ISO/TC 183 - Copper, lead, zinc and nickel ores and concentrates

This document specifies an acid digestion and vapour generation atomic absorption spectrometric method for the determination of the mercury content in copper sulfide concentrates. This document is applicable to mass fraction of mercury between 5 µg/g and 65 µg/g in copper sulfide concentrates.

This document sets out the basic methods for sampling copper, lead, zinc and nickel concentrates from moving streams and stationary lots, including stopped-belt sampling, to provide samples for chemical analysis, physical testing and determination of moisture content, in accordance with the relevant International Standards. Where the concentrates are susceptible to significant oxidation or decomposition, a common sample that is sufficiently representative, i.e. unbiased and sufficiently precise, is used for moisture determination and chemical analysis to eliminate bias (see ISO 10251). Any large agglomerates (>10 mm) present in the primary sample are crushed prior to further sample processing. Sampling of concentrates in slurry form is specifically excluded from this document. Stopped-belt sampling is the reference method for collecting concentrate samples against which mechanical and manual-sampling procedures can be compared. Sampling from moving streams is the preferred method. Both falling-stream and cross-belt samplers are described. Sampling from stationary lots is used only where sampling from moving streams is not possible. The procedures described in this document for sampling from stationary lots only minimize some of the systematic sampling errors.

This document specifies a flow-table method for the determination of the transportable moisture limit (TML) of copper, lead and zinc sulfide concentrates, which can liquefy during transport. It is applicable to the determination of the TML of concentrates containing 10 % to 80 % (mass fraction) of lead, 10 % to 65 % (mass fraction) of zinc or 10 % to 55 % (mass fraction) of copper and is applicable to TML values in the range 3 % to 28 % (mass fraction).

This document specifies an analytical method for the determination of total chlorine content using alkaline fusion and potentiometric titration. This method is applicable to copper and nickel sulfide ores and concentrates having chlorine content in the following ranges: a) Method 1: 80 µg/g to 4 300 µg/g b) Method 2: 70 µg/g to 4 300 µg/g

This document specifies an acid digestion and inductively coupled plasma atomic emission spectrometric (ICP-AES) method for the determination of the mass fraction of cadmium in copper, lead and zinc sulfide concentrates as follows: a) for copper sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,01 % to 0,30 %; b) for lead sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,01 % to 0,30 %; c) for zinc sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,05 % to 1,00 %.

This document specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of cadmium in copper, lead and zinc sulfide concentrates as follows: a) for copper sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,01 % to 0,30 %; b) for lead sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,01 % to 0,30 %; c) for zinc sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,05 % to 0,30 %.

ISO 10258:2018 specifies two titrimetric methods for the determination of the copper content of copper sulfide concentrates in the range 15 % (m/m) to 50 % (m/m), using sodium thiosulfate after separation (method 1) or without separation (method 2) of copper from interfering elements.

ISO 11794:2017 sets out the basic methods for sampling particulate material that is mixed with a liquid, usually water, to form a slurry. In industry and in the mining and mineral processing literature, slurry is also referred to as pulp, but this term is not used in ISO 11794:2017. At very high ratios of fine particulate solids to liquids where material assumes a soft plastic form, the mixture is correctly termed as a paste. Sampling of pastes is not covered in ISO 11794:2017. The procedures described in ISO 11794:2017 apply to sampling of particulate materials that are transported in moving streams as slurries, but not pressurized slurries. These streams may fall freely or be confined in pipes, launders, flumes, sluices, spirals or similar channels. Sampling of slurries in stationary situations, such as a settled or even a well-stirred slurry in a holding vessel or dam, is not recommended and is not covered in ISO 11794:2017. ISO 11794:2017 describes procedures that are designed to provide samples representative of the slurry solids and particle-size distribution of the slurry under examination. After draining the slurry sample of fluid and measuring the fluid volume, damp samples of the contained particulate material in the slurry are available for drying (if required) and measurement of one or more characteristics in an unbiased manner and with a known degree of precision. The characteristics are measured by chemical analysis, physical testing or both. The sampling methods described are applicable to slurries that require inspection to verify compliance with product specifications, determination of the value of a characteristic as a basis for settlement between trading partners or estimation of a set of average characteristics and variances that describes a system or procedure. Provided that flow rates are not too high, the reference method against which other sampling procedures are compared is one where the entire stream is diverted into a vessel for a specified time or volume interval. This method corresponds to the stopped-belt method described in ISO 12743.

ISO 11790:2017 sets out recommended practices for the inspection of mechanical sampling systems. It serves as a reference for conformance with applicable International Standards for copper, lead, zinc and nickel concentrates. ISO 11790:2017 covers general considerations, including precision, quality variation, bias, establishment of inspection systems and inspection procedures.

