Soil quality - Determination of mercury in aqua regia soil extracts with cold-vapour atomic absorption spectrometry or cold-vapour atomic fluorescence spectrometry

ISO 16772:2004 specifies a method for the determination of mercury in an aqua regia extract of soil, obtained in accordance with ISO 11464 and ISO 11466, using cold-vapour atomic absorption spectrometry or cold-vapour atomic fluorescence spectrometry. The limit of determination of the method is at least 0,1 mg/kg.

Qualité du sol - Dosage du mercure dans les extraits de sol à l'eau régale par spectrométrie d'absorption atomique de vapeur froide ou par spectrométrie de fluorescence atomique de vapeur froide

L'ISO 16772:2004 spécifie une méthode de dosage du mercure dans un extrait de sol à l'eau régale, obtenu conformément à l'ISO 11464 et à l'ISO 11466, par spectrométrie d'absorption atomique ou spectrométrie de fluorescence atomique de vapeur froide. La limite de dosage est au moins de 0,1 mg/kg.

Kakovost tal - Določevanje živega srebra po razklopu v zlatotopki z atomsko absorpcijsko spektrometrijo s tehniko hladnih par (CV-AAS) ali atomsko fluorescentno spektrometrijo s tehniko hladnih par (CV-AFS)

Ta mednarodni standard določa metodo za določevanje živega srebra po razklopu v zlatotopki pri ekstraktih tal, pridobljenih v skladu s standardoma ISO 11464 in ISO 11466, z atomsko absorpcijsko spektrometrijo s tehniko hladnih par ali atomsko fluorescenčno spektrometrijo s tehniko hladnih par. Meja določevanja metode je vsaj 0,1 mg/kg.

General Information

Status
Published
Public Enquiry End Date
03-Jun-2019
Publication Date
04-Sep-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
30-Aug-2019
Due Date
04-Nov-2019
Completion Date
05-Sep-2019

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INTERNATIONAL ISO
STANDARD 16772
First edition
2004-06-01
Soil quality — Determination of mercury
in aqua regia soil extracts with cold-
vapour atomic spectrometry or cold-
vapour atomic fluorescence spectrometry
Qualité du sol — Dosage du mercure dans les extraits de sol à l'eau
régale par spectrométrie d'absorption atomique de vapeur froide ou par
spectrométrie de fluorescence atomique de vapeur froide
Reference number
ISO 16772:2004(E)
ISO 2004
---------------------- Page: 1 ----------------------
ISO 16772:2004(E)
PDF disclaimer

This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but

shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In

downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat

accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.

Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation

parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In

the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.

© ISO 2004

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 either ISO at the address below or

ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2004 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 16772:2004(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. 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.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 16772 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical

methods and soil characteristics.
© ISO 2004 – All rights reserved iii
---------------------- Page: 3 ----------------------
INTERNATIONAL STANDARD ISO 16772:2004(E)
Soil quality — Determination of mercury in aqua regia soil
extracts with cold-vapour atomic spectrometry or cold-vapour
atomic fluorescence spectrometry

WARNING — Mercury is highly toxic. Safety measures shall be taken in handling mercury and

mercury solutions. Mercury compounds should not be introduced into the environment. The

laboratory handling these compounds should be aware of the relevant international and national

legislation regulating the handling of mercury and its compounds.
1 Scope

This International Standard specifies a method for the determination of mercury in an aqua regia extract of soil,

obtained in accordance with ISO 11464 and ISO 11466, using cold-vapour atomic absorption spectrometry or

cold-vapour atomic fluorescence spectrometry. The limit of determination of the method is at least 0,1 mg/kg.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated

references, only the edition cited applies. For undated references, the latest edition of the referenced

document (including any amendments) applies.

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

ISO 11464:1994, Soil quality — Pretreatment of samples for physico-chemical analysis

ISO 11465:1993, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric

method

ISO 11466:1995, Soil quality — Extraction of trace elements soluble in aqua regia

3 Principle

Mercury is reduced to the elemental state by tin(II) chloride solution and liberated from solution in a closed

system. The mercury vapour passes through a cell positioned in the light path of an atomic absorption

spectrometer. Its absorbance at a wavelength of 253,7 nm is measured.
The absorbance signal is a function of mercury concentration.

Alternatively, after the reduction step, the mercury vapour is injected into the cell of an atomic fluorescence

spectrometer, where the mercury atoms are excited by radiation of a specific wavelength. The intensity of the

fluorescence radiation is a function of mercury concentration.

