GB/T 11064.16-2023_English: PDF (GB/T11064.16-2023)
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 16: Determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium, aluminum, iron and sulfate contents - Inductively couple
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 16: Determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium and aluminum content -- Inductively coupled plasma atomi
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GB/T 11064.16-1989 | English | 199 |
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Lithium carbonate--Determination of sodium and potassium contents--Flame atomic emission spectrometric method
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GB/T 11064.16-1989
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Standard ID | GB/T 11064.16-2023 (GB/T11064.16-2023) | Description (Translated English) | Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 16: Determination of calcium, magnesium, copper, lead, zinc, nickel, manenases, cadmium, aluminum, iron and sulfate contents - Inductively coupled pl | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | H14 | Classification of International Standard | 77.120.99 | Word Count Estimation | 18,117 | Date of Issue | 2023-08-06 | Date of Implementation | 2024-03-01 | Older Standard (superseded by this standard) | GB/T 11064.16-2013 | Drafting Organization | Tianqi Lithium Industry Co., Ltd., Jiangxi Ganfeng Lithium Industry Co., Ltd., Yichun Silver Lithium New Energy Co., Ltd., Yahua Lithium Industry (Ya'an) Co., Ltd., Xinjiang Nonferrous Metals Research Institute, Guohe General (Qingdao) Test and Evaluation Co., Ltd., Zijin Mining Group Co., Ltd., Zhejiang Huayou Cobalt Co., Ltd., Guangdong Bangpu Recycling Technology Co., Ltd., Jiangxi Jiuling Lithium Co., Ltd. | Administrative Organization | National Nonferrous Metals Standardization Technical Committee (SAC/TC 243) | Proposing organization | China Nonferrous Metals Industry Association | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration | Standard ID | GB/T 11064.16-2013 (GB/T11064.16-2013) | Description (Translated English) | Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 16: Determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium and aluminum content - Inductively coupled plasma atomic | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | H64 | Classification of International Standard | 77.120.99 | Word Count Estimation | 8,868 | Older Standard (superseded by this standard) | GB/T 11064.17-1989; GB/T 11064.18-1989 | Drafting Organization | Ganzhou Nonferrous Metallurgy Research Institute | Administrative Organization | National Standardization Technical Committee of non-ferrous metals | Regulation (derived from) | National Standards Bulletin 2013 No. 23 | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | Summary | This standard specifies the lithium carbonate, lithium hydroxide monohydrate, calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium, lithium determination of the amount of aluminum chloride. This standard applies to lithium carbonate, lithium | Standard ID | GB/T 11064.16-1989 (GB/T11064.16-1989) | Description (Translated English) | Lithium carbonate--Determination of sodium and potassium contents--Flame atomic emission spectrometric method | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | H14 | Classification of International Standard | 71.06 | Word Count Estimation | 4,429 | Date of Issue | 1989/3/31 | Date of Implementation | 1990/2/1 | Quoted Standard | GB 1.4; GB 1467; GB 7728 | Drafting Organization | Xinjiang Non-ferrous metals Institute | Regulation (derived from) | National Standards Bulletin 2013 No. 17 | Proposing organization | China Institute of Standard Metrology, China Nonferrous Metals Industry Corporation | Issuing agency(ies) | State Bureau of Technical Supervision | Summary | This Standard specifies Determination of sodium and potassium content of lithium carbonate. This Standard is applicable to the determination of phosphor-grade lithium carbonate, sodium and potassium. Measurement range: 0. 000050% to 0. 0050%. |
GB/T 11064.16-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
CCS H 14
Replacing GB/T 11064.16-2013
Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride - Part 16:
Determination of calcium, magnesium, copper, lead, zinc,
nickel, manganese, cadmium, aluminum, iron and sulfate
contents - Inductively coupled plasma atomic emission
spectrometry
ISSUED ON: AUGUST 06, 2023
IMPLEMENTED ON: MARCH 01, 2024
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 5
1 Scope ... 7
2 Normative references ... 7
3 Terms and definitions ... 8
4 Principle ... 8
5 Reagents or materials ... 8
6 Instruments and equipment ... 10
7 Samples ... 10
8 Test steps ... 10
9 Test data processing ... 12
10 Precision ... 12
11 Test report ... 15
Annex A (informative) Recommended analytical spectral lines and instrument
operating parameters ... 16
Annex B (informative) Statistics data derived from laboratory results ... 17
Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride - Part 16:
Determination of calcium, magnesium, copper, lead, zinc,
nickel, manganese, cadmium, aluminum, iron and sulfate
contents - Inductively coupled plasma atomic emission
spectrometry
1 Scope
This document describes methods for the determination of calcium, magnesium, copper,
lead, zinc, nickel, manganese, cadmium, aluminum, iron, and sulfate content in lithium
carbonate, lithium hydroxide monohydrate, and lithium chloride.
