GB/T 15076.6-1994 Chemical analysis method of tantalum and niobium - Determination of silicon content in tantalum
Some standard content:
National Standard of the People's Republic of China
Chemical analysis method of niobium
Determination of silicon content in tantalum
Methods for chemical analysis of tantalum and niobium-Determination of silicon content in tantalumGB/T 15076.6-94
Part I Method 1 Anion exchange separation Silicon molybdenum blue spectrophotometry 1 Subject content and scope of application
This standard specifies the method for the determination of silicon content in tantalum. This standard is applicable to the determination of silicon content in molybdenum and also to the determination of silicon content in its hydroxide. Determination range: 0.0005%~～0.07%.
2 Reference standards
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB1467 General principles and general provisions for chemical analysis methods for metallurgical products GB7729 General principles for spectrophotometric methods for chemical analysis of metallurgical products 3 Principles of the method
The sample is dissolved with hydrofluoric acid and nitric acid, and the test solution containing nitric acid and hydrofluoric acid (Lc(HNO,)=0.35mol/1.,c(HF)=1.1mol/L) is separated by anion exchange. The fluoride ions are masked with boric acid, and silicon and ammonium molybdate generate silicomolybdenum heteropoly acid at pH 1-2. In sulfuric acid solution (c(H,SO,)=0.6mol/L), 1-nitro-2-phenol-4-sulfonic acid is used to reduce it to silicomolybdenum blue, and its absorbance is measured at a wavelength of 800nm on a spectrophotometer.
4 Reagents
Pure water that has undergone secondary ion exchange and sub-boiling distillation is used for the preparation of reagents and tests. 4.1
Boric acid, extra pure.
4.2Sodium nitrate solution (50g/L), premium grade. 4.3
Nitric acid (1+1), extra pure.
Oxyfluoric acid (1+1), extra pure.
4.5 Nitric acid (1+25, extra pure.
4.6 Ammonium molybdate solution: weigh 10g ammonium molybdate [(NH,)Mo,O24·4H20, extra pure] in a 200ml beaker, add 100ml water, heat to dissolve, add 0.5mL ammonia nitrogen water (p0.90g/mL, extra pure) and mix well. Store in a plastic bottle. 4.7 Sulfuric acid (1+1).
4.8 Oxalic acid solution (50g/L).
4.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L) Approved by the State Administration of Technical Supervision on May 9, 1994 502
Implementation on December 1, 1994
GB/T 1 5076. 6--94
L, prepared when needed), dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when needed), mix well. This solution is valid for 1 week. 4.10 Ammonium nitrate-ammonium fluoride-ammonium bifluoride solution: weigh 240g ammonium nitrate, 18g ammonium fluoride, and 14g ammonium bifluoride in a 1000mL plastic bottle, add water to dissolve and dilute to 1000mL, mix well. 4.11 Silicon standard storage solution: weigh 0.2140g of high-purity silicon dioxide that has been calcined at 1000℃ for 1h and cooled to room temperature in a desiccator in a 30mL platinum crucible, add 2g Anhydrous sodium carbonate (extra pure) is melted on a blowtorch until transparent, and the melting is continued for 2 minutes, and then cooled. Place the platinum in a 250mL plastic beaker, add 100mL boiling water to soak, stir until the frit is completely dissolved, wash out the crucible with hot water, cool, transfer to a 1000mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 100μg silicon in 1mL. 4.12 Silicon standard solution: Transfer 10.00mL of silicon standard storage solution (4.11) to a 100mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 5 Instruments and devices
5.1 Spectrophotometer.
5.2 Ion exchange column.
5.2.1 Preparation of ion exchange column: Use a polyethylene tube with an inner diameter of 8-10 mm and a length of 220-250 mm. Pull one end into a capillary tube of 600-700 mm and make the other end into a funnel shape to make an ion exchange column with a capacity of 13-15 ml. Fill the column with polyethylene filaments about 8 mm thick near one end of the capillary tube, and add 7-7.5 mL of slurry-like strong alkaline anion exchange resin ( Styrene type, strong base 200×8) is injected into the exchange column, and bubbles are exhausted. The flow rate is adjusted to 1.0～1.5mL/min by controlling the capillary outlet height. 5.2.2 Treatment and regeneration of ion exchange column: First, soak the ion exchange column with hydrofluoric acid (4.4) for 24h, and then rinse the exchange column with 40mL hydrofluoric acid (1+4) and 30mL nitric acid (4.5) in sequence. Use 20mL aqueous solution containing 2mL hydrofluoric acid (4.4) and 1mL nitric acid (4.3) to check whether the column is qualified according to 6.4.2~~6.4.4. The difference in absorbance between the test solution and the reagent blank that does not flow through the column and measured with 2cm absorption blood and water as reference should not be greater than 0.012. Otherwise, repeat the elution with hydrofluoric acid (1+4) and nitric acid (4.5) until it is qualified. After use, the ion exchange column is rinsed with 100 mL of ammonium nitrate-ammonium fluoride-ammonium bifluoride (4.10), and then rinsed with 50 mL of nitric acid (4.5), and can be reused. 6 Analysis steps
6.1 Determination quantity
Weigh two samples, measure independently, and take the average value. 6.2 Samples
Weigh the samples according to Table 1, accurate to 0.0001g. Table 1
Silicon content
0. 0005~~0. 0020
>0. 0020~~0. 0100
>0. 010~~0. 025
>0. 025~～0. 070
6.3 Blank test
Carry out a blank test along with the sample.