NOTE Tin(II) chloride as a reduction substance is specified in this International Standard because sodium

borohydride reduces many elements common in soil extract solutions to the elemental state, which cause matrix problems

under particular circumstances.
© ISO 2004 – All rights reserved 1
---------------------- Page: 4 ----------------------
ISO 16772:2004(E)
4 Reagents and gases

All reagents shall be of recognized analytical grade. Use deionized water or water distilled from an all-glass

apparatus, complying with grade 2 as defined in ISO 3696. The water used for blank determinations, and for

preparing reagents and standard solutions shall have a mercury concentration that is negligible compared with

the lowest calibration concentration, e.g. 10 times of the determination limit of the method.

4.1 Hydrochloric acid, w(HCl) = 37 %; c(HCl) ≈ 12 mol/l, ρ (HCl) ≈ 1,18 g/ml.
The same batch of hydrochloric acid should be used throughout the procedure.
4.2 Nitric acid, w(HNO ) = 65 %, c(HNO ) ≈ 14,5 mol/l, ρ (HNO ) ≈ 1,40 g/ml.
3 3
The same batch of nitric acid should be used throughout the procedure.

When different batches of acids are used throughout the procedure, the blank shall be controlled for each

batch.
4.3 Nitric acid, diluted solution (1+4), c(HNO ) ≈ 4 mol/l.

Add slowly 250 ml of nitric acid (4.2) to 500 ml of water in a 1000 ml volumetric flask, mix and fill to the mark

with water.
4.4 Aqua regia, diluted solution (1+9).

Add 21 ml hydrochloric acid (4.1) and 7 ml nitric acid (4.2) to 500 ml of water in a 1000 ml volumetric flask,

mix and fill to the mark with water.
4.5 Tin(II) chloride solution, ρ (SnCl ‚ 2H O) = 100 g/l, c(Sn) = 0,443 mol/l.
2 2

Dissolve 10 g of SnCl ‚ 2H O in 30 ml of hydrochloric acid (4.1), transfer to a 100 ml volumetric flask and fill

2 2

to the mark with water. The blank concentration of mercury can be reduced by bubbling a stream of nitrogen

through the solution for 30 min, if necessary. Prepare this solution on the day of use.

NOTE Other concentrations of tin(II) chloride may be necessary using other systems.

4.6 Mercury, stock solution corresponding to ρ (Hg) = 1000 mg/l.
4.6.1 General
Two sources of stock solutions can be used:
 commercially available stock solutions (4.6.2);
 stock solutions prepared in the laboratory from elemental mercury (4.6.3).
4.6.2 Commercially available stock solutions
Certified commercial stock solutions should preferably be used.

Commercial as well as home-made stock solutions should be checked on a regular basis.

NOTE Commercially available stock solutions have the advantage that they limit the need to handle toxic mercury.

However, special care needs to be taken that these solutions are supplied with a certified composition from a reputable

source.
2 © ISO 2004 – All rights reserved
---------------------- Page: 5 ----------------------
ISO 16772:2004(E)
4.6.3 Stock solutions prepared in the laboratory from elemental mercury

In a beaker covered with a watch glass, dissolve 100 mg ± 0,4 mg of mercury metal [minimum purity

w(Hg) = 99,99 %] with 17 ml nitric acid (4.2). Dilute with water, boil gently to expel nitrous oxides, cool and

transfer quantitatively into a 100 ml volumetric flask and fill to the mark with water. This solution is stable for at

least six months.
4.7 Mercury, standard solution corresponding to ρ (Hg) = 20 mg/l.

Pipette 2 ml of the stock mercury solution (4.6) into a 100 ml volumetric flask, add 10 ml nitric acid (4.3), mix

and fill to the mark with water.
4.8 Mercury, standard solution corresponding to ρ (Hg) = 0,2 mg/l.

Pipette 1 ml of the standard mercury solution (4.7) into a 100 ml volumetric flask, add 10 ml of nitric acid (4.3),

mix and fill to the mark with water. Prepare this solution on the day of use.

Low-level mercury standard solutions should be stored in suitable silica flasks or use PFA or FEP bottles as

mercury vapour diffuses through low density polyethene bottles.
4.9 Argon or nitrogen.

Argon or nitrogen with a purity of 99,99% should be used as carrier gases. For atomic fluorescence

spectrometric techniques, argon is strongly recommended because the sensitivity is higher than with nitrogen.

5 Apparatus
5.1 Usual laboratory glassware.

All glassware or PFA, FEP bottles shall be carefully cleaned for determinations involving trace elements,

e.g. by immersion in aqueous nitric acid solution of 5 % volume fraction for a minimum of 6 h, followed by

rinsing with water before use. The nitric acid shall be replaced each week. Grade B volumetric glassware is

adequate for this analysis (see ISO 648 and ISO 1042).

5.2 Atomic absorption spectrometer (AAS), equipped with a mercury hollow cathode or an electrodeless

discharge lamp (which gives a greater light intensity) operated at a current recommended by the lamp and

instrument manufacturer, and an automatic background correction device.