This document is applicable to the determination of calcium, magnesium, copper, lead,
zinc, nickel, manganese, cadmium, aluminum, iron, and sulfate content in lithium
carbonate, lithium hydroxide monohydrate, and lithium chloride. The measurement
range of each element is shown in Table 1.
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 8170, Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 17433, Foundation terms for chemical analysis of metallurgical products
3 Terms and definitions
For the purposes of this document, the terms and definitions defined in GB/T 17433
apply.
4 Principle
Lithium carbonate and lithium hydroxide monohydrate are decomposed with nitric acid.
Lithium chloride is dissolved in water. In nitric acid medium, the matrix matching
standard curve method is used to determine the contents of calcium, magnesium, copper,
lead, zinc, nickel, manganese, cadmium, aluminum, iron, and sulfate on an inductively
coupled plasma atomic emission spectrometer.
5 Reagents or materials
Unless otherwise stated, only reagents confirmed to be of guaranteed reagents are used
in the analysis.
5.1 Water, GB/T 6682, grade 2.
5.2 High purity lithium carbonate (mass fraction is greater than 99.99%, Fe, Cu, Pb, Zn,
Ni, Ca, Mg, Mn, Cd, Al, are all less than 0.0001%).
5.3 Nitric acid (1+1).
5.4 Calcium standard storage solution: Weigh 0.2497 g of spectrally pure calcium
carbonate into a 200 mL beaker. Then add 20.00 mL of nitric acid (5.3) and dissolve at
low temperature until clear. Cool down. Transfer to a 100 mL volumetric flask. Use
water to set the volume constant. Shake well. 1 mL of this solution contains 1.0 mg of
calcium.
5.5 Magnesium standard storage solution: Weigh 0.1658 g of magnesium oxide [w
(MgO) ≥99.99%] that has been pre-burned at 800°C for 2 h and cooled to room
temperature in a desiccator into a 200 mL beaker. Add 20.00 mL of nitric acid (5.3).
Dissolve at low temperature until clear and cool. Transfer to a 100 mL volumetric flask.
Use water to set the volume constant. Shake well. 1 mL of this solution contains 1.0 mg
of magnesium.
5.6 Copper standard storage solution: Weigh 0.100 g of pure metallic copper (spectrally
pure, clean surface oxide before use) into a 200 mL beaker. Add 20.00 mL nitric acid
(5.3). Dissolve at low temperature until clear. Cool down. Transfer to a 100 mL
volumetric flask. Use water to set the volume constant. Shake well. 1 mL of this solution
contains 1.0 mg of copper.
5.7 Lead standard storage solution: Weigh 0.1077 g of spectrally pure lead dioxide into
a 200 mL beaker. Add 20.00 mL of nitric acid (5.3). Dissolve at low temperature until
clear. Cool down. Transfer to a 100 mL volumetric flask. Use water to set the volume
constant. Shake well. 1 mL of this solution contains 1.0 mg of lead.
5.8 Zinc standard storage solution: Weigh 0.1000 g of pure metallic zinc (spectrally
pure, clean surface oxide before use) into a 200 mL beaker. Add 20.00 mL of nitric acid
(5.3). Dissolve at low temperature until clear. Cool down. Transfer to a 100 mL
volumetric flask. Use water to set the volume constant. Shake well. 1 mL of this solution
contains 1.0 mg of zinc.
5.9 Nickel standard storage solution: Weigh 0.100 g of pure metallic nickel (spectrally
pure, clean surface oxide before use) into a 200 mL beaker. Add another 20.00 mL of
nitric acid (5.3). Dissolve at low temperature until clear. Cool down. Transfer to a 100
mL volumetric flask. Use water to set the volume constant. Shake well. 1 mL of this
solution contains 1.0 mg of nickel.
5.10 Manganese standard storage solution: Weigh 0.100 g of pure metallic manganese
(spectrally pure, clean surface oxide before use) into a 200 mL beaker. Add 20.00 mL
of nitric acid (5.3). Dissolve at low temperature until clear. Cool down. Transfer to a
100 mL volumetric flask. Use water to set the volume constant. Shake well. 1 mL of
this solution contains 1.0 mg of manganese.
5.11 Cadmium standard storage solution: Weigh 0.100 g of pure metal cadmium
(spectrally pure, clean surface oxide before use) into a 200 mL beaker. Add 20.00 mL
of nitric acid (5.3). Dissolve at low temperature until clear. Cool down. Transfer to a
100 mL volumetric flask. Use water to set the volume constant. Shake well. 1 mL of
this solution contains 1.0 mg of cadmium.