6.4 Determination
Absorption dish
[. Draw curve numbers
6.4.1 Place the sample (6.2) in a 60mL plastic bottle, add 1mL sodium nitrate solution (4.2), 1mL nitric acid (4.3), and 3mL hydrofluoric acid (4.4), cover the bottle cap, place it in a water bath and heat until the sample is completely dissolved, remove it, and cool it. Add 15mL water and mix it. 6.4.2 Pass the test solution through the treated ion exchange column (5.2), wash the plastic bottle with 30mL nitric acid (4.5) three times and rinse the exchange 503
column, and collect the effluent in a 120mL plastic bottle. GB/T 15076.6—94
6.4.3 Add 3g of boric acid (4.1), place in a boiling water bath and heat for 10min, mix, continue heating for 5min, take out, immediately add 10mL of ammonium molybdate solution (4.6), mix, and place for 10min. Add 5mL of sulfuric acid (4.7), 10ml of oxalic acid solution (4.8), and 2mL of reducing agent solution (4.9) in sequence, mix, and cool. Transfer to a 100mL volumetric flask, dilute to the mark with water, and mix. Place for 15min. 6.4.4 Transfer part of the solution to the corresponding absorption dish according to Table 1, and measure its absorbance at a wavelength of 800nm on a spectrophotometer with water as a reference.
6.4.5 Subtract the absorbance of the blank solution accompanying the sample, and find the silicon content from the corresponding working curve according to Table 1. 6.5 Drawing of working curve
6.5.1 Working curve 1
6.5.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70, 1.00 mL of silicon standard solution (4.12) into a set of plastic bottles. 6.5.1.2 Add 3.3 mL of nitric acid (4.3) and 3 mL of hydrofluoric acid (4.4), and add water to 50 mL. The following operations are carried out according to 6.4.3 and 6.4.4. 6.5.1.3 Subtract the absorbance of the reagent blank, and draw the working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 6.5.2 Working curve II
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00mL of silicon standard solution (4.12) into a group of 120mL plastic bottles, and operate as in 6.5.1.2 and 6.5.1.3. 7 Calculation and expression of analysis results
Calculate the percentage of silicon content according to the following formula:
Si(%)=
Where; mi-
Silicon amount found from the working curve, ug; mass of the sample, g.
8 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Silicon content
0. 0005 ~ 0. 0010
>0. 0010~~0.0025
>0. 0025~0. 0070
>0.0070～0.0150
>0.015~~0.040
>0. 040~~0. 070
Tolerance
Part 2 Method 4-Methyl-pentanone-［2] Extraction and separation of silicon molybdenum blue spectrophotometry 9 Subject content and scope of application
This standard specifies the method for the determination of silicon content in saw. %
This standard is applicable to the determination of silicon content in saw and also to the determination of silicon content in its hydroxide. Determination range: 0.0005%~0.07%.
10 Reference standards
GB/T 15076.6--94
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis method standards GB1467 General principles and general provisions for chemical analysis method standards for metallurgical products GB7729 General rules for spectrophotometric methods for chemical analysis of metallurgical products 11 Principle of the method
The sample is dissolved in hydrofluoric acid and nitric acid. In a test solution containing nitric acid and hydrofluoric acid (c(HNO,) = 5 mol/L, c(HF) 9 mol/L), the main body was extracted and separated with 4-methyl-pentanone-(2). The fluoride ions were masked with boric acid, and silicomolybdic heteropoly acid was generated with ammonium molybdate at pH 1-2. In a sulfuric acid solution [c(HzSO,) = 0.6 mol/L], 1-amino-2-naphthophenol-4-sulfonic acid was used to reduce silicomolybdenum blue, and its absorbance was measured at a wavelength of 800 nm on a spectrophotometer.
12 Reagents
Pure water that had been subjected to secondary exchange and sub-boiling distillation was used for the preparation of reagents and experiments. 12.1 Boric acid, extra pure.
12.2 Nitric acid (p1.42 g/mL), extra pure. 12.3 Hydrofluoric acid (el.14 g/mL), extra pure. 12.4 4-Methyl-pentanone-23 (abbreviated as MIBK): In a 500mL plastic separatory funnel, add 20ml water, 40ml nitric acid (12.2), and 40ml hydrofluoric acid (12.3), and mix well. Add 200ml MIBK, shake for 2min, and let stand to separate. Remove the aqueous phase and put the organic phase in a plastic bottle. Treat when needed.
12.5 Sodium nitrate solution (50g/L), high-grade purity. 12.6 Ammonium molybdate solution: Weigh 10g ammonium molybdate [(NH,)Mo,Oz4·4H,0, extra pure] in a 200mL beaker, add 100ml water, heat to dissolve, add 0.5ml nitrogen water (e0.90g/ml, extra pure), and mix well. In a plastic bottle. 12.7 Sulfuric acid (1+1).