5.3 Atomic fluorescence spectrometer (AFS), equipped with a specific mercury lamp, a fixed 254 nm

filter and a photomultiplier tube for the detection of fluorescence radiation.

Operate at a current recommended by the lamp and instrument manufacturer (see also EN 13506).

5.4 Cold-vapour generator, batch system or an automated flow injection analysis system (FIAS),

adaptable either to the atomic absorption spectrometer (5.2) or to the atomic fluorescence spectrometer (5.3),

according to the detection technique used for the determination of mercury
...

SLOVENSKI STANDARD
SIST ISO 16772:2019
01-oktober-2019
Kakovost tal - Določevanje živega srebra po razklopu v zlatotopki z atomsko
absorpcijsko spektrometrijo s tehniko hladnih par (CV-AAS) ali atomsko
fluorescentno spektrometrijo s tehniko hladnih par (CV-AFS)

Soil quality - Determination of mercury in aqua regia soil extracts with cold-vapour atomic

absorption spectrometry or cold-vapour atomic fluorescence spectrometry
Qualité du sol - Dosage du mercure dans les extraits de sol à l'eau régale par
spectrométrie d'absorption atomique de vapeur froide ou par spectrométrie de
fluorescence atomique de vapeur froide
Ta slovenski standard je istoveten z: ISO 16772:2004
ICS:
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST ISO 16772:2019 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST ISO 16772:2019
---------------------- Page: 2 ----------------------
SIST ISO 16772:2019
INTERNATIONAL ISO
STANDARD 16772
First edition
2004-06-01
Soil quality — Determination of mercury
in aqua regia soil extracts with cold-
vapour atomic spectrometry or cold-
vapour atomic fluorescence spectrometry
Qualité du sol — Dosage du mercure dans les extraits de sol à l'eau
régale par spectrométrie d'absorption atomique de vapeur froide ou par
spectrométrie de fluorescence atomique de vapeur froide
Reference number
ISO 16772:2004(E)
ISO 2004
---------------------- Page: 3 ----------------------
SIST ISO 16772:2019
ISO 16772:2004(E)
PDF disclaimer

This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but

shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In

downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat

accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.

Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation

parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In

the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.

© ISO 2004

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 either ISO at the address below or

ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2004 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 16772:2019
ISO 16772:2004(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. 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.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 16772 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical

methods and soil characteristics.
© ISO 2004 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 16772:2019
---------------------- Page: 6 ----------------------
SIST ISO 16772:2019
INTERNATIONAL STANDARD ISO 16772:2004(E)
Soil quality — Determination of mercury in aqua regia soil
extracts with cold-vapour atomic spectrometry or cold-vapour
atomic fluorescence spectrometry

WARNING — Mercury is highly toxic. Safety measures shall be taken in handling mercury and

mercury solutions. Mercury compounds should not be introduced into the environment. The

laboratory handling these compounds should be aware of the relevant international and national

legislation regulating the handling of mercury and its compounds.
1 Scope

This International Standard specifies a method for the determination of mercury in an aqua regia extract of soil,

obtained in accordance with ISO 11464 and ISO 11466, using cold-vapour atomic absorption spectrometry or

cold-vapour atomic fluorescence spectrometry. The limit of determination of the method is at least 0,1 mg/kg.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated

references, only the edition cited applies. For undated references, the latest edition of the referenced

document (including any amendments) applies.

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

ISO 11464:1994, Soil quality — Pretreatment of samples for physico-chemical analysis

ISO 11465:1993, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric

method

ISO 11466:1995, Soil quality — Extraction of trace elements soluble in aqua regia

3 Principle

Mercury is reduced to the elemental state by tin(II) chloride solution and liberated from solution in a closed

system. The mercury vapour passes through a cell positioned in the light path of an atomic absorption

spectrometer. Its absorbance at a wavelength of 253,7 nm is measured.
The absorbance signal is a function of mercury concentration.

Alternatively, after the reduction step, the mercury vapour is injected into the cell of an atomic fluorescence

spectrometer, where the mercury atoms are excited by radiation of a specific wavelength. The intensity of the

fluorescence radiation is a function of mercury concentration.

NOTE Tin(II) chloride as a reduction substance is specified in this International Standard because sodium

borohydride reduces many elements common in soil extract solutions to the elemental state, which cause matrix problems

under particular circumstances.
© ISO 2004 – All rights reserved 1
---------------------- Page: 7 ----------------------
SIST ISO 16772:2019
ISO 16772:2004(E)
4 Reagents and gases

All reagents shall be of recognized analytical grade. Use deionized water or water distilled from an all-glass

apparatus, complying with grade 2 as defined in ISO 3696. The water used for blank determinations, and for

preparing reagents and standard solutions shall have a mercury concentration that is negligible compared with

the lowest calibration concentration, e.g. 10 times of the determination limit of the method.

