GB/T 3257.16-1999 Chemical analysis methods for bauxite ores - Determination of gallium trioxide content by rhodamine B extraction spectrophotometry
Some standard content:
ICS73.060
National Standard of the People's Republic of China
GB/T3257.16--1999
Methods for chemical analysis of bauxite--Determination of gallium oxide concentration-Rhodamine B-extraction photometric Method Issued on August 30, 1999
Implemented on April 1, 2000
Issued by the State Administration of Quality and Technical Supervision
GB/T3257.16—1999
This standard is prepared in accordance with the relevant provisions of GB/T1.1-1993 "Guidelines for Standardization Work Unit 1: Rules for Drafting and Presentation of Standards Part 1: Basic Provisions for Standardization" and GB/T1.4-1988 "Guidelines for Standardization Work Provisions for Chemical Analysis Method Standards Preparation".
This standard is a revision of the analysis method based on the original GB/T3257.16-1982, and its content is basically unchanged. From the date of entry into force, this standard will replace GB/T3257.16-1982. Appendix A is the appendix of the standard.
This standard is proposed by the State Bureau of Nonferrous Metals Industry. This standard is under the jurisdiction of the China Nonferrous Metals Industry Standard Metrology and Quality Research Institute. This standard was drafted by China Nonferrous Metals Industry Standard Metrology and Quality Research Institute and Zhengzhou Light Metal Research Institute. The drafting units of this standard are: Shanxi Aluminum Factory Research Institute and Guangxi Metallurgical Geology Research Institute. The main drafters of this standard are: Huang Anping, He Yuqing, Li Desheng, Liu Liangcheng, Guo Danqi, Wu Jingru and Luo Zhaosi. 1 Scope
National Standard of the People's Republic of China
Chemical analysis method of bauxite
Rhodamine B-extraction photometric method
Determination of gallium trioxide concentration
Methods for chemical analysis of bauxite-Determination of gallium oxide concentration-Rhodamine B-extraction photometric method This standard specifies the method for determining the gallium trioxide content in bauxite. GB/T3257.16-1999
Replaces GB/T3257.16--1982
This standard applies to the determination of gallium trioxide content in bauxite ore, with a determination range of 0.002% to 0.050%. 2 Method Summary
The sample is in a 5.5 mol/L hydrochloric acid medium, and gallium chloride is extracted with toluene-methyl isobutyl ketone solvent. The latter forms a colored complex with rhodamine B, and the absorbance of the color solution is measured at a wavelength of 555 nm. The interference of trivalent iron is eliminated by reduction with titanium trichloride. 3 Reagents
3.1 Sodium hydroxide.
3.2 Sodium peroxide.
3.3 Hydrochloric acid (p=1.19 g/mL).
3.4 Hydrochloric acid (5.5 mol/L).
3.5 Titanium trichloride (150 g/L).
3.6 Rhodamine B solution (5g/L): Dissolve 1.00g of Rhodamine B in hydrochloric acid (3.4) and transfer to a 200mL volumetric flask, dilute to scale with hydrochloric acid (3.4), and shake well.
3.7 Toluene-methyl isobutyl ketone mixed solvent: Mix 6 parts of toluene with 3.5 parts of methyl isobutyl ketone. 3.8 Gallium trioxide standard stock solution:
Weigh 0.1000g of gallium trioxide (spectrally pure) in a 250mL beaker, add 100mL of hydrochloric acid (3.4), place in a water bath and heat to dissolve, remove, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to scale with hydrochloric acid (3.4), and shake well. This solution contains 0.1mg of gallium trioxide per milliliter.
3.9 Gallium trioxide standard solution:
Take 10.00mL of the above solution (3.8) into a 1000mL volumetric flask, dilute to the mark with dilute hydrochloric acid (3.4), and shake well. This solution contains 0.001mg gallium trioxide per milliliter.
Approved by the State Administration of Quality and Technical Supervision on August 30, 1999 and implemented on April 1, 2000
4 Instruments
Spectrophotometer.
5 Sample
5.1 The sample should pass through a 74um sieve.
GB/T3257.16—1999
5.2 The sample should be dried at 105°C ± 5°C for 2h in advance, placed in a desiccator, and cooled to room temperature. 6 Analysis steps
6.1 Number of measurements
The same sample should be measured three times independently and the average value should be taken. 6.2 Sample quantity
Weigh 0.25g of sample, accurate to 0.0001g. 6.3 Blank test
Carry out a blank test with the sample.