12.8 Oxalic acid Solution (50g/L).
12.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L, prepared when needed) to dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when needed), and mix well. This solution is valid for one week.
12.10 Silicon standard storage solution: weigh 0.2140g of high-purity silica that has been calcined at 1000℃ for 1h and placed in a desiccator to cool to room temperature, add 2g anhydrous sodium carbonate (extra pure) to 30ml platinum sulfide, melt on a blowtorch until transparent, continue melting for 2min, and cool. Place the platinum crucible in a 250mL plastic beaker, add 100mL boiling water to soak, and stir until The melt is completely dissolved, washed out with hot water, cooled, transferred to a 1000mL volumetric flask, diluted to the mark with water, mixed, and stored in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: Transfer 10.00mL of silicon standard storage solution (12.10) to a 100mL volumetric flask, dilute to the mark with water, mix, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary with a length of 100-150mm on the mouth of a 60mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extraction, medical gloves should be worn to prevent hydrofluoric acid burns. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the samples according to Table 3, accurate to 0.0001g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test along with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove and cool. 14.5.2 Absorb the test solution into a plastic extraction bottle (13.2), then absorb 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, place the aqueous phase in a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g of boric acid to a plastic bottle, place it in a boiling water bath and heat to dissolve for 10 minutes, mix well, continue heating for 5 minutes, take it out, immediately add 12mL of ammonium molybdate solution (12.6), mix well, and let it stand for 10 minutes. Add 5mL of sulfuric acid (12.7), 10ml of oxalic acid solution (12.8), and 2ml of reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the scale with water, mix well, and let it stand for 15 minutes. 14.5.4 Transfer part of the solution to the corresponding absorption dish according to Table 3, use water as a reference, and measure its absorbance at a wavelength of 800nm on a spectrophotometer.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70, 1.00 mL of silicon standard solution (12.11) into a 120 mL plastic bottle. 14.6.1.2 Add 2 mL of nitric acid (12.2) and 2 mL of hydrofluoric acid (12.3), and add water to 50 mL. The following procedures are as in 6.5.3 to 6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw the working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon content according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506www.bzxz.net
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (3) -78 "Determination of silicon content in button (silicon molybdenum blue absorption photometry)" will be invalid.040
>0. 040~~0. 070
Tolerance
Part 2 Method 4-Methyl-pentanone-［2] Extraction and separation of silicon molybdenum blue spectrophotometry 9 Subject content and scope of application
This standard specifies the method for determining the silicon content in saw. %
This standard is applicable to the determination of silicon content in saws and also to the determination of silicon content in its hydroxide. Determination range: 0.0005%~0.07%.
10 Reference standards
GB/T 15076.6--94
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB1467 General principles and general provisions for chemical analysis methods of metallurgical products GB7729 General principles for spectrophotometric methods for chemical analysis of metallurgical products 11 Principle of the method
The sample is dissolved with hydrofluoric acid and nitric acid. In a test solution containing nitric acid and hydrofluoric acid (c(HNO,) = 5 mol/L, c(HF) 9 mol/L), the main body was extracted and separated with 4-methyl-pentanone-(2). The fluoride ions were masked with boric acid, and silicomolybdic heteropoly acid was generated with ammonium molybdate at pH 1-2. In a sulfuric acid solution [c(HzSO,) = 0.6 mol/L], 1-amino-2-naphthophenol-4-sulfonic acid was used to reduce silicomolybdenum blue, and its absorbance was measured at a wavelength of 800 nm on a spectrophotometer.
12 Reagents
Pure water that had been subjected to secondary exchange and sub-boiling distillation was used for the preparation of reagents and experiments. 12.1 Boric acid, extra pure.
12.2 Nitric acid (p1.42 g/mL), extra pure. 12.3 Hydrofluoric acid (el.14 g/mL), extra pure. 12.4 4-Methyl-pentanone-23 (abbreviated as MIBK): In a 500mL plastic separatory funnel, add 20ml water, 40ml nitric acid (12.2), and 40ml hydrofluoric acid (12.3), and mix well. Add 200ml MIBK, shake for 2min, and let stand to separate. Remove the aqueous phase and put the organic phase in a plastic bottle. Treat when needed.
12.5 Sodium nitrate solution (50g/L), high-grade purity. 12.6 Ammonium molybdate solution: Weigh 10g ammonium molybdate [(NH,)Mo,Oz4·4H,0, extra pure] in a 200mL beaker, add 100ml water, heat to dissolve, add 0.5ml nitrogen water (e0.90g/ml, extra pure), and mix well. In a plastic bottle. 12.7 Sulfuric acid (1+1).
12.8 Oxalic acid Solution (50g/L).
12.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L, prepared when needed) to dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when needed), and mix well. This solution is valid for one week.