4.1 Hydrochloric acid, w(HCl) = 37 %; c(HCl) ≈ 12 mol/l, ρ (HCl) ≈ 1,18 g/ml.
The same batch of hydrochloric acid should be used throughout the procedure.
4.2 Nitric acid, w(HNO ) = 65 %, c(HNO ) ≈ 14,5 mol/l, ρ (HNO ) ≈ 1,40 g/ml.
3 3
The same batch of nitric acid should be used throughout the procedure.

When different batches of acids are used throughout the procedure, the blank shall be controlled for each

batch.
4.3 Nitric acid, diluted solution (1+4), c(HNO ) ≈ 4 mol/l.

Add slowly 250 ml of nitric acid (4.2) to 500 ml of water in a 1000 ml volumetric flask, mix and fill to the mark

with water.
4.4 Aqua regia, diluted solution (1+9).

Add 21 ml hydrochloric acid (4.1) and 7 ml nitric acid (4.2) to 500 ml of water in a 1000 ml volumetric flask,

mix and fill to the mark with water.
4.5 Tin(II) chloride solution, ρ (SnCl ‚ 2H O) = 100 g/l, c(Sn) = 0,443 mol/l.
2 2

Dissolve 10 g of SnCl ‚ 2H O in 30 ml of hydrochloric acid (4.1), transfer to a 100 ml volumetric flask and fill

2 2

to the mark with water. The blank concentration of mercury can be reduced by bubbling a stream of nitrogen

through the solution for 30 min, if necessary. Prepare this solution on the day of use.

NOTE Other concentrations of tin(II) chloride may be necessary using other systems.

4.6 Mercury, stock solution corresponding to ρ (Hg) = 1000 mg/l.
4.6.1 General
Two sources of stock solutions can be used:
 commercially available stock solutions (4.6.2);
 stock solutions prepared in the laboratory from elemental mercury (4.6.3).
4.6.2 Commercially available stock solutions
Certified commercial stock solutions should preferably be used.

Commercial as well as home-made stock solutions should be checked on a regular basis.

NOTE Commercially available stock solutions have the advantage that they limit the need to handle toxic mercury.

However, special care needs to be taken that these solutions are supplied with a certified composition from a reputable

source.
2 © ISO 2004 – All rights reserved
---------------------- Page: 8 ----------------------
SIST ISO 16772:2019
ISO 16772:2004(E)
4.6.3 Stock solutions prepared in the laboratory from elemental mercury

In a beaker covered with a watch glass, dissolve 100 mg ± 0,4 mg of mercury metal [minimum purity

w(Hg) = 99,99 %] with 17 ml nitric acid (4.2). Dilute with water, boil gently to expel nitrous oxides, cool and

transfer quantitatively into a 100 ml volumetric flask and fill to the mark with water. This solution is stable for at

least six months.
4.7 Mercury, standard solution corresponding to ρ (Hg) = 20 mg/l.

Pipette 2 ml of the stock mercury solution (4.6) into a 100 ml volumetric flask, add 10 ml nitric acid (4.3), mix

and fill to the mark with water.
4.8 Mercury, standard solution corresponding to ρ (Hg) = 0,2 mg/l.

Pipette 1 ml of the standard mercury solution (4.7) into a 100 ml volumetric flask, add 10 ml of nitric acid (4.3),

mix and fill to the mark with water. Prepare this solution on the day of use.

Low-level mercury standard solutions should be stored in suitable silica flasks or use PFA or FEP bottles as

mercury vapour diffuses through low density polyethene bottles.
4.9 Argon or nitrogen.

Argon or nitrogen with a purity of 99,99% should be used as carrier gases. For atomic fluorescence

spectrometric techniques, argon is strongly recommended because the sensitivity is higher than with nitrogen.

5 Apparatus
5.1 Usual laboratory glassware.

All glassware or PFA, FEP bottles shall be carefully cleaned for determinations involving trace elements,

e.g. by immersion in aqueous nitric acid solution of 5 % volume fraction for a minimum of 6 h, followed by

rinsing with water before use. The nitric acid shall be replaced each week. Grade B volumetric glassware is

adequate for this analysis (see ISO 648 and ISO 1042).

5.2 Atomic absorption spectrometer (AAS), equipped with a mercury hollow cathode or an electrodeless

discharge lamp (which gives a greater light intensity) o
...

