GB/T 11064.15-2013 English PDF (GBT11064.15-2013)

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GB/T 11064.15-2013: Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 15: Determination of fluoride content -- Ion selective method
GB/T 11064.15-2013
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing GB/T 11064.15-1989
Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and
lithium chloride -
Part 14. Determination of fluoride content - Ion
selective 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 ... 6 
5 Samples ... 6 
6 Analysis steps ... 6 
7 Calculation of analysis results ... 8 
8 Precision ... 8 
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 15 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 15. Determination of fluoride content –
Ion selective method
1 Scope
This Part of GB/T 11064 specifies the determination method of fluoride content in
lithium carbonate.
This Part applies to the determination of fluoride content in lithium carbonate. The
determination range is 0.0005% ~ 0.10%.
2 Method summary
The sample is decomposed with nitric acid; use sodium citrate - nitrate solution as
ionic strength adjustment solution; at the condition that the pH value is 7.0, use
fluoride ion selective electrode to determine the fluorine content.
3 Reagents
Unless otherwise indicated, all reagents used in this Part are analytical reagent, the
water used is double-deionized water.
3.1 Nitric acid (1 + 3), guarantee reagent.
3.2 Sulfuric acid (1 + 1), guarantee reagent.
3.3 Sulfuric acid (9 + 95), guarantee reagent.
3.4 Sodium hydroxide solution (40g/L).
3.5 Sodium citrate - nitrate solution. Weigh 294g of sodium citrate dihydrate and 20g
of potassium nitrate; place in a 500mL beaker; add water to dissolve; transfer to a
1000mL volumetric flask; dilute with water to the mark; mix well.
3.6 P-nitrophenol indicator (1g/L).
3.7 Fluorine standard stock solution. Weigh 2.210g of sodium fluoride that has been
7 Calculation of analysis results
Fluorine content is calculated in mass fraction w(F-), expressed in %, according to
equation (1).
Where.
V1 - The volume of the fluorine-containing standard solution B (3.9) in the test
solution, in milliliters (mL);
V0 - The volume of the fluorine-containing standard solution B (3.9) in the blank
solution, in milliliters (mL);
V - The total volume of the test solution, in milliliters (mL);
V2 - The volume of the pipette test solution, in milliliters (mL).
m - The mass of the sample, in grams (g);
5 - The mass concentration of fluorine standard solution B (3.9), in micrograms per
milliliter (μg/mL).
The result shall be expressed to two decimal places. Those less than 0.1% shall be
expressed to three decimal places, and those less than 0.01% shall be expressed to
four 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 2, adopts linear
interpolation or epitaxy method to obtain.
Table 2
w(F-)/% 0.0013 0.052 0.10
r/% 0.0005 0.005 0.02
8.2 Allowable difference
The difference of analysis results among laboratories shall not be more than the
allowable difference in Table 3.
Table 3
Mass fraction of fluoride/% Allowable difference/%
0.0005 ~ 0.0010 0.0004
>0.0010 ~ 0.0050 0.0008
>0.0050 ~ 0.010 0.0020
>0.010 ~ 0.050 0.005
>0.050 ~ 0.075 0.008
>0.075 ~ 0.10 0.012
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;
- Determination date.