GB/T 14353.18-2014 English PDF (GBT14353.18-2014)

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GB/T 14353.18-2014: Methods for chemical analysis of copper ores, lead ores and zine ores -- Part 18: Determination of copper content, lead content, zinc content, cobalt content and nickel content
GB/T 14353.18-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060
D 40
Methods for chemical analysis of copper ores, lead
ores and zinc ores - Part 18: Determination of copper
content, lead content, zinc content, cobalt content and
nickel content
ISSUED ON: DECEMBER 05, 2014
IMPLEMENTED ON: APRIL 01, 2015
Issued by: General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 5 
3 Principle ... 6 
4 Reagents ... 6 
5 Instruments ... 8 
6 Test pieces ... 8 
7 Analysis steps ... 8 
8 Calculation of results ... 10 
9 Precision ... 11 
10 Quality assurance and control ... 11 
Appendix A (Informative) Instrument reference working conditions and
interference from coexisting ions ... 13 
Appendix B (Informative) Statistical processing of data of interlaboratory test
results ... 14 
References ... 22 
Methods for chemical analysis of copper ores, lead
ores and zinc ores - Part 18: Determination of copper
content, lead content, zinc content, cobalt content and
nickel content
Caution: The personnel who uses this Part shall have hands-on
experience in formal laboratory work. This Part 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 Part of GB/T 14353 specifies the simultaneous determination of copper
content, lead content, zinc content, cobalt content and nickel content in copper
ores, lead ores and zinc ores by the inductively coupled plasma-atomic
emission spectrometry.
This Part applies to the simultaneous determination of copper content, lead
content, zinc content, cobalt content and nickel content in copper ores, lead
ores and zinc ores by inductively coupled plasma-atomic emission spectrometry.
Determination range: copper of 0.002% ~ 8.5%; lead of 0.01% ~ 5%; zinc of
0.005% ~ 3%; cobalt of 0.001 5% ~ 0.5%; nickel of 0.003% ~ 0.5%.
The method detection-limit: 0.000 66% for copper, 0.003 2% for lead, 0.001 7%
for zinc, 0.000 47% for cobalt, 0.001 0% for nickel.
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.
GB/T 6682, Water for analytical laboratory use - Specification and test
methods
GB/T 14505, Method for chemical analysis of rocks and ores - General rules
and regulations
3 Principle
Place the sample, which has been decomposed by hydrochloric acid-nitric acid-
hydrofluoric acid-perchloric acid, in a 20% nitric acid medium (containing 3%
hydrochloric acid); introduce the solution of the to-be-tested sample into a high-
temperature plasma torch, so that the to-be-tested elements are activated into
ions and atoms that emit characteristic spectral lines of the contained elements.
Measure the emission spectrum intensity of ions and atoms of each element at
the specified wavelength; the emission spectrum intensity shall be proportional
to the concentration of the to-be-measured element. Use the calibration curve
method; calculate the content of the to-be-measured element by the computer
of the instrument.
4 Reagents
Unless otherwise stated, only use analytical reagents and laboratory water in
accordance with GB/T 6682 in the analysis.
4.1 Nitric acid (ρ = 1.42 g/mL).
4.2 Hydrofluoric acid (ρ = 1.13 g/mL). Warning: Hydrofluoric acid is toxic and
highly corrosive. Wear anti-corrosion gloves during the operation, to
prevent contact with skin.
4.3 Hydrochloric acid (ρ = 1.19 g/mL).
4.4 Perchloric acid (ρ = 1.68 g/mL). Warning: Explosive materials, handle
with care!
4.5 Mixed acid (nitric acid + hydrochloric acid = 4 + 1).
4.6 Nitric acid (1+9).
4.7 Preparation of standard solution
4.7.1 Prepare the copper standard solution according to the following steps:
a) Copper standard stock solution [ρ(Cu) = 1.00 mg/mL]: Weigh 0.500 0 g of
metallic copper (>99.99%); put it in a 250 mL beaker; cover with a watch
glass; add 10 mL of nitric acid (1+1) along the beaker wall; slightly heat it;
after all of it is dissolved, add 10 mL of sulfuric acid (1+1); steam until white
smoke of sulfur trioxide emits; remove and cool; add water to dissolve the
copper salt; use water to wash off the watch glass; cool and transfer to a
500 mL volumetric flask; use water to dilute to the mark; shake well;
b) Copper standard solution [ρ(Cu) = 100.0 μg/mL]: Divide 25.00 mL of
copper standard stock solution [4.7.1a)] into a 250 mL volumetric flask;
use hydrochloric acid (5+95) to dilute it to the mark; shake well;
c) Copper standard solution [ρ(Cu) = 20.0 μg/mL]: Divide 50.00 mL of copper
standard solution [4.7.1b)] into a 250 mL volumetric flask; use hydrochloric
acid (5+95) to dilute to the mark; shake well.
4.7.2 Prepare the lead standard solution according to the following steps:
a) Lead standard stock solution [ρ(Pb) = 1.00 mg/mL]: Weigh 1.000 0 g of
metallic lead (>99.99%); put it in a 250 mL beaker; cover with a watch
glass; add 10 mL of nitric acid (1+1) along the beaker wall; after heating
and dissolving, use a small amount of water to wash the watch glass;
transfer it to a 1 000 mL volumetric flask; use water to dilute to the mark;
shake well;
b) Lead standard solution [ρ(Pb) = 20.0 μg/mL]: Divide 20.00 mL of lead
standard stock solution [4.7.2a)]; put it in a 1 000 mL volumetric flask; use
water to dilute to the mark; shake well.
4.7.3 Prepare the zinc standard solution according to the following steps:
a) Zinc standard stock solution [ρ(Zn) = 1.00 mg/mL]: Weigh 1.000 0 g of
metallic zinc (>99.99%); put it in a 250 mL beaker; cover with a watch
glass; add 10 mL of hydrochloric acid (1+1) along the beaker wall; let it
have autolysis (if the acid is not enough, it can be added); after it is
completely dissolved, use water to wash off the watch glass; transfer it
into a 1 000 mL volumetric flask; use water to dilute to the mark; shake
well;
b) Zinc standard solution [ρ(Zn) = 20.0 μg/mL]: Divide 20.00 mL of zinc
standard stock solution [4.7.3a)]; put it in a 1 000 mL volumetric flask; use
water to dilute to the mark; shake well.
4.7.4 Prepare the cobalt standard solution according to the following steps:
a) Cobalt standard stock solution [ρ(Co) = 100 μg/mL]: Weigh 0.100 0 g of
metallic cobalt (>99.99%); put it in a 100 mL beaker; cover with a watch
glass; add 20 mL of nitric acid (1+1) along the beaker wall; heat to dissolve;
evaporate to dryness at low temperature; use a small amount of water to
rinse the watch glass; add 5 mL of hydrochloric acid (4.3); evaporate to
dryness at low temperature; repeat once. Add 10 mL of hydrochloric acid
(4.3) to dissolve the cobalt salt; cool it; use water to transfer it into a 1 000
mL volumetric flask and dilute it to the mark; shake well, and set aside.