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.RPVNRQualité du sol - Dosage du mercure dans les extraits de sol à l'eau régale par spectrométrie d'absorption atomique de vapeur froide ou par spectrométrie de fluorescence atomique de vapeur froideSoil quality - Determination of mercury in aqua regia soil extracts with cold-vapour atomic absorption spectrometry or cold-vapour atomic fluorescence spectrometry71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis13.080.10Chemical characteristics of soilsICS:Ta slovenski standard je istoveten z:ISO 16772:2004oSIST ISO 16772:2019en01-maj-2019oSIST ISO 16772:2019SLOVENSKI

STANDARD
oSIST ISO 16772:2019
Reference numberISO 16772:2004(E)© ISO 2004

INTERNATIONAL STANDARD ISO16772First edition2004-06-01Soil quality — Determination of mercury in aqua regia soil extracts with cold-vapour atomic spectrometry or cold-vapour atomic fluorescence spectrometryQualité du sol — Dosage du mercure dans les extraits de sol à l'eau régale par spectrométrie d'absorption atomique de vapeur froide ou par spectrométrie de fluorescence atomique de vapeur froide

oSIST ISO 16772:2019

ISO 16772:2004(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.

ISO 2004 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 either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel.

+ 41 22 749 01 11 Fax
+ 41 22 749 09 47 E-mail
copyright@iso.org Web
www.iso.org Published in Switzerland
ii © ISO 2004 – All rights reserved
oSIST ISO 16772:2019

ISO 16772:2004(E) © ISO 2004 – All rights reserved iii 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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. 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. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 16772 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics.

oSIST ISO 16772:2019
oSIST ISO 16772:2019

INTERNATIONAL STANDARD ISO 16772:2004(E) © ISO 2004 – All rights reserved 1 Soil quality — Determination of mercury in aqua regia soil extracts with cold-vapour atomic spectrometry or cold-vapour atomic fluorescence spectrometry WARNING — Mercury is highly toxic. Safety measures shall be taken in handling mercury and mercury solutions. Mercury compounds should not be introduced into the environment. The laboratory handling these compounds should be aware of the relevant international and national legislation regulating the handling of mercury and its compounds. 1 Scope This International Standard specifies a method for the determination of mercury in an aqua regia extract of soil, obtained in accordance with ISO 11464 and ISO 11466, using cold-vapour atomic absorption spectrometry or cold-vapour atomic fluorescence spectrometry. The limit of determination of the method is at least 0,1 mg/kg. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use — Specification and test methods ISO 11464:1994, Soil quality — Pretreatment of samples for physico-chemical analysis ISO 11465:1993, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric method ISO 11466:1995, Soil quality — Extraction of trace elements soluble in aqua regia 3 Principle Mercury is reduced to the elemental state by tin(II) chloride solution and liberated from solution in a closed system. The mercury vapour passes through a cell positioned in the light path of an atomic absorption spectrometer. Its absorbance at a wavelength of 253,7 nm is measured. The absorbance signal is a function of mercury concentration. Alternatively, after the reduction step, the mercury vapour is injected into the cell of an atomic fluorescence spectrometer, where the mercury atoms are excited by radiation of a specific wavelength. The intensity of the fluorescence radiation is a function of mercury concentration. NOTE Tin(II) chloride as a reduction substance is specified in this International Standard because sodium borohydride reduces many elements common in soil extract solutions to the elemental state, which cause matrix problems under particular circumstances. oSIST ISO 16772:2019

ISO 16772:2004(E) 2 © ISO 2004 – All rights reserved 4 Reagents and gases All reagents shall be of recognized analytical grade. Use deionized water or water distilled from an all-glass apparatus, complying with grade 2 as defined in ISO 3696. The water used for blank determinations, and for preparing reagents and standard solutions shall have a mercury concentration that is negligible compared with the lowest calibration concentration, e.g. 10 times of the determination limit of the method. 4.1 Hydrochloric acid, w(HCl) = 37 %; c(HCl) ≈ 12 mol/l, ρ (HCl) ≈ 1,18 g/ml. The same batch of hydrochloric acid should be used throughout the procedure. 4.2 Nitric acid, w(HNO3) = 65 %, c(HNO3) ≈ 14,5 mol/l, ρ (HNO3) ≈ 1,40 g/ml. The same batch of nitric acid should be used throughout the procedure. When different batches of acids are used throughout the procedure, the blank shall be controlled for each batch. 4.3 Nitric acid, diluted solution (1+4), c(HNO3) ≈ 4 mol/l. Add slowly 250 ml of nitric acid (4.2) to 500 ml of water in a 1000 ml volumetric flask, mix and fill to the mark with water. 4.4 Aqua regia, diluted solution (1+9). Add 21 ml hydrochloric acid (4.1) and 7 ml nitric acid (4.2) to 500 ml of water in a 1000 ml volumetric flask, mix and fill to the mark with water. 4.5 Tin(II) chloride solution, ρ (SnCl2 ‚ 2H2O) = 100 g/l, c(Sn) = 0,443 mol/l. Dissolve 10 g of SnCl2 ‚ 2H2O in 30 ml of hydrochloric acid (4.1), transfer to a 100 ml volumetric flask and fill to the mark with water. The blank concentration of mercury can be reduced by bubbling a stream of nitrogen through the solution for 30 min, if necessary. Prepare this solution on the day of use. NOTE Other concentrations of tin(II) chloride may be necessary using other systems. 4.6 Mercury, stock solution corresponding to ρ (Hg) = 1000 mg/l. 4.6.1 General Two sources of stock solutions can be used: =commercially available stock solutions (4.6.2); =stock solutions prepared in the laboratory from elemental mercury (4.6.3). 4.6.2 Commercially available stock solutions Certified commercial stock solutions should preferably be used. Commercial as well as home-made stock solutions should be checked on a regular basis. NOTE Commercially available stock solutions have the advantage that they limit the need to handle toxic mercury. However, special care needs to be taken that these solutions are supplied with a certified composition from a reputable source. oSIST ISO 16772:2019