12.10 Silicon standard storage solution: weigh 0.2140g of high-purity silica that has been calcined at 1000℃ for 1h and placed in a desiccator to cool to room temperature, add 2g anhydrous sodium carbonate (extra pure) to 30ml platinum sulfide, melt on a blowtorch until transparent, continue melting for 2min, and cool. Place the platinum crucible in a 250mL plastic beaker, add 100mL boiling water to soak, and stir until The melt is completely dissolved, washed out with hot water, cooled, transferred to a 1000mL volumetric flask, diluted to the mark with water, mixed, and stored in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: Transfer 10.00mL of silicon standard storage solution (12.10) to a 100mL volumetric flask, dilute to the mark with water, mix, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary with a length of 100-150mm on the mouth of a 60mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extraction, medical gloves should be worn to prevent hydrofluoric acid burns. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the samples according to Table 3, accurate to 0.0001g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test along with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove and cool. 14.5.2 Absorb the test solution into a plastic extraction bottle (13.2), then absorb 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, place the aqueous phase in a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g of boric acid to a plastic bottle, place it in a boiling water bath and heat to dissolve for 10 minutes, mix well, continue heating for 5 minutes, take it out, immediately add 12mL of ammonium molybdate solution (12.6), mix well, and let it stand for 10 minutes. Add 5mL of sulfuric acid (12.7), 10ml of oxalic acid solution (12.8), and 2ml of reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the scale with water, mix well, and let it stand for 15 minutes. 14.5.4 Transfer part of the solution to the corresponding absorption dish according to Table 3, use water as a reference, and measure its absorbance at a wavelength of 800nm on a spectrophotometer.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70, 1.00 mL of silicon standard solution (12.11) into a 120 mL plastic bottle. 14.6.1.2 Add 2 mL of nitric acid (12.2) and 2 mL of hydrofluoric acid (12.3), and add water to 50 mL. The following procedures are as in 6.5.3 to 6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw the working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon content according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (3) -78 "Determination of silicon content in button (silicon molybdenum blue absorption photometry)" will be invalid.040
>0. 040~~0. 070
Tolerance
Part 2 Method 4-Methyl-pentanone-［2] Extraction and separation of silicon molybdenum blue spectrophotometry 9 Subject content and scope of application
This standard specifies the method for determining the silicon content in saw. %
This standard is applicable to the determination of silicon content in saws and also to the determination of silicon content in its hydroxide. Determination range: 0.0005%~0.07%.
10 Reference standards
GB/T 15076.6--94
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB1467 General principles and general provisions for chemical analysis methods of metallurgical products GB7729 General principles for spectrophotometric methods for chemical analysis of metallurgical products 11 Principle of the method
The sample is dissolved with hydrofluoric acid and nitric acid. In a test solution containing nitric acid and hydrofluoric acid (c(HNO,) = 5 mol/L, c(HF) 9 mol/L), the main body was extracted and separated with 4-methyl-pentanone-(2). The fluoride ions were masked with boric acid, and silicomolybdic heteropoly acid was generated with ammonium molybdate at pH 1-2. In a sulfuric acid solution [c(HzSO,) = 0.6 mol/L], 1-amino-2-naphthophenol-4-sulfonic acid was used to reduce silicomolybdenum blue, and its absorbance was measured at a wavelength of 800 nm on a spectrophotometer.
12 Reagents
Pure water that had been subjected to secondary exchange and sub-boiling distillation was used for the preparation of reagents and experiments. 12.1 Boric acid, extra pure.
12.2 Nitric acid (p1.42 g/mL), extra pure. 12.3 Hydrofluoric acid (el.14 g/mL), extra pure. 12.4 4-Methyl-pentanone-23 (abbreviated as MIBK): In a 500mL plastic separatory funnel, add 20ml water, 40ml nitric acid (12.2), and 40ml hydrofluoric acid (12.3), and mix well. Add 200ml MIBK, shake for 2min, and let stand to separate. Remove the aqueous phase and put the organic phase in a plastic bottle. Treat when needed.
12.5 Sodium nitrate solution (50g/L), high-grade purity. 12.6 Ammonium molybdate solution: Weigh 10g ammonium molybdate [(NH,)Mo,Oz4·4H,0, extra pure] in a 200mL beaker, add 100ml water, heat to dissolve, add 0.5ml nitrogen water (e0.90g/ml, extra pure), and mix well. In a plastic bottle. 12.7 Sulfuric acid (1+1).
12.8 Oxalic acid Solution (50g/L).
12.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L, prepared when needed) to dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when needed), and mix well. This solution is valid for one week.
12.10 Silicon standard storage solution: weigh 0.2140g of high-purity silica that has been calcined at 1000℃ for 1h and placed in a desiccator to cool to room temperature, add 2g anhydrous sodium carbonate (extra pure) to 30ml platinum sulfide, melt on a blowtorch until transparent, continue melting for 2min, and cool. Place the platinum crucible in a 250mL plastic beaker, add 100mL boiling water to soak, and stir until The melt is completely dissolved, washed out with hot water, cooled, transferred to a 1000mL volumetric flask, diluted to the mark with water, mixed, and stored in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: Transfer 10.00mL of silicon standard storage solution (12.10) to a 100mL volumetric flask, dilute to the mark with water, mix, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary with a length of 100-150mm on the mouth of a 60mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extraction, medical gloves should be worn to prevent hydrofluoric acid burns. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the samples according to Table 3, accurate to 0.0001g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test along with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove and cool. 14.5.2 Absorb the test solution into a plastic extraction bottle (13.2), then absorb 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, place the aqueous phase in a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g of boric acid to a plastic bottle, place it in a boiling water bath and heat to dissolve for 10 minutes, mix well, continue heating for 5 minutes, take it out, immediately add 12mL of ammonium molybdate solution (12.6), mix well, and let it stand for 10 minutes. Add 5mL of sulfuric acid (12.7), 10ml of oxalic acid solution (12.8), and 2ml of reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the scale with water, mix well, and let it stand for 15 minutes. 14.5.4 Transfer part of the solution to the corresponding absorption dish according to Table 3, use water as a reference, and measure its absorbance at a wavelength of 800nm on a spectrophotometer.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70, 1.00 mL of silicon standard solution (12.11) into a 120 mL plastic bottle. 14.6.1.2 Add 2 mL of nitric acid (12.2) and 2 mL of hydrofluoric acid (12.3), and add water to 50 mL. The following procedures are as in 6.5.3 to 6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw the working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon content according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (3) -78 "Determination of silicon content in button (silicon molybdenum blue absorption photometry)" will be invalid.07%.
