ISO/FDIS 13546

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 13546
ISO/TC 183
Copper concentrates —
Secretariat: SA
Determination of mercury content
Voting begins on:
2021­04­26 — Cold vapour atomic absorption
spectrometric method
Voting terminates on:
2021­06­21
RECIPIENTS OF THIS DRAFT ARE INVITED TO
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO­
ISO/FDIS 13546:2021(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN­
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO 2021
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ISO/FDIS 13546:2021(E)
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© ISO 2021

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Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus ..................................................................................................................................................................................................................... 3

7 Sampling and sampling preparation ............................................................................................................................................... 4

7.1 Test sample ................................................................................................................................................................................................. 4

7.2 Test portion ................................................................................................................................................................................................ 4

8 Procedure..................................................................................................................................................................................................................... 4

8.1 Number of determinations ........................................................................................................................................................... 4

8.2 Blank test ..................................................................................................................................................................................................... 4

8.3 Dissolution of the test portion ................................................................................................................................................... 4

8.4 Storage of digested solutions ...................................................................................................................................................... 5

8.5 Preparation of sample solutions .............................................................................................................................................. 5

8.6 Preparation of test solutions ....................................................................................................................................................... 5

8.7 Preparation of calibration solutions ..................................................................................................................................... 5

8.8 Preparation of mercury calibration graph ...................................................................................................................... 5

8.9 Determination of mercury content in test solutions .............................................................................................. 6

9 Expression of results ........................................................................................................................................................................................ 6

10 Procedure for obtaining the final result ...................................................................................................................................... 6

11 Precision ....................................................................................................................................................................................................................... 6

11.1 Expression of precision ................................................................................................................................................................... 6

11.2 Procedure for obtaining the final result ............................................................................................................................ 7

11.3 Precision between laboratories ................................................................................................................................................ 7

11.4 Check of trueness .................................................................................................................................................................................. 8

11.4.1 General...................................................................................................................................................................................... 8

11.4.2 Type of certified reference material or reference material......................................................... 8

programme ........................................................................................................................................................................... 8

11.4.4 Reference material certified or characterized by one laboratory ......................................... 9

12 Test report ................................................................................................................................................................................................................... 9

Annex A (normative) Procedure for obtaining the final results ...........................................................................................10

Bibliography .............................................................................................................................................................................................................................11

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This document was prepared by Technical Committee ISO/TC 183, Copper, lead, zinc and nickel ores and

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WARNING — The use of this document can involve hazardous materials, operations and

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This document specifies an acid digestion and vapour generation atomic absorption spectrometric

method for the determination of the mercury content in copper sulfide concentrate.

This document is applicable to mass fraction of mercury between 5 µg/g and 65 µg/g in copper sulfide

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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 4787, Laboratory glassware — Volumetric instruments — Methods for testing of capacity and for use

ISO 9599, Copper, lead, zinc and nickel sulfide concentrates — Determination of hygroscopic moisture

ISO 12743:2018, Copper, lead, zinc and nickel concentrates — Sampling procedures for determination of

ISO Guide 35, Reference materials — Guidance for characterization and assessment of homogeneity and

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

The test portion is decomposed by treatment with hydrochloric and nitric acid at a temperature

of between 60 °C and 80 °C followed by the addition of potassium permanganate as oxidizing agent.

Subsequently, the potassium permanganate is reduced by hydroxylamine hydrochloride. The mercury

vapour is generated by vapour generation using tin (II) chloride as reduction agent. The equipment is set

to measure the absorbance at 253,7 nm. The absorbances of the test and calibration solutions, including

those of certified or other reference materials, are compared to determine the mercury content.

During the analysis, use only reagents of recognized analytical grade and grade 2 water in accordance

5.10 Aqua regia. Mix 300 ml of hydrochloric acid (5.6) and 100 ml nitric acid (5.5). Prepare freshly for

5.11 Tin (II) chloride solution, 100 g/l. Add 10 g of tin (II) chloride (5.1) to 80 ml sulfuric acid solution

(5.9). Heat and swirl to dissolve. Cool the solution and dilute with deionized water to 100 ml and mix

Continuously stir the solution with a magnetic stirrer for at least 2 h before use and maintain stirring

Tin (II) chloride solution, 100 g/l: add 10 g of tin (II) chloride (5.1) to 20 ml of deionized water. Add

continuously 60 ml of sulfuric acid solution (5.8). Heat and swirl to dissolve. Cool, dilute to 100 ml with