. by
helium Superposition). In Order to avoid the growth
4.11.2.1 Potassium hydrogenphthalate concentrate.
of bacteria or algae, store the eluent in the dark and
renew every 2 d to 3 d.
The addition of the following eluent concentrate to
the Sample has proved to be helpful for Sample
pretreatment and eluent preparation (4.11.2.2).
4.11.1 Examples of eluents for ion chromatography
using the suppressor technique.
Place 20,5 g of potassium hydrogenphthalate (4.3) in
a graduated flask of nominal capacity 1 000 ml, and
For the application of the suppressor technique,
dilute to volume with water.
sodium hydroxide and satt solutions of weakly
such as sodium carbonate/
dissociated acids,
The Solution contains 0,l mol/ of potassium
sodium hydrogencarbonate, sodium hydrogencar-
hydrogenphthalate and is stable for a longer period
bonate and sodium tetraborate are used.
of time if stored at 4 “C to 6 “C.
4.11.2.2 Potassium hydrogenphthalate eluent.
4.11.1 .l Sodium carbonate/sodium hydrogencar-
bonate concentrate.
For the determination of F, Cl, NO,, PO,, Br, NO,,
and SO, in a Single run, the following eluent, as an
The addition of the following eluent concentrate to
example, has proved to be successful.
the Sample has proved to be successful for Sample
pretreatment and eluent preparation (see 4.11 .1.2).
Place 50 ml of the concentrate (4.11.2.1) in a gradu-
ated flask of nominal capacity 5 000 ml, dilute to
Place 25,4 g of sodium carbonate (4.2) and 25,2 g of
volume with water and adjust to pH 8,5.
sodium hydrogencarbonate (4.1) in a graduated flask
of nominal capacity 1 000 ml, and dilute to volume
The Solution contains 0,001 mol/1 of potassium
with water.
hydrogenphthalate.
The Solution contains 0,24 mol/1 of sodium carbon-
4.12 Stock solutions.
ate and 0,3 mol/1 of sodium hydrogencarbonate and
is stable for several months if stored at 4 “C to
Prepare stock solutions of concentration 1 000 mg/l
6 OC.
for each of the anions: F, Cl, NO,, PO,, Br, NO, and
so,.
4.11.1.2 Sodium carbonate/sodium hydrogencar-
Dissolve the appropriate mass of each of the sub-
bonate eluent.
stances, prepared as stated in table 2, in a small
The following eluent has proved to be applicable for
quantity of water in graduated flasks of nominal ca-
the determination of F, Cl, NO,, PO,, Br, NO, and
pacity 1 000 ml. Dilute to volume with water. The
SO, in a Single determination.
solutions are stable for several months if stored at
4 “C to 6 “C.
Place 50 ml of the concentrate (4.11.1.1) in a gradu-
ated flask of nominal capacity 5 000 ml, and dilute
Nitrite is easily oxidized to nitrate and therefore care
to volume with water. should be taken to ensure the stability of its con-
centration.
The Solution contains 0,002 4 mol/1 of sodium car-
bonate and 0,003 mol/1 of sodium hydrogencar- Alternatively, use commercially available stock sol-
bonate. utions of the required concentration.
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SIST EN ISO 10304-1:1998
ISO 10304=1:1992(E)
Table 2 - Mass Portion and pretreatment for stock solutions
ttreatment by dryin ‘1
Duration Temperature Mass of Portion
4
Anion Salt
h “C
Cl
1 2,210 0
Fluoride NaF 105
NaCI 2 105 1,648 4
Chloride
NaNO, 1 105 1,499 8
Nitrite
Orthophosphate KH,PO, 1 105 1,433 0
Bromide NaBr 6 105 1,287 7
NaNO, 24 105 1,370 7
Nitrate
Sulfate Na,SO, 1 105 1,479 0
1) Let the substance cool in a sealed desiccator after drying.
I
4.12.1 Mixed Standard solutions.
Table 3 - Volumes of stock solutions for the
Depending upon requirements, prepare Standard
preparation of the mixed Standard Solution l
solutions of different anion composition and con-
I
Anion
centration from the stock solutions (4.12). The risk
Stock solution
concentration
Anion
of changes in concentration caused by interaction
ml
rng/l
with the vessel material increases with decreasing
anion concentration. Thus, the use of polytetra-
F 1 IO
fluoroethylene (PTFE) or polyethylene vessels has
Cl IO 100
proved to be satisfactory for the storage of fluoride
and chloride Standard solutions. Experience indi- 1 IO
NO2
cates that nitrate Standard salutions are more stable
1 10
PO4
in borosilicate bottles.
Br 1 IO
IO 100
To avoid Cross contamination, always use the Same NO3
vessels for the Same anions and concentrations. 10 100
SO4
4.12.2 Mixed Standard Solution 1.
Pipette IO ml of the mixed Standard Solution I
(4.12.2) into a graduated flask of nominal capacity
The mass concentrations of this Solution are as fol-
100 ml, and dilute to volume with water.
lows:
p (F, NO,, PO,, Br) - IO mg/l
Store the Solution in a polyethylene vessel. The sol-
ution is stable for only 1 d to 2 d, even if stored at
p (Cl, NO,, SO,) = 100 mg/l
4 “C to 6 “C.
Pipette the volumes given in table 3 into a graduated
flask of nominal capacity
...
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