10 Reference standards
GB/T 15076.6--94
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis method standards GB1467 General principles and general provisions for chemical analysis method standards for metallurgical products GB7729 General principles for spectrophotometric methods for chemical analysis of metallurgical products 11 Principle of the method
The sample is dissolved in hydrofluoric acid and nitric acid. In a test solution containing nitric acid and hydrofluoric acid (c(HNO,) = 5 mol/L, c(HF) 9 mol/L), the main body was extracted and separated with 4-methyl-pentanone-(2). The fluoride ions were masked with boric acid, and silicomolybdic heteropoly acid was generated with ammonium molybdate at pH 1-2. In a sulfuric acid solution [c(HzSO,) = 0.6 mol/L], 1-amino-2-naphthophenol-4-sulfonic acid was used to reduce silicomolybdenum blue, and its absorbance was measured at a wavelength of 800 nm on a spectrophotometer.
12 Reagents
Pure water that had been subjected to secondary exchange and sub-boiling distillation was used for the preparation of reagents and experiments. 12.1 Boric acid, extra pure.
12.2 Nitric acid (p1.42 g/mL), extra pure. 12.3 Hydrofluoric acid (el.14 g/mL), extra pure. 12.4 4-Methyl-pentanone-23 (abbreviated as MIBK): In a 500mL plastic separatory funnel, add 20ml water, 40ml nitric acid (12.2), and 40ml hydrofluoric acid (12.3), and mix well. Add 200ml MIBK, shake for 2min, and let stand to separate. Remove the aqueous phase and put the organic phase in a plastic bottle. Treat when needed.
12.5 Sodium nitrate solution (50g/L), high-grade purity. 12.6 Ammonium molybdate solution: Weigh 10g ammonium molybdate [(NH,)Mo,Oz4·4H,0, extra pure] in a 200mL beaker, add 100ml water, heat to dissolve, add 0.5ml nitrogen water (e0.90g/ml, extra pure), and mix well. In a plastic bottle. 12.7 Sulfuric acid (1+1).
12.8 Oxalic acid Solution (50g/L).
12.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L, prepared when needed) to dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when needed), and mix well. This solution is valid for one week.
12.10 Silicon standard storage solution: weigh 0.2140g of high-purity silica that has been calcined at 1000℃ for 1h and placed in a desiccator to cool to room temperature, add 2g anhydrous sodium carbonate (extra pure) to 30ml platinum sulfide, melt on a blowtorch until transparent, continue melting for 2min, and cool. Place the platinum crucible in a 250mL plastic beaker, add 100mL boiling water to soak, and stir until The melt is completely dissolved, washed out with hot water, cooled, transferred to a 1000mL volumetric flask, diluted to the mark with water, mixed, and stored in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: Transfer 10.00mL of silicon standard storage solution (12.10) to a 100mL volumetric flask, dilute to the mark with water, mix, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary with a length of 100-150mm on the mouth of a 60mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extraction, medical gloves should be worn to prevent hydrofluoric acid burns. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the samples according to Table 3, accurate to 0.0001g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test along with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove and cool. 14.5.2 Absorb the test solution into a plastic extraction bottle (13.2), then absorb 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, place the aqueous phase in a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g of boric acid to a plastic bottle, place it in a boiling water bath and heat to dissolve for 10 minutes, mix well, continue heating for 5 minutes, take it out, immediately add 12mL of ammonium molybdate solution (12.6), mix well, and let it stand for 10 minutes. Add 5mL of sulfuric acid (12.7), 10ml of oxalic acid solution (12.8), and 2ml of reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the scale with water, mix well, and let it stand for 15 minutes. 14.5.4 Transfer part of the solution to the corresponding absorption dish according to Table 3, use water as a reference, and measure its absorbance at a wavelength of 800nm on a spectrophotometer.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70, 1.00 mL of silicon standard solution (12.11) into a 120 mL plastic bottle. 14.6.1.2 Add 2 mL of nitric acid (12.2) and 2 mL of hydrofluoric acid (12.3), and add water to 50 mL. The following procedures are as in 6.5.3 to 6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw the working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon content according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (3) -78 "Determination of silicon content in button (silicon molybdenum blue absorption photometry)" will be invalid.07%.
