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Methods for chemical analysis of copper concentrates - Part 1: Determination of copper content - Iodine titration method and electrogravimetric method
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| GB/T 3884.1-2012 | English | 125 |
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Methods for chemical analysis of copper concentrates - Part 1: Determination of copper content - Iodine titration method
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| GB/T 3884.1-2000 | English | 279 |
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Methods for chemical analysis of copper concentrates. Determination of copper content
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Methods for chemical analysis of copper concentrates--The thiosulfate-iodometric method for the determination of copper content
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Similar standards GB/T 4103.14 | GB/T 3884.4 | GB/T 3884.1-2025: Methods for chemical analysis of copper concentrates - Part 1: Determination of copper content - Iodine titration method and electrogravimetric method
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.30
CCS H 13
Replacing GB/T 3884.1-2012, GB/T 3884.13-2012
Methods for chemical analysis of copper concentrates - Part
1.Determination of copper content - Iodine titration method
and electrogravimetric method
(ISO 10469.2006 Copper sulfide concentrates - Determination of copper -
Electrogravimetric method, MOD)
Issued on: OCTOBER 31, 2025
Implemented on: MAY 01, 2026
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
Introduction... 7
1 Scope... 9
2 Normative references... 9
3 Terms and definitions... 9
4 Method 1.Long iodine titration method... 9
5 Method 2.Short iodine titration method... 15
6 Electrogravimetric method... 20
7 Test report... 28
Appendix A (Informative) Comparison of structure numbers between this document
and ISO 10469.2006... 29
Appendix B (Informative) Technical differences between this document and ISO
10469.2006 and the reasons therefor... 31
Methods for chemical analysis of copper concentrates - Part
1.Determination of copper content - Iodine titration method
and electrogravimetric method
WARNING – Persons using this document shall have practical experience in
formal laboratory work. This document does not address all possible security
issues. It is the responsibility of the user to take appropriate safety and health
measures and to ensure compliance with the conditions which are set by the
relevant national regulations.
1 Scope
This document describes methods for determining the copper content in copper
concentrates and copper slag concentrates using iodine titration method and
electrogravimetric method.
This document applies to the determination of copper content in copper concentrates
and copper slag concentrates. The determination range is 12.00% ~ 50.00%.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this
document and are indispensable for its application. For dated references, only the
edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
GB/T 3884.2, Methods for chemical analysis of copper concentrates - Part 2.
Determination of gold and silver contents - Flame atomic absorption
spectrometric method and fire assay method
GB/T 6682, Water for analytical laboratory use - Specification and test methods
3 Terms and definitions
No terms and definitions need to be defined in this document.
4 Method 1.Long iodine titration method
4.1 Principle
Decompose the sample by hydrochloric acid, nitric acid and sulfuric acid; add sodium
thiosulfate solution to the dilute sulfuric acid solution to separate copper ions from the
solution in the form of copper sulfide. Dissolve the precipitate in a mixed acid; adjust
the pH of the solution to 3.0 ~ 4.0; use ammonium fluoride to mask the iron; add
potassium iodide to react with divalent copper. The precipitated iodine is titrated with
standard sodium thiosulfate solution using starch as an indicator to determine copper
content. Correct the copper content in the filtrate using atomic absorption spectrometry.
4.2 Reagents
Unless otherwise stated, use only reagents that are identified as analytical reagents in
the analysis.
4.2.1 Water, GB/T 6682, Grade III.
4.2.2 Pure copper sheet (wCu≥99.99%). Place the pure copper in a gently boiling acetic
acid solution (1+4) for 1 minute; remove it and rinse it with water and anhydrous
ethanol at least twice; then bake it in an oven at 100 ℃ ~ 105 ℃ for 4 minutes; cool it;
place it in a ground glass bottle for later use.
4.2.3 Potassium iodide.
4.2.4 Hydrochloric acid (ρ = 1.19 g/mL).
4.2.5 Nitric acid (ρ = 1.42 g/mL).
4.2.6 Sulfuric acid (ρ = 1.84 g/mL).
4.2.7 Nitric acid (1+1).
4.2.8 Mixed acid of nitric acid and sulfur. Slowly add 3 parts of sulfuric acid (4.2.6)
along the wall of the cup to 7 parts of nitric acid (4.2.5) while stirring; mix well and
cool before use.