ISO 13543:2016 specifies the method for determining the mass of contained metal in a lot, based on the wet mass, moisture content and dry basis metal content of the lot. The procedure for estimating the variance and confidence intervals for the mass of contained metal is also specified.

ISO 10378:2016 specifies a fire assay gravimetric and flame atomic absorption spectrometric method for the determination of the mass fraction of gold and silver in copper, lead, and zinc sulfide concentrates as follows. - Copper concentrates The method is applicable to the determination of mass fractions of gold from 0,5 g/t to 300 g/t and of mass fractions of silver from 25 g/t to 1 500 g/t in copper sulfide concentrates containing mass fractions of copper from 15 % to 60 %. - Lead concentrates The method is applicable to the determination of mass fractions of gold from 0,1 g/t to 25 g/t and of mass fractions of silver from 200 g/t to 3 500 g/t in lead sulfide concentrates containing mass fractions of lead from 10 % to 80 %. - Zinc concentrates The method is applicable to the determination of mass fractions of gold from 0,1 g/t to 12 g/t and of mass fractions of silver from 10 g/t to 800 g/t in zinc sulfide concentrates containing mass fractions of zinc up to 60 %.

ISO 9599:2015 specifies a gravimetric loss-in-mass method for the determination of the hygroscopic moisture content in analysis samples of copper, lead, zinc, and nickel sulfide concentrates. The method is applicable to copper, lead, zinc, and nickel sulfide concentrates free from volatile organic flotation reagents, for example kerosene, and with hygroscopic moisture contents between 0,05 % (m/m) and 2 % (m/m). The hygroscopic moisture content is used to correct the analysis results from the equilibrated moisture level to the dry basis. NOTE The result of the determination of hygroscopic moisture content using this International Standard should not be reported as part of the analysis of a concentrate sample. Whenever the bulk moisture content of a commercial shipment of concentrate is required, ISO 10251 should be used. The determination of hygroscopic moisture content and the determination of bulk moisture content are connected with each other. In both determinations, the same state of dryness has to be achieved, in order to ascertain the correct metal content of a lot. This method is not applicable to sulfide concentrates that are susceptible to oxidation (see 6.3, note 2). Annex A sets out a modified procedure, which can be used for sulfide concentrates that are susceptible to oxidation.

ISO 15247:2015 specifies an acid dissolution and flame atomic absorption spectrometric method for the determination of silver content of zinc sulfide concentrates. The method is applicable to the determination of silver in zinc sulfide concentrates containing up to 60 % (m/m) zinc in the form of zinc blende and related materials. The method is applicable to silver contents from 10 g/t to 500 g/t.

ISO 13547-2:2014 specifies an acid digestion and inductively coupled plasma atomic emission spectrometric (ICP-AES) method for the determination of the mass fraction of arsenic in copper, lead, zinc, and nickel sulfide concentrates as follows: for copper sulfide concentrates, the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 2,0 %; for lead sulfide concentrates, the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 1,0 %; for zinc sulfide concentrates, the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 0,6 %; for nickel sulfide concentrates, the method is applicable to the determination of mass fraction of arsenic from 0,05 % to 1,0 %.

ISO 13547-1:2014 specifies an iron hydroxide concentration and inductively coupled plasma atomic emission spectrometric (ICP-AES) method for the determination of the mass fraction of arsenic in copper, lead, zinc, and nickel sulfide concentrates as follows: for copper sulfide concentrates, the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 2,0 %; for lead sulfide concentrates, the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 1,0 %; for zinc sulfide concentrates, the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 0,6 %; for nickel sulfide concentrates, the method is applicable to the determination of mass fraction of arsenic from 0,05 % to 1,0 %.

ISO 12745:2008 provides guidelines to test for bias over a wide range of mass measurement techniques, to estimate the precision for each technique and to calculate the precision for wet mass when estimated by applying one of those techniques. The guidelines are based on the application of statistical tests to verify that a mass measurement technique is unbiased, to estimate the variance as the most basic measure for its precision and to check the linearity of a static scale over its working range. Calibration methods and performance tests for compliance with applicable regulations generate test results that can be used to quantify precision and bias for each of these mass measurement techniques and to verify linearity for static weighing devices. The guidelines apply to mass measurement techniques used to estimate the wet mass for cargoes or shipments of mineral concentrate as the basis for freight and insurance charges and for preliminary payments or for final settlements between trading partners.

ISO 12739:2006 specifies an ion-exchange/EDTA titrimetric method for the determination of the mass fraction of zinc in zinc concentrates. The method is applicable to zinc sulfide concentrates having a mass fraction of zinc in the range from 11 % to 62 %.