6.4 Determination
6.4.1Put the sample (6.2) into a 25mL silver crucible, add 2g of sodium hydroxide (3.1), heat it on an electric furnace to melt it, take it out and add 0.5g of sodium peroxide (3.2), put it in a high-temperature furnace, melt it at 750℃ for 15min, take it out, cool it slightly, put it in a 250mL beaker, add 30mL of hot water, and after the melt falls off, wash out the crucible with 2 drops of hydrochloric acid (3.4) and hot water, add hydrochloric acid (3.3) dropwise while stirring until the hydroxide precipitate is completely dissolved, add 46mL of hydrochloric acid (3.3), cool to room temperature, transfer it to a 100mL volumetric flask, dilute to the scale with water, and shake well. 6.4.2 Take 5.00mL or 10.00mL of the above solution (6.4.1) and place it in a 60mL separatory funnel. 6.4.3 Add 0.5mL of titanium trichloride solution (3.5), shake, and place for 35 minutes. Add 10.00mL of toluene-methyl isobutyl ketone mixed solvent (3.7), shake for 1 minute, and discard the aqueous phase after separation. Add 5mL of hydrochloric acid (3.4) and 0.5mL of titanium trichloride solution (3.5), shake for 30 minutes, and discard the aqueous phase. Add 5mL of hydrochloric acid (3.4), shake for 30 minutes, and discard the aqueous phase. Add 10mL of hydrochloric acid (3.4), 0.5mL of titanium trichloride solution (3.5) and 1.00mL of rhodamine B solution (3.6) to the organic phase, shake for 1 minute, and discard the aqueous phase after separation. Let the organic phase stand for 30 minutes and aspirate the solution with a dry pipette.
6.4.4 Use 1 cm of absorbent to measure the absorbance at 555 nm wavelength in the spectrophotometer, taking the blank sample as reference, and find the corresponding gallium trioxide content from the working curve. Note: When taking 5.00 mL of solution, 5 mL of hydrochloric acid (3.4) should be added. 7 Drawing of calibration curve
Take 0, 1.00, 2.00, 3.00, 4.00, 5.00 mL of gallium trioxide standard solution (3.9), place them in a group of 60 mL separating funnels, add 10.0, 9.0, 8.0, 7.0, 6.0, 5.0 mL of hydrochloric acid (3.4) respectively, and follow the analysis steps (6.4.3) to measure the absorbance and draw the calibration curve.
8 Expression of analysis results
Calculate the percentage of gallium trioxide according to the following formula: mo×V,/. × 100
Ga203（%）=
Wherein: m1--the amount of trioxide found on the calibration curve, g; V. Total volume of test solution, mL;
V,——the volume of test solution taken, mL;
mo—the mass of the test material, g.
Allowable difference
GB/T3257.16—1999
The difference between the analysis results of laboratories shall not be greater than the allowable difference listed in Table 1. Table 1
Ga2O3 content
0.002 0~0.005 0
>0.005 0~0.010
>0.010~0.050
Allowance
A1 Method Summary
GB/T3257.16-1999
Appendix A
(Standard Appendix)
Electrothermal graphite flame atomic absorption spectrometry for the determination of gallium trioxide content The sample is melted and decomposed with sodium hydroxide and sodium peroxide, and the gallium is atomized in an electrothermal graphite tube furnace in a nitric acid medium using a wavelength of 287.4nm. The determination range is 0.001% to 0.010%. Aluminum has a sensitizing effect on the determination of gallium. By adding a constant amount of aluminum to the standard series and adding aluminum to the sample to make it equal to the amount of aluminum in the standard, the interference of aluminum on gallium can be eliminated and the determination sensitivity can be improved. A2 Reagent
A2.1 Sodium hydroxide.
A2.2 Nitric acid (1+1).
A2.3 Sodium hydroxide solution (100g/L). A2.4 Aluminum solution: Weigh 1.324g of aluminum sheet (99.99% should not contain gallium), dissolve in 100mL sodium hydroxide solution (A2.3), transfer to a 100mL volumetric flask, this solution contains 25mg aluminum oxide per milliliter. A2.5 Sodium hydroxide solution (20g/L).
A2.6 Gallium trioxide standard solution:
A2.6.1 Weigh 0.0500g gallium trioxide (spectrally pure) in a 100mL beaker, add 20mL aqua regia, heat to dissolve, evaporate to dryness, then evaporate to dryness twice with 10mL nitric acid, add 5mL nitric acid, heat to dissolve the salt, transfer to a 500mL volumetric flask, dilute to scale with water, and shake well. This solution contains 0.1mg gallium trioxide per milliliter. A2.6.2 Take 5.00 mL of the above solution (A2.6.1) and put it into a 500 mL volumetric flask, add 5 mL of nitric acid, and dilute to the mark with water. This solution contains 0.001 mg of gallium trioxide per mL. A3 Apparatus
Atomic absorption spectrophotometer, with gallium hollow cathode lamp, graphite tube furnace. The working conditions of the atomic absorption spectrophotometer are shown in Table A1 and Table A2. Table A1 Measurement conditions
Slit unit
Lamp current
Drying current 30A, temperature about 100°C. Ashing current 100A, temperature about 680～700°C. Recorder input signal
Table A2 Atomization conditions
Atomization
Atomization ash current 280A, temperature about 2400～2500°C. Use a cup-type atomizer.