5.12 Aluminum standard storage solution: Weigh 0.100 g of pure metallic aluminum
(spectrally pure, clean surface oxide before use) into a 200 mL beaker. Add 20.00 mL
of nitric acid (5.3). Dissolve at low temperature until clear. Cool down. Transfer to a
100 mL volumetric flask. Use water to set the volume constant. Shake well. 1 mL of
this solution contains 1.0 mg of aluminum.
5.13 Iron standard storage solution: Weigh 0.100 g of pure metal wire (spectrally pure,
clean surface oxide before use) into a 200 mL beaker. Add 20.00 mL of nitric acid (5.3).
Dissolve in water bath until clear. Cool down. Transfer to a 100 mL volumetric flask.
Use water to set the volume constant. Shake well. 1 mL of this solution contains 1.0 mg
of iron.
5.14 Sulfate standard storage solution: Weigh 0.5446 g of potassium sulfate (mass
......
GB/T 11064.16-2013
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing GB/T 11064.16-1989
Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride -
Part 16. Determination of calcium, magnesium, copper, lead,
zinc, nickel, manganese, cadmium and aluminum content -
Inductively coupled plasma atomic emission spectrometry
ISSUED ON. NOVEMBER 27, 2013
IMPLEMENTED ON. AUGUST 01, 2014
Issued by.
General Administration of Quality Supervision, Inspection
and Quarantine of the People’s Republic of China;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Method Summary... 5
3 Reagents ... 5
4 Instrument ... 7
5 Samples ... 7
6 Analysis Steps ... 7
7 Calculation of Analysis Results ... 8
8 Precision ... 9
9 Test report ... 10
Foreword
GB/T 11064 “Methods for chemical analysis of lithium carbonate, lithium hydroxide
monohydrate and lithium chloride” is divided into 16 parts.
- Part 1. Determination of lithium carbonate content - Acid-alkali titrimetric method;
- Part 2. Determination of lithium hydroxide content - Acid-alkali titrimetric method;
- Part 3. Determination of lithium chloride content - Potentiometric method;
- Part 4. Determination of potassium and sodium content - Flame atomic
absorption spectrometric method;
- Part 5. Determination of calcium content - Flame atomic absorption spectrometric
method;
- Part 6. Determination of magnesium content - Flame atomic absorption
spectrometric method;
- Part 7. Determination of iron content - 1,10-phenanthroline spectrophotometric
method;
- Part 8. Determination of silicon content - Molybdenum blue spectrophotometric
method;
- Part 9. Determination of sulfate content - Barium sulfate nephelometry method;
- Part 10. Determination of chloride content - Silver chloride nephelometry method;
- Part 11. Determination of Acid-insolubles Content - Gravimetric method;
- Part 12. Determination of carbonate content - Determination of lithium chloride
content - Potentiometric method;
- Part 13. Determination of aluminum content - Chromazurol S-cetylpyridine
bromide spectrophotometric method;
- Part 14. Determination of arsenic content - Molybdenum blue spectrophotometric
method;
- Part 15. Determination of fluoride content - Ion selective method;
- Part 16. Determination of calcium, magnesium, copper, lead, zinc, nickel,
manganese, cadmium and aluminum content - Inductively coupled plasma
atomic emission spectrometry.
This Part is part 16 of GB/T 11064.
This Part is drafted in accordance with rules given in GB/T 1.1-2009.
This Part replaces GB/T 11064.17-1989 "Lithium carbonate - Determination of iron
and lead contents – Coprecipitation-flame atomic absorption spectrometric method"
and GB/T 11064.18-1989 "Lithium carbonate - Determination of calcium, magnesium,
copper, zinc, nickel, manganese and cadmium content - Ion exchange-flame atomic
absorption spectrometric method".
Compared with GB/T 11064.17-1989 and GB/T 11064.18-1989, the main technical
changes are as follows.
- The determination method is modified from "Flame atomic absorption
spectrometric method" to "Inductively coupled plasma atomic emission
spectrometry";
- ADD the repeatability terms;
- RE-EDIT the text format; ADD the test report.
This Part shall be under the jurisdiction of National Standardization Technical
Committee of Nonferrous Metals (SAC/TC 243).
Drafting organizations of this Part. Ganzhou Non-ferrous Metallurgy Research
Institute, Xinjiang Research Institute of Non ferrous Metals, and Beijing General
Research Institute of Mining & Metallurgy.
The main drafters of this Part. Liu Hong, Pan Jianzhong, Li Ying, Guan Yuzhen, Wang
Hongchuan, and Feng Xianjin.
The historical version replaced by this Part is as follows.
- GB/T 11064.18-1989.
Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride -
Part 16. Determination of calcium, magnesium, copper, lead,
zinc, nickel, manganese, cadmium and aluminum content -
Inductively coupled plasma atomic emission spectrometry
1 Scope
This Part of GB/T 11064 specifies the determination method of calcium, magnesium,
copper, lead, zinc, nickel, manganese, cadmium and aluminum content in lithium
carbonate, in lithium hydroxide monohydrate, and in lithium chloride.