ISO 10469:2006 specifies an electrogravimetric method for the determination of the mass fraction of copper in copper sulfide concentrates in the range 15 % to 50 %.

ISO 13291:2006 specifies a solvent extraction/titrimetric method for the determination of the mass fraction of zinc in zinc sulfide concentrates. The method is applicable to zinc sulfide concentrates having a mass fraction of zinc in the range from 11 % to 62 %.

ISO 10251:2006 specifies methods for the determination of moisture content of a lot of copper, lead, zinc or nickel concentrate, defined as the percentage mass loss of the moisture test portion under the conditions of drying specified in this document. ISO 10251:2006 is not applicable to drying samples used for determination of volatile elements such as mercury and sulfur.

ISO 12744:2006 specifies methods for checking the precision of primary sampling, sample processing, chemical analysis, physical testing and determination of moisture content of copper, lead, zinc and nickel concentrates being carried out in accordance with the methods specified in ISO 12743, expressed in terms of standard deviations.

ISO 13292:2006 specifies methods for checking whether there is any bias in the sampling of copper, lead, zinc and nickel concentrates, where the sampling is carried out in accordance with the methods specified in ISO 12743. These methods can also be used for comparing alternative sampling regimes, checking whether there is any bias in sample processing and for checking possible significant differences in sampling at different places, e.g. at loading and discharge points, or the analysis of exchange samples.

This Technical Report outlines simple procedures to check the performance and calibration status of static scales. The test sequence is intended for routine applications, generating results which can be used to calculate explicit scale performance parameters (precision, bias and linearity) in accordance with the relevant equations shown in ISO 12745, Copper, lead and zinc ores and concentrates — Precision and bias of mass measurement techniques. It is stressed that the basic procedures described below do not replace comprehensive technical manuals published by National Weights and Measures authorities to comply with legal and other specific requirements.

This International Standard specifies a hydroxide precipitation and EDTA titrimetric method for the determination of the zinc content of zinc ores and concentrates containing 10 % (m/m) to 60%(m/m) zinc.

This International Standard specifies a lead sulfate precipitation EDTA titrimetric method after acid decomposition for determination of the lead content of lead sulfide concentrates. The method is applicable to lead sulfide concentrates having lead content in the range 50 % (m/m) to 80%(m/m). The method is not applicable to lead concentrates containing more than 1 % (m/m) of barium.

This International Standard specifies a fire assay and flame atomic absorption spectrometric procedure for the determination of silver and gold contents of zinc sulfide concentrates. The method is applicable to the determination of silver and gold in zinc sulfide concentrates containing up to 60 % (m/m) zinc in the form of zinc blende and related materials. The method is applicable to silver contents from 10 g/t to 500 g/t and gold contents from 0,1 g/t to 12 g/t.

This International Standard specifies a fire assay and flame atomic absorption spectrometric procedure for the determination of silver and gold contents of lead sulfide concentrates. The method is applicable to the determination of silver and gold in lead sulfide concentrates containing 10 % (m/m) to 80 % (m/m) lead. The method is applicable to silver contents from 200 g/t to 2 000 g/t and gold contents from 0,1 g/t to 25 g/t.

Specifies a lead sulfate precipitation EDTA titrimetric method for the determination of lead content in lead sulfide concentrates. Applicable to all lead sulfide concentrates with lead content in the range from 10 % (m/m) to 80 % (m/m).

This document sets out the basic methods for sampling copper, lead, zinc and nickel concentrates from moving streams and stationary lots, including stopped-belt sampling, to provide samples for chemical analysis, physical testing and determination of moisture content, in accordance with the relevant International Standards. Where the concentrates are susceptible to significant oxidation or decomposition, a common sample that is sufficiently representative, i.e. unbiased and sufficiently precise, is used for moisture determination and chemical analysis to eliminate bias (see ISO 10251). Any large agglomerates (>10 mm) present in the primary sample are crushed prior to further sample processing. Sampling of concentrates in slurry form is specifically excluded from this document. Stopped-belt sampling is the reference method for collecting concentrate samples against which mechanical and manual-sampling procedures can be compared. Sampling from moving streams is the preferred method. Both falling-stream and cross-belt samplers are described. Sampling from stationary lots is used only where sampling from moving streams is not possible. The procedures described in this document, for sampling from stationary lots, only minimize some of the systematic sampling errors.

ISO 10258:2015 specifies two titrimetric methods for the determination of the copper content of copper sulfide concentrates in the range 15 % (m/m) to 50 % (m/m), using sodium thiosulfate after separation (method 1) or without separation (method 2) of copper from interfering elements.