ISO 16772:2004(E) © ISO 2004 – All rights reserved 3 4.6.3 Stock solutions prepared in the laboratory from elemental mercury In a beaker covered with a watch glass, dissolve 100 mg ± 0,4 mg of mercury metal [minimum purity w(Hg) = 99,99 %] with 17 ml nitric acid (4.2). Dilute with water, boil gently to expel nitrous oxides, cool and transfer quantitatively into a 100 ml volumetric flask and fill to the mark with water. This solution is stable for at least six months. 4.7 Mercury, standard solution corresponding to ρ (Hg) = 20 mg/l. Pipette 2 ml of the stock mercury solution (4.6) into a 100 ml volumetric flask, add 10 ml nitric acid (4.3), mix and fill to the mark with water. 4.8 Mercury, standard solution corresponding to ρ (Hg) = 0,2 mg/l. Pipette 1 ml of the standard mercury solution (4.7) into a 100 ml volumetric flask, add 10 ml of nitric acid (4.3), mix and fill to the mark with water. Prepare this solution on the day of use. Low-level mercury standard solutions should be stored in suitable silica flasks or use PFA or FEP bottles as mercury vapour diffuses through low density polyethene bottles. 4.9 Argon or nitrogen. Argon or nitrogen with a purity of 99,99% should be used as carrier gases. For atomic fluorescence spectrometric techniques, argon is strongly recommended because the sensitivity is higher than with nitrogen. 5 Apparatus 5.1 Usual laboratory glassware. All glassware or PFA, FEP bottles shall be carefully cleaned for determinations involving trace elements, e.g. by immersion in aqueous nitric acid solution of 5 % volume fraction for a minimum of 6 h, followed by rinsing with water before use. The nitric acid shall be replaced each week. Grade B volumetric glassware is adequate for this analysis (see ISO 648 and ISO 1042). 5.2 Atomic absorption spectrometer (AAS), equipped with a mercury hollow cathode or an electrodeless discharge lamp (which gives a greater light intensity) operated at a current recommended by the lamp and instrument manufacturer, and an automatic background correction device. 5.3 Atomic fluorescence spectromete

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NORME ISO
INTERNATIONALE 16772
Première édition
2004-06-01
Qualité du sol — Dosage du mercure
dans les extraits de sol à l'eau régale par
spectrométrie d'absorption atomique de
vapeur froide ou par spectrométrie de
fluorescence atomique de vapeur froide
Soil quality — Determination of mercury in aqua regia soil extracts with
cold-vapour atomic spectrometry or cold-vapour atomic fluorescence
spectrometry
Numéro de référence
ISO 16772:2004(F)
ISO 2004
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ISO 16772:2004(F)
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© ISO 2004

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ii © ISO 2004 – Tous droits réservés
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ISO 16772:2004(F)
Avant-propos

L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes nationaux de

normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est en général confiée

aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude a le droit de faire partie du

comité technique créé à cet effet. Les organisations internationales, gouvernementales et non

gouvernementales, en liaison avec l'ISO participent également aux travaux. L'ISO collabore étroitement avec

la Commission électrotechnique internationale (CEI) en ce qui concerne la normalisation électrotechnique.

Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI,

Partie 2.

La tâche principale des comités techniques est d'élaborer les Normes internationales. Les projets de Normes

internationales adoptés par les comités techniques sont soumis aux comités membres pour vote. Leur

publication comme Normes internationales requiert l'approbation de 75 % au moins des comités membres

votants.

L'attention est appelée sur le fait que certains des éléments du présent document peuvent faire l'objet de

droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable de ne

pas avoir identifié de tels droits de propriété et averti de leur existence.