4.2.9 Mixed acid. Mix 15 parts of nitric acid (4.2.5) with 5 parts of perchloric acid (ρ =
1.67 g/mL); slowly add 3 parts of sulfuric acid (4.2.6) along the wall of the beaker while
stirring; mix well and cool before use.
4.2.10 Sodium thiosulfate solution (200 g/L, freshly prepared and used immediately).
4.2.11 Saturated ammonium acetate solution.
4.2.12 Saturated solution of ammonium bifluoride (stored in polyethylene bottles).
4.2.13 Potassium thiocyanate solution (100 g/L).
4.2.14 Sodium thiosulfate standard titration solution (cNa2S2O3·5H2O≈0.04 mol/L), shall be
recalibrated once a week, and prepared and calibrated in the following manner.
ρ – mass concentration of copper in the filtrate, obtained from the working curve, in
micrograms per milliliter (μg/mL);
V4 – total volume of residual copper solution, in milliliters (mL).
Express the calculation result to two decimal places.
4.7 Precision
4.7.1 Repeatability
For the measured values of the two independent test results that are obtained under
repetitive conditions, within the average range given in Table 1, the absolute difference
between the two test results does not exceed the repeatability limit (r); the case of
exceeding the repeatability limit (r) is not more than 5%. The repeatability limit (r) is
obtained using linear interpolation or extrapolation as shown in Table 1.
4.7.2 Reproducibility
The absolute difference between two independent test results obtained under
reproducibility conditions shall not exceed the reproducibility limit (R) within the range
of average values given in Table 2, and the number of cases exceeding the
reproducibility limit (R) shall not exceed 5%. The reproducibility limit (R) shall be
obtained by linear interpolation or extrapolation method according to the data in Table
2.
5 Method 2.Short iodine titration method
5.1 Principle
After the sample is decomposed by hydrochloric acid, nitric acid, bromine or perchloric
acid, use saturated ammonium acetate solution to adjust the pH of the solution to 3.0 ~
4.0; use ammonium fluoride to mask iron; add potassium iodide to react with divalent
copper. The precipitated iodine is titrated with standard sodium thiosulfate solution
using starch as an indicator to determine the copper content.
5.2 Reagents
Unless otherwise stated, use only reagents that are identified as analytical reagents in
the analysis.
5.2.1 Water, GB/T 6682, Grade III.
5.2.2 Pure copper sheet (wcu≥99.99%). Place the pure copper in a gently boiling glacial
acetic acid solution (1+4) for 1 minute; remove it, and use water and anhydrous ethanol
to rinse it twice respectively; dry it in an oven at 100 ℃ ~ 105 ℃ for 4 minutes; cool
it; place it in a ground glass bottle for later use.
5.2.3 Potassium iodide.
5.2.4 Hydrochloric acid (ρ = 1.19 g/mL).
5.2.5 Nitric acid (ρ = 1.42 g/mL).
5.2.6 Perchloric acid (ρ = 1.67 g/mL).
5.2.7 Sulfuric acid (ρ = 1.84 g/mL).
5.2.8 Bromine.
5.2.9 Nitric acid (1+1).
5.2.10 Nitric-sulfur mixed acid. Slowly add 300 mL of sulfuric acid (5.2.7) along the
wall of the beaker to 700 mL of nitric acid (5.2.5) while stirring; mix well and cool
before use.
5.2.11 Saturated ammonium acetate solution.
5.2.12 Saturated solution of ammonium bifluoride (stored in polyethylene bottles).
5.2.13 Potassium thiocyanate solution (100 g/L).
5.2.14 Sodium thiosulfate standard titration solution (cNa2S2O3·5H2O≈0.04 mol/L), shall be
recalibrated once a week, and prepared and calibrated in the following manner.
a) Preparation. Weigh 100 g of sodium thiosulfate (Na2S2O3·5H2O) into a 1 000
mL beaker; add 500 mL of sodium carbonate solution (4 g/L); transfer to a 10
L brown reagent bottle; use boiling and cooled water to dilute to about 10 L;
shake well; let stand for two weeks. When using, filter the mixture into the
lower bottle; mix well; let stand for 2 hours; store in the dark.
