CN100367025C - Method for measuring alumina in cryolite - Google Patents
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- CN100367025C CN100367025C CNB2005100706684A CN200510070668A CN100367025C CN 100367025 C CN100367025 C CN 100367025C CN B2005100706684 A CNB2005100706684 A CN B2005100706684A CN 200510070668 A CN200510070668 A CN 200510070668A CN 100367025 C CN100367025 C CN 100367025C
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- 229910001610 cryolite Inorganic materials 0.000 title claims abstract description 35
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000005303 weighing Methods 0.000 claims abstract description 37
- 238000005406 washing Methods 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 58
- 239000002244 precipitate Substances 0.000 claims description 40
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 39
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 32
- 229910052697 platinum Inorganic materials 0.000 claims description 29
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000009835 boiling Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 17
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000004380 ashing Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000004062 sedimentation Methods 0.000 abstract 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 2
- 238000005516 engineering process Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 15
- 230000007935 neutral effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 150000004673 fluoride salts Chemical class 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
Abstract
The present invention relates to a method for measuring alumina in cryolite, particularly to a chemistry analysis detection technology method for measuring substance components particularly to for measuring the aluminum oxide content in a cryolite product. The present invention has a reagent preparation process, a fine sample grinding process, a sample weighing process, a sample dissolving process, a sedimentation washing process, a sedimentation burning condition process, a sedimentation cooling process and a sedimentation weighing process. The present invention can accurately and quickly measure the aluminum oxide content in the cryolite, the present invention is suitable for cryolite products produced by all nationwide manufacturing plants, and the cryolite products reach national standard quality requirements.
Description
Technical Field
A method for measuring alumina in cryolite relates to a chemical analysis detection technical method for measuring substance components, in particular to the measurement of the alumina content in cryolite products.
Background
In the industrial production of metallic aluminum, the components of cryolite produced by fluoride salt manufacturers can have certain influence on the production process of products. The content of alumina in cryolite is high, particularly when the content of alumina in the cryolite exceeds 4%, the downstream production process of the remelting aluminum ingot is influenced, in the production process of the remelting aluminum ingot, if the content of alumina in the cryolite is too high, the addition of the cryolite can cause the local alumina content of electrolyte to be too high, and the accurate control of the electrolyte molecular ratio is also influenced, but a method for measuring the content of alumina in the cryolite is not available at present.
Under normal production conditions, the total amount of orthocryolite and cryolite in cryolite (i.e. the major component of the cryolite product) is generally greater than 98%, and the content of alumina is very low (less than 0.2%), wherein the content of the major component of cryolite is calculated without considering the influence of alumina, but when the content of alumina is too high (such as greater than 1%), the calculated value of the major component of the cryolite product has a large deviation from the actual content if the content of alumina is not considered. The determination of alumina in cryolite is important.
Disclosure of Invention
The invention aims to provide the method for measuring the alumina in the cryolite, which has high measuring accuracy, meets the requirements of cryolite users, improves the working efficiency and saves the production cost.
The method is realized by the following technical scheme.
A method for measuring alumina in cryolite comprises the processes of reagent preparation, sample fine grinding, sample weighing, sample dissolving, precipitate washing, precipitate burning, precipitate cooling and weighing; the method is characterized by comprising the following steps:
a. preparing a reagent: preparing an aluminum chloride solution with the concentration of 50-300 g/L; acetic acid solution with weight concentration of 2-10 percent; silver nitrate solution with the concentration of 10 g/L;
b. grinding the sample until the sample passes through a 74-micron sieve, drying the sample in an oven at 105-110 ℃ for 2 hours, and placing the sample in a dryer to cool the sample to room temperature;
c. and (3) dissolving: weighing 0.5-1 g of sample, placing the sample in a beaker, adding 50-150 ml of water and 10-100 ml of aluminum chloride solution with the concentration of 50-200 g/L, stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 2-20 min, and taking down;
d. washing process, ignition of precipitate, cooling and weighing of precipitate: filtering with filter paper, transferring all the precipitate onto the filter paper, washing with boiling 2-10% acetic acid solution until the filtrate is free of chloride ions, and washing with hot water to neutrality; putting the precipitate and filter paper into a constant-weight platinum crucible, ashing the platinum crucible on an electric furnace, then moving the platinum crucible into a high-temperature furnace at 850-1050 ℃, burning the platinum crucible for 30min, taking out the platinum crucible, putting the platinum crucible into a drier, cooling the platinum crucible to room temperature, and weighing;
e. the content of alumina in cryolite is calculated according to the following formula:
in the formula: m is 1 -amount of precipitate after subtraction of blank, g;
m0 - sample size, g.
The method can accurately and quickly measure the content of the alumina in the cryolite. The invention is suitable for all fluoride salt manufacturers in China to produce cryolite products meeting the national standard quality requirements.
Detailed Description
The invention is further illustrated with reference to examples as follows:
a method for measuring alumina in cryolite comprises the steps of reagent preparation, sample weighing, sample dissolving, precipitate washing, precipitate burning, precipitate cooling and weighing.
The content of alumina in cryolite is calculated according to the following formula:
in the formula: m is 1 -amount of precipitate after subtraction of blank, g;
m 0 sample size, g.
The reagents required to be prepared in the invention are as follows: 1, 50-300 g/L of aluminum chloride solution; 2, 2 to 10 percent of acetic acid solution; 3 silver nitrate solution 10g/L.