10 Reference standards
GB/T 15076.6--94
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis method standards GB1467 General principles and general provisions for chemical analysis method standards for metallurgical products GB7729 General principles for spectrophotometric methods for chemical analysis of metallurgical products 11 Principle of the method
The sample is dissolved in hydrofluoric acid and nitric acid. In a test solution containing nitric acid and hydrofluoric acid (c(HNO,) = 5 mol/L, c(HF) 9 mol/L), the main body was extracted and separated with 4-methyl-pentanone-(2). The fluoride ions were masked with boric acid, and silicomolybdic heteropoly acid was generated with ammonium molybdate at pH 1-2. In a sulfuric acid solution [c(HzSO,) = 0.6 mol/L], 1-amino-2-naphthophenol-4-sulfonic acid was used to reduce silicomolybdenum blue, and its absorbance was measured at a wavelength of 800 nm on a spectrophotometer.
12 Reagents
Pure water that had been subjected to secondary exchange and sub-boiling distillation was used for the preparation of reagents and experiments. 12.1 Boric acid, extra pure.
12.2 Nitric acid (p1.42 g/mL), extra pure. 12.3 Hydrofluoric acid (el.14 g/mL), extra pure. 12.4 4-Methyl-pentanone-23 (abbreviated as MIBK): In a 500mL plastic separatory funnel, add 20ml water, 40ml nitric acid (12.2), and 40ml hydrofluoric acid (12.3), and mix well. Add 200ml MIBK, shake for 2min, and let stand to separate. Remove the aqueous phase and put the organic phase in a plastic bottle. Treat when needed.
12.5 Sodium nitrate solution (50g/L), high-grade purity. 12.6 Ammonium molybdate solution: Weigh 10g ammonium molybdate [(NH,)Mo,Oz4·4H,0, extra pure] in a 200mL beaker, add 100ml water, heat to dissolve, add 0.5ml nitrogen water (e0.90g/ml, extra pure), and mix well. In a plastic bottle. 12.7 Sulfuric acid (1+1).
12.8 Oxalic acid Solution (50g/L).
12.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L, prepared when needed) to dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when needed), and mix well. This solution is valid for one week.
12.10 Silicon standard storage solution: weigh 0.2140g of high-purity silica that has been calcined at 1000℃ for 1h and placed in a desiccator to cool to room temperature, add 2g anhydrous sodium carbonate (extra pure) to 30ml platinum sulfide, melt on a blowtorch until transparent, continue melting for 2min, and cool. Place the platinum crucible in a 250mL plastic beaker, add 100mL boiling water to soak, and stir until The melt is completely dissolved, washed out with hot water, cooled, transferred to a 1000mL volumetric flask, diluted to the mark with water, mixed, and stored in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: Transfer 10.00mL of silicon standard storage solution (12.10) to a 100mL volumetric flask, dilute to the mark with water, mix, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary with a length of 100-150mm on the mouth of a 60mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extraction, medical gloves should be worn to prevent hydrofluoric acid burns. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the samples according to Table 3, accurate to 0.0001g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test along with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove and cool. 14.5.2 Absorb the test solution into a plastic extraction bottle (13.2), then absorb 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, place the aqueous phase in a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g of boric acid to a plastic bottle, place it in a boiling water bath and heat to dissolve for 10 minutes, mix well, continue heating for 5 minutes, take it out, immediately add 12mL of ammonium molybdate solution (12.6), mix well, and let it stand for 10 minutes. Add 5mL of sulfuric acid (12.7), 10ml of oxalic acid solution (12.8), and 2ml of reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the scale with water, mix well, and let it stand for 15 minutes. 14.5.4 Transfer part of the solution to the corresponding absorption dish according to Table 3, use water as a reference, and measure its absorbance at a wavelength of 800nm on a spectrophotometer.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70, 1.00 mL of silicon standard solution (12.11) into a 120 mL plastic bottle. 14.6.1.2 Add 2 mL of nitric acid (12.2) and 2 mL of hydrofluoric acid (12.3), and add water to 50 mL. The following procedures are as in 6.5.3 to 6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw the working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon content according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (3) -78 "Determination of silicon content in button (silicon molybdenum blue absorption photometry)" will be invalid.6mol/L], 1-amino-2-naphthophenol-4-sulfonic acid was reduced to silicon molybdenum blue, and its absorbance was measured at a wavelength of 800nm on a spectrophotometer.
12 Reagents
Pure water that has been exchanged twice and distilled sub-boilingly was used for the preparation of reagents and experiments. 12.1 Boric acid, extra pure.
12.2 Nitric acid (p1.42g/mL), extra pure. 12.3 Hydrofluoric acid (el.14g/mL), extra pure. 12.4 4-Methyl-pentanone-23 (abbreviated as MIBK): In a 500mL plastic separatory funnel, add 20ml water, 40ml nitric acid (12.2), and 40ml hydrofluoric acid (12.3), and mix well. Add 200ml MIBK, shake for 2min, and let stand to separate. Remove the aqueous phase and put the organic phase in a plastic bottle. Dispose when needed.