ISO 11794:2010 sets out the basic methods for sampling particulate material that is mixed with a liquid, usually water, to form a slurry. In industry and in the mining and mineral processing literature, slurry is also referred to as pulp, but this term is not used in ISO 11794:2010. At very high ratios of fine particulate solids to liquids where material assumes a soft plastic form, the mixture is correctly termed as a paste. Sampling of pastes is not covered in ISO 11794:2010. The procedures described in ISO 11794:2010 apply to sampling of particulate materials that are transported in moving streams as slurries, but not pressurized slurries. These streams may fall freely or be confined in pipes, launders, flumes, sluices, spirals or similar channels. Sampling of slurries in stationary situations, such as a settled or even a well-stirred slurry in a holding vessel or dam, is not recommended and is not covered in ISO 11794:2010. ISO 11794:2010 describes procedures that are designed to provide samples representative of the slurry solids and particle-size distribution of the slurry under examination. After draining the slurry sample of fluid and measuring the fluid volume, damp samples of the contained particulate material in the slurry are available for drying (if required) and measurement of one or more characteristics in an unbiased manner and with a known degree of precision. The characteristics are measured by chemical analysis, physical testing or both. The sampling methods described are applicable to slurries that require inspection to verify compliance with product specifications, determination of the value of a characteristic as a basis for settlement between trading partners or estimation of a set of average characteristics and variances that describes a system or procedure.

ISO 11790:2010 sets out recommended practices for the inspection of mechanical sampling systems. It serves as a reference for conformance with applicable International Standards for copper, lead, zinc and nickel concentrates. ISO 11790:2010 covers general considerations, including precision, quality variation, bias, establishment of inspection systems and inspection procedures.

ISO 12742:2007 specifies a flow-table method for the determination of the transportable moisture limit (TML) of copper, lead and zinc sulfide concentrates, which may liquefy during transport. ISO 12742:2007 is applicable to the determination of the TML of concentrates containing 10 % to 80 % (mass fraction) of lead, or 10 % to 65 % (mass fraction) of zinc, or 10 % to 55 % (mass fraction) of copper. It is applicable to TMLs in the range 3 % to 28 % (mass fraction).

ISO 12743:2006 sets out the basic methods for sampling copper, lead, zinc and nickel concentrates from moving streams and stationary lots, including stopped-belt sampling, to provide samples for chemical analysis, physical testing and determination of moisture content, in accordance with the relevant International Standards.

ISO 10378:2005 specifies a fire assay gravimetric and flame atomic absorption spectrometric method for the determination of the mass fraction of gold and silver in copper, lead and zinc sulfide concentrates.

This International Standard specifies an acid decomposition, solvent extraction, flame atomic absorption spectrometric procedure for the determination of gold in zinc sulfide concentrates. The method is applicable to the determination of gold in zinc concentrates containing up to 60 % (m/m) zinc in the form of zinc blende and related materials. The method is applicable to gold contents from 0,5 g/t to 12 g/t.

Fire assaying comprises the following steps: crucible fusion, cupellation, parting (followed by flame atomic absorption spectrometry), retreatment, correction for blank contamination. The method is applicable for copper sulfide concentrates containing 15 % (m/m) to 60 % (m/m) copper, mainly in the form of chalcopyrite and related sulfide minerals, and gold contents from 0,5 g/t to 300 g/t and silver contents from 25 g/t to 1500 g/t.

Specifies two titrimetric methods for the determination of the copper content of copper sulfide concentrates in the range 15 % (m/m) to 50 % (m/m), titrating free iodine isolated by reaction between iodide ions and copper(II) ions with sodium thiosulfate using soluble starch as the indicator after separation (method 1) or without separation (method 2) of copper from interfering elements.

The principle of the method specified is decomposing a test portion in nitric and sulfuric acids, separating copper from interfering elements (silver, arsenic, antimony, selenium, tin, iron, bismuth, and tellurium), determining traces of copper in the electrolyte, the filtrate, all precipitates and residues by flame atomic absorption spectrometry (FAAS), dissolving and analysing copper deposits for coprecipitated elements, mainly silver, by FAAS or plasma atomic emission spectrometry. The method is applicable for copper contents of copper sulfide concentrates in the range 15 % (m/m) to 50 % (m/m).

The method given is applicable to copper, lead and zinc sulfide concentrates free from volatile organic flotation reagents, e.g. kerosene, and with hygroscopic moisture contents between 0,05 % (m/m) and 2 % (m/m). It is used to correct the analysis results from the equilibrated moisture level to the dry basis. This method is not applicable to sulfide concentrates which are susceptible to oxidation. Annex A sets out a modified procedure which can be used in this case.