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GB/T 11064.16-2013 PDF in English


GB/T 11064.16-2013 (GB/T11064.16-2013, GBT 11064.16-2013, GBT11064.16-2013)
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GB/T 11064.16-2013: PDF in English (GBT 11064.16-2013)

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...
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.