b) Calibration. Weigh three portions of 0.080 g pure copper sheet (5.2.2), accurate
to 0.000 01 g; place them in 250 mL Erlenmeyer beakers respectively; add 10
mL of nitric acid (5.2.9); heat on a hot plate at a low temperature until
completely dissolved, and the remaining volume is about 3 mL; continue to
add 1 mL ~ 2 mL of sulfuric acid (5.2.7) and evaporate until dry; remove and
cool to room temperature; use 30 mL of water to rinse the beaker wall; heat to
boiling, remove and cool to room temperature; add saturated ammonium
acetate solution (5.2.11) until the color just turns dark blue and there is an
excess of 1 mL; then add 3 mL of saturated ammonium bifluoride solution
(5.2.12) and shake well. Add 2 ~ 3 g of potassium iodide (5.2.3); shake to
dissolve; immediately titrate with sodium thiosulfate standard solution until
light yellow; add 2 mL of starch solution (5.2.15); continue titrating until light
blue; add 5 mL of potassium thiocyanate solution (5.2.13); shake vigorously
until the blue color deepens, and titrate until the blue color just disappears as
the endpoint. Perform a blank test along with the calibration.
Calculate the actual concentration of the sodium thiosulfate standard titration solution
according to Formula (3).
Where.
с – actual concentration of the sodium thiosulfate standard titration solution, in moles
per liter (mol/L);
m2 – mass of the pure copper sheet, in grams (g);
V5 – volume of sodium thiosulfate standard titration solution consumed in titrating the
copper solution during calibration, in milliliters (mL);
V6 – volume of sodium thiosulfate standard titration solution consumed in titrating the
copper blank solution during calibration, in milliliters (mL);
63.546 – molar mass of copper, in grams per mole (g/mol).
Perform four parallel calibrations, and retain the results to four significant figures. If
the range of the results is no greater than 5 × 10⁻⁵ mol/L, take the average value;
otherwise, repeat the calibration.
5.2.15 Starch solution (5 g/L).
5.3 Test sample
5.3.1 The sample particle size shall not exceed 100 μm.
5.3.2 Dry the sample in an oven at 100 ℃ ~ 105 ℃ for 1 hour; then cooled to room
temperature in a desiccator for later use.
5.4 Procedure
5.4.1 Test portion
Weigh 0.25 g of sample (5.3), accurate to 0.000 1 g.
5.4.2 Parallel test
Perform two tests in parallel, and take the average value.
5.4.3 Blank test
Carry out a blank test along with the sample.
5.4.4 Determination
5.4.4.1 Sample preparation
5.4.4.1.1 Place the sample in a 250 mL Erlenmeyer beaker; use a small amount of water
to moisten it; add 10 mL of hydrochloric acid (5.2.4); place it on a hot plate to dissolve
at low temperature for 3 min ~ 5 min; remove it and let it cool slightly [if the test portion
sticks to the bottom, add 1 mL ~ 2 mL of saturated ammonium fluoride solution
(5.2.12)]; add 5 mL of nitric acid (5.2.5). Proceed according to 5.4.4.1.2 or 5.4.4.1.3
depending on the state of the solution.
5.4.4.1.2 If the solution is clear and free of residue after adding nitric acid, add 0.5 mL
~ 1 mL of bromine (5.2.8); cover with a watch glass; mix well; heat at low temperature
until the red smoke stops and the bromine is completely decomposed; remove and cool
slightly; use a small amount of water to wash the watch glass; continue heating and
evaporating until nearly dry; remove and cool to room temperature; use about 30 mL of
water to rinse the watch glass and the glass wall.
5.4.4.1.3 If the solution becomes turbid or has residue after adding nitric acid, add 3 mL
~ 5 mL of perchloric acid (5.2.6); cover with a watch glass and continue heating until
thick white fumes are produced and the volume is reduced to a small volume [when the
content of arsenic, antimony, and tin is high, add hydrobromic acid (ρ = 1.42 g/mL) to
remove impurities]; remove the sample. If the sample contains chromium, after the
perchloric acid produces thick white fumes, add 3 mL of hydrochloric acid (5.2.4) to
remove the red and yellow fumes, repeating twice (when the chromium content is too
high and repeated use of hydrochloric acid cannot remove it completely; or when the
calcium content is ≥5% and the magnesium content is ≥10%, use the long iodine
method), and remove the sample. If there are still undissolved residues after the
perchloric acid produces fumes, remove the sample, cool it to room temperature, add 1
mL ~ 2 mL of saturated ammonium bifluoride solution (5.2.12) and 5 mL of nitric acid-
sulfur mixture (5.2.10); then heat until thick white fumes are produced and the residue
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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