Range extension
Sheath argon flow
Sampling volume
Carrier argon flow
A4 Sample
A4.1 The sample should pass through a 74μm sieve.
GB/T3257.16—1999
A4.2 Before analysis, it should be dried at 105-110℃ for 2h, placed in a desiccator, and cooled to room temperature. A5 Analysis steps
A5.1 Determination quantity
The same sample should be measured three times independently and the average value should be taken. A5.2 Sample quantity
Weigh 0.1g sample, accurate to 0.0001g. A5.3. Blank test
Carry out a blank test along with the sample.
A5.4 Determination
Put the sample into a silver crucible pre-filled with 2.0g sodium hydroxide (A2.1), add 0.1g sodium peroxide, heat it on an electric furnace to melt it, move it into a high-temperature furnace, melt it at 750℃ for 15min, take out the crucible, and cool it. Put the crucible into a 200mL beaker, soak it with 30mL boiling water, wash it and take out the crucible. Transfer the solution and insoluble matter into a 100mL volumetric flask, dilute it to the scale with water, and mix it. A5.5 Dry filter it into a 100mL dry small plastic bottle. A5.6 Take 25mL of the filtrate into a 100mL beaker and add high-purity aluminum solution (A2.4). Note: According to the aluminum content in each sample, add a calculated amount of aluminum solution (A2.4) to make the total aluminum oxide concentration in the solution 2mg/mL. A5.7 Add nitric acid (A2.2) dropwise until the solution is neutral (indicated by pH paper), then add 0.5 mL in excess. Heat and concentrate the solution to about 20 mL, and cool.
A5.8 Transfer the solution into a 25 mL volumetric flask, dilute to the mark with water, and shake well. Measure the peak height on an atomic absorption spectrophotometer, draw a calibration curve at the same time, and find the corresponding gallium trioxide amount from the calibration curve. A6 Drawing of the calibration curve
Take 0, 0.50, 1.00, 1.50, 2.00, and 2.50 mL of gallium trioxide solution (A2.6.2) in a group of 100 mL beakers pre-filled with 25 mL of sodium hydroxide solution (A2.5) and 2.00 mL of aluminum solution (A2.4). The following analysis steps A5.7 and A5.8 are used for determination. Draw a calibration curve with the gallium trioxide content and the absorption peak height as the horizontal axis and the vertical axis, respectively. A7 Expression of analysis results
Calculate the percentage of gallium trioxide according to the following formula: Ga0(%) = (c - co)V × 10-6
Wherein: c—concentration of gallium trioxide obtained from the calibration curve, μg/mL; —amount of gallium trioxide contained in the blank test solution obtained from the calibration curve, ug; CowwW.bzxz.Net
V-—volume of the solution to be tested, mL;
mass of the sample equivalent to the solution taken, g. A8 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table A3. 5
Gallium trioxide content
0.0010~0.0020
>0.0020~0.0050
>0.0050~0.010
GB/T 3257.16-1999
Allowable Difference
National Standard of the People's Republic of China
Chemical Analysis Method for Bauxite Ore
Rhodamine B Extraction Spectrophotometry
Determination of Gallium Trioxide Content
GB/T3257.16—1999
Published by China Standards Press
No. 16, Sanlihebei Street, Fuxingmenwai, Beijing
Postal Code: 100045
Tel: 68522112
China Standards Press Printed by Qinhuangdao Printing House, Xinhua Bookstore, Beijing Distribution Office, Xinhua Bookstores in all regions. Reproduction is prohibited.
Copyright reserved
Format: 880×12301/16
First edition in February 2000
Printing sheet: 3/4
Number of words: 12,000
First printing in February 2000
Print run: 1-1000
Book number: 155066·1-16442
Price: RMB 8.00
Heading: 398-226 Take 25mL of the filtrate in a 100mL beaker and add high-purity aluminum solution (A2.4). Note: According to the aluminum content in each sample, add the calculated amount of aluminum solution (A2.4) to make the total aluminum oxide concentration in the solution 2mg/mL. A5.7 Add nitric acid (A2.2) dropwise until the solution is neutral (indicated by pH test paper), then add 0.5mL in excess. Heat and concentrate the solution to about 20mL and cool.