12.5 Sodium nitrate solution (50g/L), premium grade. 12.6 Ammonium molybdate solution: weigh 10g ammonium molybdate [(NH,)Mo,Oz4·4H,0, extra pure] in a 200mL beaker, add 100mL water, heat to dissolve, add 0.5mL nitrogen water (e0.90g/ml, extra pure), mix well. In a plastic bottle. 12.7 Sulfuric acid (1+1).
12.8 Oxalic acid solution (50g/L).
12.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L, prepared when used) to dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when used), mix well. This solution is valid for one week.
12.10 Silicon standard stock solution: weigh 0.2140g of high-purity silicon dioxide that has been calcined at 1000℃ for 1h and cooled to room temperature in a desiccator, add 2g of anhydrous sodium carbonate (extra pure) to 30ml of platinum alkali, melt on a blowtorch until transparent, continue melting for 2min, and cool. Place the platinum crucible in a 250mL plastic beaker, add 100mL of boiling water to leaching, stir until the frit is completely dissolved, wash out with hot water, cool, transfer to a 1000mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: transfer 10.00mL of silicon standard stock solution (12.10) to a 100mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary tube with a length of 100-150 mm on the mouth of a 60 mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extracting, medical gloves should be worn to prevent burns from hydrofluoric acid. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the sample according to Table 3, accurate to 0.0001 g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove it and cool it. 14.5.2 Pipette the test solution into the plastic extraction bottle (13.2), then aspirate 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, put the aqueous phase into a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g boric acid to the plastic bottle, place it in a boiling water bath and heat to dissolve for 10min, mix well, continue heating for 5min, take it out, immediately add 12mL ammonium molybdate solution (12.6), mix well, and let it stand for 10min. Add 5mL sulfuric acid (12.7), 10mlL oxalic acid solution (12.8), and 2ml reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the mark with water, mix well, and let it stand for 15min. 14.5.4 Transfer part of the solution into the corresponding absorption dish according to Table 3, and measure its absorbance at a wavelength of 800nm on a spectrophotometer with water as the reference.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find out the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70.1.00mL of silicon standard solution (12.11) into a 120mL plastic bottle. 14.6.1.2 Add 2mL nitric acid (12.2) and 2mL hydrofluoric acid (12.3), and add water to 50mL. The following operations are carried out according to 6.5.3~6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw a working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (3) -78 "Determination of silicon content in button (silicon molybdenum blue absorption photometry)" will be invalid.6mol/L], 1-amino-2-naphthophenol-4-sulfonic acid was reduced to silicon molybdenum blue, and its absorbance was measured at a wavelength of 800nm on a spectrophotometer.
12 Reagents
Pure water that has been exchanged twice and distilled sub-boilingly was used for the preparation of reagents and experiments. 12.1 Boric acid, extra pure.
12.2 Nitric acid (p1.42g/mL), extra pure. 12.3 Hydrofluoric acid (el.14g/mL), extra pure. 12.4 4-Methyl-pentanone-23 (abbreviated as MIBK): In a 500mL plastic separatory funnel, add 20ml water, 40ml nitric acid (12.2), and 40ml hydrofluoric acid (12.3), and mix well. Add 200ml MIBK, shake for 2min, and let stand to separate. Remove the aqueous phase and put the organic phase in a plastic bottle. Dispose when needed.
12.5 Sodium nitrate solution (50g/L), premium grade. 12.6 Ammonium molybdate solution: weigh 10g ammonium molybdate [(NH,)Mo,Oz4·4H,0, extra pure] in a 200mL beaker, add 100mL water, heat to dissolve, add 0.5mL nitrogen water (e0.90g/ml, extra pure), mix well. In a plastic bottle. 12.7 Sulfuric acid (1+1).
12.8 Oxalic acid solution (50g/L).
12.9 Reducing agent solution: weigh 0.3g 1-amino-2-naphthol-4-sulfonic acid in a 400mL beaker, add 20mL anhydrous sodium sulfite solution (70g/L, prepared when used) to dissolve, add 180mL anhydrous sodium bisulfite solution (100g/L, prepared when used), mix well. This solution is valid for one week.