L'ISO 16772 a été élaborée par le comité technique ISO/TC 190, Qualité du sol, sous-comité SC 3, Méthodes

chimiques et caractéristiques du sol.
© ISO 2004 – Tous droits réservés iii
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NORME INTERNATIONALE ISO 16772:2004(F)
Qualité du sol — Dosage du mercure dans les extraits de sol à
l'eau régale par spectrométrie d'absorption atomique de vapeur
froide ou par spectrométrie de fluorescence atomique de
vapeur froide

AVERTISSEMENT — Le mercure est extrêmement toxique. Des mesures de sécurité doivent être

prises pour la manipulation du mercure et des solutions de mercure. Il convient de ne pas introduire

des composés du mercure dans l’environnement. Il convient que le laboratoire manipulant ces

composés connaisse la législation nationale et internationale régissant la manipulation du mercure et

de ses composés.
1 Domaine d'application

La présente Norme internationale spécifie une méthode de dosage du mercure dans un extrait de sol à l’eau

régale, obtenu conformément à l’ISO 11464 et à l’ISO 11466, par spectrométrie d’absorption atomique ou

spectrométrie de fluorescence atomique de vapeur froide. La limite de dosage est au moins de 0,1 mg/kg.

2 Références normatives

Les documents de référence suivants sont indispensables pour l'application du présent document. Pour les

références datées, seule l'édition citée s'applique. Pour les références non datées, la dernière édition du

document de référence s'applique (y compris les éventuels amendements).

ISO 3696:1987, Eau pour laboratoire à usage analytique — Spécification et méthodes d'essai

ISO 11464:1994, Qualité du sol — Prétraitement des échantillons pour analyses physico-chimiques

ISO 11465:1993, Qualité du sol — Détermination de la teneur pondérale en matière sèche et en eau —

Méthode gravimétrique

ISO 11466:1995, Qualité du sol — Extraction des éléments en traces solubles dans l'eau régale

3 Principe

Le mercure est réduit à l’état élémentaire par une solution de chlorure stanneux et libéré de la solution dans

un système fermé. La vapeur de mercure traverse une cuve placée dans le trajet optique d’un spectromètre

d’absorption atomique. On mesure son absorbance à une longueur d’onde de 253,7 nm.

Le signal d’absorbance est fonction de la concentration en mercure.

Ou bien, à l’issue de l’étape de réduction, la vapeur de mercure est injectée dans la cuve d’un spectromètre

de fluorescence atomique où les atomes de mercure sont excités par la radiation d’une longueur d’onde

donnée. L’intensité de la radiation de fluorescence est fonction de la concentration en mercure.

NOTE La substance de réduction spécifiée dans la présente Norme internationale est le chlorure stanneux, car le

borohydrure de sodium réduit de nombreux éléments que l’on trouve couramment dans les solutions d’extrait de sol à

l’état élémentaire, ce qui crée des problèmes de matrice dans certaines circonstances.

© ISO 2004 – Tous droits réservés 1
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ISO 16772:2004(F)
4 Réactifs et gaz

Tous les réactifs doivent être de qualité analytique reconnue. Utiliser de l’eau désionisée ou de l’eau distillée

provenant d’un appareillage entièrement en verre et conforme à la qualité 2 de l’ISO 3696. L’eau utilisée pour

les dosages à blanc et pour préparer les réactifs ainsi que les solutions étalons doit avoir une concentration

en mercure négligeable par rapport à la concentration minimale d’étalonnage, par exemple 10 fois la limite de

dosage de la méthode.
4.1 Acide chlorhydrique, w(HCl) = 37 %, c(HCl) ≈ 12 mol/l, ρ (HCl) ≈ 1,18 g/ml.

Il convient d’utiliser le même lot d’acide nitrique tout au long de la mise en œuvre du mode opératoire.

4.2 Acide nitrique, w(HNO ) = 65 %, c(HNO ) ≈ 14,5 mol/l, ρ (HNO ) ≈ 1,40 g/ml.
3 3 3

Il convient d’utiliser le même lot d’acide nitrique tout au long de la mise en œuvre du mode opératoire.

En cas d’utilisation de lots différents d’acides au cours de la mise en œuvre du mode opératoire, le blanc doit

être contrôlé pour chaque lot.
4.3 Solution d’acide nitrique diluée (1 + 4), c(HNO ) ≈ 4 mol/l.

Ajouter lentement 250 ml d’acide nitrique (4.2) à 500 ml d’eau dans une fiole jaugée de 1 000 ml, mélanger et

compléter au trait repère avec de l’eau.
4.4 Solution d’eau régale diluée (1 + 9).

Ajouter 21 ml d’acide chlorhydrique (4.1) et 7 ml d’acide nitrique (4.2) à 500 ml d’eau dans une fiole jaugée de

1 000 ml, mélanger et compléter au trait repère avec de l’eau.