A5.8 Transfer the solution to a 25mL volumetric flask, dilute to the mark with water, and shake well. Measure the peak height on an atomic absorption spectrophotometer and draw a calibration curve at the same time. Find the corresponding gallium trioxide amount from the calibration curve. A6 Drawing of calibration curve
Put 0, 0.50, 1.00, 1.50, 2.00, 2.50mL of gallium trioxide solution (A2.6.2) in a set of 100mL beakers pre-filled with 25mL of sodium hydroxide solution (A2.5) and 2.00mL of aluminum solution (A2.4). Perform the following analysis according to steps A5.7 and A5.8. Draw the calibration curve with gallium trioxide content and absorption peak height as the horizontal and vertical axes, respectively. A7 Expression of analysis results
Calculate the percentage of gallium trioxide according to the following formula: Ga0(%) = (c - co)V × 10-6
Wherein: c—concentration of gallium trioxide obtained from the calibration curve, μg/mL; —amount of gallium trioxide contained in the blank test solution obtained from the calibration curve, ug; Co
V-—volume of the solution to be tested, mL;
mass of the sample equivalent to the solution taken, g. A8 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table A3. 5
Gallium trioxide content
0.0010~0.0020
>0.0020~0.0050
>0.0050~0.010
GB/T 3257.16-1999
Allowable Difference
National Standard of the People's Republic of China
Chemical Analysis Method for Bauxite Ore
Rhodamine B Extraction Spectrophotometry
Determination of Gallium Trioxide Content
GB/T3257.16—1999
Published by China Standards Press
No. 16, Sanlihebei Street, Fuxingmenwai, Beijing
Postal Code: 100045
Tel: 68522112
China Standards Press Printed by Qinhuangdao Printing House, Xinhua Bookstore, Beijing Distribution Office, Xinhua Bookstores in all regions. Reproduction is prohibited.
Copyright reserved
Format: 880×12301/16
First edition in February 2000
Printing sheet: 3/4
Number of words: 12,000
First printing in February 2000
Print run: 1-1000
Book number: 155066·1-16442
Price: RMB 8.00
Heading: 398-226 Take 25mL of the filtrate in a 100mL beaker and add high-purity aluminum solution (A2.4). Note: According to the aluminum content in each sample, add the calculated amount of aluminum solution (A2.4) to make the total aluminum oxide concentration in the solution 2mg/mL. A5.7 Add nitric acid (A2.2) dropwise until the solution is neutral (indicated by pH test paper), then add 0.5mL in excess. Heat and concentrate the solution to about 20mL and cool.
A5.8 Transfer the solution to a 25mL volumetric flask, dilute to the mark with water, and shake well. Measure the peak height on an atomic absorption spectrophotometer and draw a calibration curve at the same time. Find the corresponding gallium trioxide amount from the calibration curve. A6 Drawing of calibration curve
Put 0, 0.50, 1.00, 1.50, 2.00, 2.50mL of gallium trioxide solution (A2.6.2) in a set of 100mL beakers pre-filled with 25mL of sodium hydroxide solution (A2.5) and 2.00mL of aluminum solution (A2.4). Perform the following analysis according to steps A5.7 and A5.8. Draw the calibration curve with gallium trioxide content and absorption peak height as the horizontal and vertical axes, respectively. A7 Expression of analysis results
Calculate the percentage of gallium trioxide according to the following formula: Ga0(%) = (c - co)V × 10-6
Wherein: c—concentration of gallium trioxide obtained from the calibration curve, μg/mL; —amount of gallium trioxide contained in the blank test solution obtained from the calibration curve, ug; Co
V-—volume of the solution to be tested, mL;
mass of the sample equivalent to the solution taken, g. A8 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table A3. 5
Gallium trioxide content
0.0010~0.0020
>0.0020~0.0050
>0.0050~0.010
GB/T 3257.16-1999
Allowable Difference
National Standard of the People's Republic of China
Chemical Analysis Method for Bauxite Ore
Rhodamine B Extraction Spectrophotometry
Determination of Gallium Trioxide Content
GB/T3257.16—1999
Published by China Standards Press
No. 16, Sanlihebei Street, Fuxingmenwai, Beijing
Postal Code: 100045
Tel: 68522112
China Standards Press Printed by Qinhuangdao Printing House, Xinhua Bookstore, Beijing Distribution Office, Xinhua Bookstores in all regions. Reproduction is prohibited.
Copyright reserved
Format: 880×12301/16
First edition in February 2000
Printing sheet: 3/4
Number of words: 12,000
First printing in February 2000
Print run: 1-1000
Book number: 155066·1-16442
Price: RMB 8.00
Heading: 398-22
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