12.10 Silicon standard stock solution: weigh 0.2140g of high-purity silicon dioxide that has been calcined at 1000℃ for 1h and cooled to room temperature in a desiccator, add 2g of anhydrous sodium carbonate (extra pure) to 30ml of platinum alkali, melt on a blowtorch until transparent, continue melting for 2min, and cool. Place the platinum crucible in a 250mL plastic beaker, add 100mL of boiling water to leaching, stir until the frit is completely dissolved, wash out with hot water, cool, transfer to a 1000mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: transfer 10.00mL of silicon standard stock solution (12.10) to a 100mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary tube with a length of 100-150 mm on the mouth of a 60 mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extracting, medical gloves should be worn to prevent burns from hydrofluoric acid. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the sample according to Table 3, accurate to 0.0001 g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove it and cool it. 14.5.2 Pipette the test solution into the plastic extraction bottle (13.2), then aspirate 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, put the aqueous phase into a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g boric acid to the plastic bottle, place it in a boiling water bath and heat to dissolve for 10min, mix well, continue heating for 5min, take it out, immediately add 12mL ammonium molybdate solution (12.6), mix well, and let it stand for 10min. Add 5mL sulfuric acid (12.7), 10mlL oxalic acid solution (12.8), and 2ml reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the mark with water, mix well, and let it stand for 15min. 14.5.4 Transfer part of the solution into the corresponding absorption dish according to Table 3, and measure its absorbance at a wavelength of 800nm on a spectrophotometer with water as the reference.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find out the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70.1.00mL of silicon standard solution (12.11) into a 120mL plastic bottle. 14.6.1.2 Add 2mL nitric acid (12.2) and 2mL hydrofluoric acid (12.3), and add water to 50mL. The following operations are carried out according to 6.5.3~6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw a working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (3) -78 "Determination of silicon content in button (silicon molybdenum blue absorption photometry)" will be invalid.2140g of high-purity silicon dioxide that was previously burned at 1000℃ for 1h and placed in a desiccator to cool to room temperature is added to 30ml of platinum, and 2g of anhydrous sodium carbonate (extra pure) is added. It is melted on a blowtorch until transparent, and the melting is continued for 2min, and then cooled. The platinum crucible is placed in a 250mL plastic beaker, and 100mL of boiling water is added for leaching. Stir until the frit is completely dissolved, wash out with hot water, cool, transfer to a 1000mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 100μg silicon in 1ml. 12.11 Silicon standard solution: Transfer 10.00mL of silicon standard stock solution (12.10) to a 100mL volumetric flask, dilute to scale with water, mix well, and store in a plastic bottle. This solution contains 10μg silicon in 1mL. 13 Instruments and devices
13.1 Spectrophotometer.
13.2 Plastic extraction bottle: Weld a plastic capillary with a length of 100-150mm on the mouth of a 60mL plastic bottle. 14 Analysis steps
14.1 Safety measures
When handling the organic phase and extraction, medical gloves should be worn to prevent hydrofluoric acid burns. 14.2 Determination quantity
GB/T15076.6—94
Weigh two samples, measure independently, and take the average value. 14.3 Samples
Weigh the sample according to Table 3, accurate to 0.0001g. Table 3
Silicon content, %
0. 0005~0. 0020
>0. 0020~0. 0100
>0. 010~0. 025
>0, 025~～0. 070
14.4 Blank test
Carry out a blank test with the sample.
14.5 Determination
Absorption dish + cm2
Working curve number
14.5.1 Place the sample (14.3) in a 60mL dry plastic bottle, add 1mL sodium nitrate solution (12.5), 2ml nitric acid (12.2) and drop a total of 2mL hydrofluoric acid (12.3) to dissolve the sample. Place the plastic bottle in a boiling water bath and heat for 2min, remove it and cool it. 14.5.2 Pipette the test solution into the plastic extraction bottle (13.2), then aspirate 15mL MIBK (12.4), shake for 2min, let stand to separate, put the aqueous phase into the original plastic bottle, and discard the organic phase. Repeat the extraction 4 times with 15, 10, 10, and 5mL MIBK (12.4) respectively. For the last extraction, put the aqueous phase into a 120mL plastic bottle and add 45mL water. 14.5.3 Add 4g boric acid to the plastic bottle, place it in a boiling water bath and heat to dissolve for 10min, mix well, continue heating for 5min, take it out, immediately add 12mL ammonium molybdate solution (12.6), mix well, and let it stand for 10min. Add 5mL sulfuric acid (12.7), 10mlL oxalic acid solution (12.8), and 2ml reducing agent solution (12.9) in sequence, mix well, cool, transfer to a 100mL volumetric flask, dilute to the mark with water, mix well, and let it stand for 15min. 14.5.4 Transfer part of the solution into the corresponding absorption dish according to Table 3, and measure its absorbance at a wavelength of 800nm on a spectrophotometer with water as the reference.
14.5.5 Subtract the absorbance of the blank solution accompanying the sample, and find out the silicon content from the corresponding working curve according to Table 3. 14.6 Drawing of working curve
14.6.1 Working curve 1
14.6.1.1 Transfer 0, 0.10, 0.30, 0.50, 0.70.1.00mL of silicon standard solution (12.11) into a 120mL plastic bottle. 14.6.1.2 Add 2mL nitric acid (12.2) and 2mL hydrofluoric acid (12.3), and add water to 50mL. The following operations are carried out according to 6.5.3~6.5.4. 14.6.1.3 Subtract the absorbance of the reagent blank, and draw a working curve with the amount of silicon as the horizontal axis and the absorbance as the vertical axis. 14.6.2 Working curve 1
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00, 7.00 mL of silicon standard solution (12.11) into a set of 120 ml plastic bottles. The following operations are carried out according to 14.6.1.2 to 14.6.1.3. 15 Calculation and expression of analysis results
Calculate the percentage of silicon according to the following formula:
Si(%)=m;X10-6
Where: m—the amount of silicon found from the working curve, g. mo---the mass of the sample, g.
16 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 506
Additional Notes:
0. 0005~~0. 0010
>0. 0010~0. 0025
>0.00250.0070
>0. 0070~0.0150
>0.015~0. 040
>0. 040~0. 070
GB/T15076.6—94
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Refinery. This standard is drafted by Ningxia Nonferrous Metals Refinery. The main drafter of this standard is Song Yunjia.
From the date of implementation of this standard, the former Ministry
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