This Part applies to the determination of the content of calcium, magnesium, copper, lead,
zinc, nickel, manganese, cadmium, aluminum in lithium carbonate, in lithium hydroxide
monohydrate, and in lithium chloride. The determination range is 0.000 1%~0.008 0% for
manganese, cadmium, nickel, and zinc; 0.000 2%~0.008 0% for calcium, aluminum,
copper, and magnesium; 0.000 4%~0.008 0% for lead.
2 Method Summary
The lithium carbonate and lithium hydroxide monohydrate shall be decomposed by nitric
acid; the lithium chloride shall be dissolved by water. In nitric acid medium, adopt matrix
matching method to determine the content of calcium, magnesium, copper, lead, zinc,
nickel, manganese, cadmium, and aluminum on ICP-AES instrument.
3 Reagents
Unless otherwise specified, the reagent used in this Part is an analytical pure reagent, and
the water used in this Part is the secondary deionized water.
3.1 Nitric acid (ρ=1.42g/mL).
3.2 Hydrochloric acid (ρ=1.19g/mL).
3.3 Nitric acid solution (1 + 1).
3.4 Hydrochloric acid solution (1 + 1).
3.5 Aluminum standard stock solution. weigh 0.100 0 g of pure aluminum
(spectroscopically pure, wipe off the oxide on its surface before use); place it in a 200mL
beaker; add 20 mL of hydrochloric acid (3.3); place it at low temperature; melt it to be clear;
cool down. Transfer it into a 100 mL volumetric flask; fix its volume with water; shake it.
This solution contains 1mg/mL aluminum.
3.6 Copper standard stock solution. weigh 0.100 0 g of pure copper (spectroscopically
pure, wipe off the oxide on its surface before use) and place it in a 200mL beaker; add 20
mL of Nitric acid (3.2); place it at low temperature and melt it to be clear and cool. Transfer
it in a 100 mL volumetric flask and fix its volume with water and shake it. This solution
contains 1mg/mL copper.
3.7 Zinc standard stock solution. weigh 0.100 0 g of pure zinc (spectroscopically pure,
wipe off the oxide on its surface before use); place it in a 200mL beaker; add 20 mL of
Nitric acid (3.2); place it at low temperature; melt it to be clear and cool. Transfer it in a
100 mL volumetric flask; fix its volume with water; shake it. This solution contains 1mg/mL
zinc.
3.8 Manganese standard stock solution. weigh 0.100 0 g of pure manganese
(spectroscopically pure, wipe off the oxide on its surface before use); place it in a 200mL
beaker; add 20 mL of nitric acid (3.2); place it at low temperature; melt it to be clear; cool
down. Transfer it into a 100 mL volumetric flask; fix its volume with water; shake it. This
solution contains 1mg/mL manganese.
3.9 Cadmium standard stock solution. weigh 0.100 0 g of pure cadmium
(spectroscopically pure, wipe off the oxide on its surface before use); place it in a 200mL
beaker; add 20 mL of nitric acid (3.2); place it at low temperature; melt it to be clear and
cool. Transfer it into a 100 mL volumetric flask; fix its volume with water and shake it. This
solution contains 1mg/mL cadmium.
3.10 Nickel standard stock solution. weigh 0.100 0 g of pure nickel (spectroscopically pure,
wipe off the oxide on its surface before use); place it in a 200mL beaker; add 20 mL of
nitric acid (3.2); place it at low temperature; melt it to be clear; cool down. Transfer it into a
100 mL volumetric flask; fix its volume with water; shake it. This solution contains 1mg/mL
nickel.
3.11 Lead standard stock solution. weigh 0.107 7 g of spectroscopically-pure lead dioxide;
place it into a 200 mL beaker; add 20 mL of nitric acid (3.2); place it at low temperature;
melt it to be clear; cool down. Transfer it into a 100 mL volumetric flask; fix its volume with
water; shake it. This solution contains 1mg/mL lead.
3.12 Calcium standard stock solution. weigh 0.249 7 g of spectroscopically-pure calcium
carbonate; place it into a 200 mL beaker; add 20 mL of nitric acid (3.2); place it at low
temperature; melt it to be clear; cool down. Transfer it into a 100 mL volumetric flask; fix its
volume with water; shake it. This solution contains 1mg/mL calcium.
3.13 Magnesium standard stock solution. weigh 0.165 8 g of magnesium oxide
[w(MgO)>99.99%] that has been preheated in a dry container at 800°C for 2 hours, and
8.2 Allowable difference
The difference of analysis results among laboratories shall not be more than the
allowable difference in Table 5.
Table 5
The ma...
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