4.5 Solution de chlorure stanneux, ρ (SnCl ◊ 2H O) = 100 g/l, c(Sn) = 0,443 mol/l.

2 2

Mettre en solution 10 g de SnCl ◊ 2H O dans 30 ml d’acide chlorhydrique (4.1), transvaser dans une fiole

2 2

jaugée de 100 ml et compléter au trait de jauge avec de l’eau. Si nécessaire, la concentration à blanc du

mercure peut être réduite en faisant passer un flux d’azote en fines bulles à travers la solution pendant 30 min.

Préparer cette solution le jour de son utilisation.

NOTE D’autres concentrations de chlorure stanneux peuvent être nécessaires en cas d’utilisation d’autres systèmes.

4.6 Solution mère de mercure, correspondant à ρ (Hg) = 1 000 mg/l.
4.6.1 Généralités
Deux sources de solutions mères peuvent être utilisées:
 les solutions mères disponibles dans le commerce (4.6.2);

 les solutions mères préparées dans le laboratoire à partir de mercure élémentaire (4.6.3).

4.6.2 Solutions mères disponibles dans le commerce

Il convient d’utiliser, de préférence, des solutions mères du commerce certifiées.

Il convient de contrôler régulièrement les solutions mères du commerce ainsi que celles produites en interne.

NOTE Les solutions mères disponibles dans le commerce présentent l’avantage de limiter la nécessité d’une

manipulation de mercure toxique. Cependant, veiller tout particulièrement à ce que ces solutions soient fournies avec une

composition certifiée par un fournisseur connu.
2 © ISO 2004 – Tous droits réservés
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ISO 16772:2004(F)
4.6.3 Solutions mères préparées au laboratoire à partir du mercure élémentaire

Dans un bécher recouvert d’un verre de montre, mettre en solution 100 mg ± 0,4 mg de mercure [pureté

minimale w(Hg) = 99,99 %] avec 17 ml d’acide nitrique (4.2). Diluer avec de l’eau, faire bouillir doucement afin

d’éliminer les oxydes nitreux, laisser refroidir puis transvaser quantitativement dans une fiole jaugée de

100 ml et compléter au trait repère avec de l’eau. Cette solution est stable pendant au moins six mois.

4.7 Solution étalon de mercure, correspondant à ρ (Hg) = 20 mg/l.

À l’aide d’une pipette, introduire 2 ml de la solution mère de mercure (4.6) dans une fiole jaugée de 100 ml,

ajouter 10 ml d’acide nitrique (4.3), mélanger et compléter au trait repère avec de l’eau.

4.8 Solution étalon de mercure, correspondant à ρ (Hg) = 0,2 mg/l.

À l’aide d’une pipette, introduire 1 ml de la solution étalon de mercure (4.7) dans une fiole jaugée de 100 ml,

ajouter 10 ml d’acide nitrique (4.3), mélanger et compléter au trait repère avec de l’eau. Préparer cette

solution le jour de son utilisation.

Il convient de conserver les solutions étalons à faible teneur en mercure dans des fioles appropriées en silice

ou d’utiliser des flacons en PFA ou en FEP, car les vapeurs de mercure se diffusent à travers les flacons en

polyéthylène basse densité.
4.9 Argon ou azote.

Il convient d’utiliser de l’argon ou de l’azote d’une pureté de 99,99 % comme gaz vecteur. L’argon est

vivement recommandé pour la spectrométrie de fluorescence atomique, car sa sensibilité est supérieure à

celle de l’azote.
5 Appareillage
5.1 Verrerie courante de laboratoire.

Toute la verrerie ou les flacons en PFA ou en FEP doivent être soigneusement nettoyés pour les dosages des

éléments en faibles traces, par exemple en les immergeant dans une solution aqueuse d’acide nitrique à 5 %

(fraction volumique) pendant au moins 6 h, puis en les rinçant à l’eau avant utilisation. L’acide nitrique doit

être renouvelé toutes les semaines. Une verrerie jaugée de qualité B convient pour cette analyse (voir

l’ISO 648 et l’ISO 1042).

5.2 Spectromètre d’absorption atomique (SAA), celui-ci est équipé d’une lampe à cathode creuse au

mercure ou d’une lampe à décharge sans électrode (qui fournit une intensité lumineuse plus grande),

fonctionnant avec le courant recommandé par le fabricant de la lampe et de l’instrument, et d’un dispositif de

correction du fond automatique.

5.3 Spectromètre de fluorescence atomique (SFA), celui-ci est équipé d’une lampe spécifique à mercure,

d’un filtre fixe de 254 nm et d’un tube photomultiplicateur pour la détection de la radiation de fluorescence. Le

faire fonctionner avec le courant recommandé par le fabricant de la lampe et de l’instrument (voir également

...

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