GB/T 11064.14-2013 English PDF (GB/T11064.14-2013)

GB/T 11064.14-2013: Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 14: Determination of arsenic content -- Molybdenum blue spectrophotometric method
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GB/T 11064.14-2013
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing GB/T 11064.14-1989
Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and
lithium chloride -
Part 14. Determination of arsenic content -
Molybdenum blue spectrophotometric method
ISSUED ON. NOVEMBER 27, 2013
IMPLEMENTED ON. AUGUST 1, 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 Instruments and devices ... 6 
5 Samples ... 7 
6 Analysis steps ... 7 
7 Calculation of analysis results ... 8 
8 Precision ... 9 
9 Test report ... 9 
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 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 14 of GB/T 11064.
This Part is drafted in accordance with rules given in GB/T 1.1-2009.
Methods for chemical analysis of lithium carbonate,
lithium hydroxide monohydrate and lithium chloride -
Part 14. Determination of arsenic content -
Molybdenum blue spectropotometic method
1 Scope
This Part of GB/T 11064 specifies the determination method of arsenic content in
lithium carbonate.
This Part applies to the determination of arsenic content in lithium carbonate. The
determination range is 0.00001% ~ 0.00020%.
2 Method summary
The sample is decomposed with hydrochloric acid; in the presence of potassium
iodide and stannous chloride, in hydrochloric acid medium, use zinc particles to
reduce; generated arsine is absorbed by iodine solution. In 0.2mol/L sulfuric acid
medium, arsenic and molybdate form arsenic molybdenum yellow; use ascorbic acid
to reduce it to arsenic molybdenum blue complex; measure its absorbance at where
the wavelength of the spectrophotometer is 840mm.
3 Reagents
Unless otherwise indicated, all reagents used in this Part are analytical reagent, the
water used is double-deionized water.
3.1 Arsenic-free zinc particles. granularity of φ1.5mm ~ 3mm.
3.2 Sulfuric acid (1 + 1), guarantee reagent.
3.3 Sulfuric acid (5 + 13), guarantee reagent.
3.4 Sulfuric acid (1 + 99), guarantee reagent.
3.5 Hydrochloric acid (ρ = 1.19g/ml), guarantee reagent.
3.6 Hydrochloric acid (1 + 1), guarantee reagent.
Where.
m1 - The arsenic content in the measurement sample solution refereed from the
working curve, in micrograms (μg);
m0 - The arsenic content in the blank solution refereed from the working curve, in
micrograms (μg);
m - The mass of the sample, in grams (g);
V - The total volume of the sample solution, in milliliters (mL);
V1 - The volume of the pipette sample solution, in milliliters (mL).
The result shall be expressed to five decimal places.
8 Precision
8.1 Repeatability
For the two independent test results obtained under repeatability conditions, within the
average-value range as given below, the absolute difference of these two test results
does not exceed the repeatability limit (r), and the situation exceeding repeatability
limit (r) is not more than 5%. Repeatability limit (r), according to Table 1, adopts linear
interpolation or epitaxy method to obtain.
Table 1
w(As)/% 0.000010 0.000074 0.00015
r/% 0.000003 0.000004 0.000005
8.2 Allowable difference
The difference of analysis results among laboratories shall not be more than the
allowable difference in Table 2.
Table 2
Mass fraction of arsenic/% Allowable difference/%
0.00001 ~ 0.00005 0.00001
>0.00005 ~ 0.00020 0.00003
9 Test report
The test report shall contain the following content.
- Sample;
- The number of this Standard;
- Analysis result and its expression;
- Difference with the basic analysis step;
- Anomalies observed in the determination;
- Test date.
GB/T 11064.14-2013
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing GB/T 11064.14-1989
Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and
lithium chloride -
Part 14. Determination of arsenic content -
Molybdenum blue spectrophotometric method
ISSUED ON. NOVEMBER 27, 2013
IMPLEMENTED ON. AUGUST 1, 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 Instruments and devices ... 6 
5 Samples ... 7 
6 Analysis steps ... 7 
7 Calculation of analysis results ... 8 
8 Precision ... 9 
9 Test report ... 9 
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 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 14 of GB/T 11064.
This Part is drafted in accordance with rules given in GB/T 1.1-2009.
Methods for chemical analysis of lithium carbonate,
lithium hydroxide monohydrate and lithium chloride -
Part 14. Determination of arsenic content -
Molybdenum blue spectropotometic method
1 Scope
This Part of GB/T 11064 specifies the determination method of arsenic content in
lithium carbonate.
This Part applies to the determination of arsenic content in lithium carbonate. The
determination range is 0.00001% ~ 0.00020%.
2 Method summary
The sample is decomposed with hydrochloric acid; in the presence of potassium
iodide and stannous chloride, in hydrochloric acid medium, use zinc particles to
reduce; generated arsine is absorbed by iodine solution. In 0.2mol/L sulfuric acid
medium, arsenic and molybdate form arsenic molybdenum yellow; use ascorbic acid
to reduce it to arsenic molybdenum blue complex; measure its absorbance at where
the wavelength of the spectrophotometer is 840mm.
3 Reagents
Unless otherwise indicated, all reagents used in this Part are analytical reagent, the
water used is double-deionized water.
3.1 Arsenic-free zinc particles. granularity of φ1.5mm ~ 3mm.
3.2 Sulfuric acid (1 + 1), guarantee reagent.
3.3 Sulfuric acid (5 + 13), guarantee reagent.
3.4 Sulfuric acid (1 + 99), guarantee reagent.
3.5 Hydrochloric acid (ρ = 1.19g/ml), guarantee reagent.
3.6 Hydrochloric acid (1 + 1), guarantee reagent.
Where.
m1 - The arsenic content in the measurement sample solution refereed from the
working curve, in micrograms (μg);
m0 - The arsenic content in the blank solution refereed from the working curve, in
micrograms (μg);
m - The mass of the sample, in grams (g);
V - The total volume of the sample solution, in milliliters (mL);
V1 - The volume of the pipette sample solution, in milliliters (mL).
The result shall be expressed to five decimal places.
8 Precision
8.1 Repeatability
For the two independent test results obtained under repeatability conditions, within the
average-value range as given below, the absolute difference of these two test results
does not exceed the repeatability limit (r), and the situation exceeding repeatability
limit (r) is not more than 5%. Repeatability limit (r), according to Table 1, adopts linear
interpolation or epitaxy method to obtain.
Table 1
w(As)/% 0.000010 0.000074 0.00015
r/% 0.000003 0.000004 0.000005
8.2 Allowable difference
The difference of analysis results among laboratories shall not be more than the
allowable difference in Table 2.
Table 2
Mass fraction of arsenic/% Allowable difference/%
0.00001 ~ 0.00005 0.00001
>0.00005 ~ 0.00020 0.00003
9 Test report
The test report shall contain the following content.
- Sample;
- The number of this Standard;
- Analysis result and its expression;
- Difference with the basic analysis step;
- Anomalies observed in the determination;
- Test date.