The samples used in the present invention should be ground to pass through a 74 μm sieve and dried in an oven at 105-110 ℃ for 2h, and then placed in a desiccator to be cooled to room temperature for use.
The weighing amount of the sample in the invention is 0.5-1 g.
The dissolution process of the sample in the invention is as follows: weighing 0.5-1 g of sample, placing the sample in a beaker, adding 50-150 ml of water and 10-100 ml of aluminum chloride solution (50-200 g/L), stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 2-20 min (continuously stirring and keeping the original volume), and taking down.
The washing process, the burning condition and the cooling and weighing conditions of the precipitate in the invention are as follows: filter with filter paper, transfer all the precipitate to filter paper, wash with boiling acetic acid solution (2-10%) until the filtrate is free of chloride ion (checked with silver nitrate solution), and wash with hot water to neutrality. Putting the precipitate and filter paper into a constant-weight platinum crucible, ashing on an electric furnace, moving into a high-temperature furnace with the temperature of 850-1050 ℃, burning for 30min, taking out, putting into a drier, cooling to room temperature, and weighing.
Example 1
A cryolite sample produced by a certain factory in China is ground to pass through a 74-micron sieve and is dried in an oven at 105 ℃ for 2 hours, and the cryolite sample is placed in a drier to be cooled to room temperature.
Putting the platinum crucible into a high-temperature furnace, igniting for 30min at 900 ℃, taking out the platinum crucible and a cover, putting the platinum crucible and the cover into a dryer, cooling to room temperature, and weighing.
Weighing 0.5000g of sample, placing the sample in a 300ml beaker, adding 80ml of water and 20ml of aluminum chloride solution (100 g/L), stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 5min (continuously stirring and keeping the original volume), taking down, filtering with slow filter paper, transferring all the precipitate onto the filter paper, washing with boiling acetic acid solution (5%) until the filtrate is free of chloride ions (detected by 10g/L silver nitrate solution), and washing with hot water until the filtrate is neutral. Putting the precipitate and filter paper into a constant-weight platinum crucible, ashing on an electric furnace, moving into a high-temperature furnace with the temperature of 900 ℃, burning for 30min, taking out, putting into a dryer, cooling to room temperature, and weighing.
A blank test was made with the sample.
The total time from weighing the sample to the end of the measurement was 2.5 hours, and the average of the results of 9 measurements was 4.28%, the standard deviation was 0.066%, and the coefficient of variation was 1.54%.
Example 2
Cryolite samples produced by a certain factory in China are ground to pass through a 74-micron sieve and are dried in an oven at 110 ℃ for 2 hours, and the cryolite samples are placed in a dryer to be cooled to room temperature.
Putting the platinum crucible into a high-temperature furnace, igniting for 30min at 900 ℃, taking out the platinum crucible and a cover, putting the platinum crucible and the cover into a dryer, cooling to room temperature, and weighing.
Weighing 1.0000g of sample, placing the sample in a 300ml beaker, adding 100ml of water and 50ml of aluminum chloride solution (100 g/L), stirring the sample by using a glass rod to enable the sample to be uniformly distributed at the bottom of the beaker, heating and boiling the sample for 5min (continuously stirring and keeping the original volume), taking down the sample, filtering the sample by using medium-speed filter paper, transferring all precipitates onto the filter paper, washing the filter paper by using boiled acetic acid solution (5%) until the filtrate has no chloride ions (detected by using silver nitrate solution), and washing the filter paper by using hot water until the filtrate is neutral. Putting the precipitate and filter paper into a constant-weight platinum crucible, ashing on an electric furnace, transferring into a high-temperature furnace at 900 ℃, burning for 30min, taking out, putting into a dryer, cooling to room temperature, weighing, and accurately weighing to 0.0001g.
A blank test was made with the sample.
The average of the results of 9 measurements was 0.80%, the standard deviation was 0.77%, and the coefficient of variation was 9.63% after 2 hours from the time of weighing the sample to the time of completion of the measurement.
Example 3
The same sample as in example 1 was used.
Weighing 0.5000g of sample, placing the sample in a 300ml beaker, adding 80ml of water and 20ml of aluminum chloride solution (100 g/L), stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 5min (continuously stirring and keeping the original volume), taking off, filtering with filter papers with different filter speeds, transferring all precipitates onto the filter papers, washing with boiling acetic acid solution (5%) until the filtrate is free of chloride ions (checked by 10g/L silver nitrate solution), and washing with hot water until the filtrate is neutral. Putting the precipitate and filter paper into a constant-weight platinum crucible, ashing on an electric furnace, transferring into a high-temperature furnace at the temperature of 900 ℃, burning for 30min, taking out, putting into a dryer, cooling to room temperature, and weighing.
The average of 4.10% of the 4-time measurements of the precipitate was filtered using a fast filter paper, the average of 4.30% of the 4-time measurements of the precipitate was filtered using a medium speed filter paper, and the average of 4.32% of the 4-time measurements of the precipitate was filtered using a slow speed filter paper. The measurement results of the medium-speed filter paper and the slow-speed filter paper are not obviously different, and the measurement results of the fast-speed filter paper are slightly lower, but still can meet the requirement of analysis accuracy.
Example 4
The same sample as in example 1 was used.
Weighing 0.5000g of sample, placing the sample in a 300ml beaker, adding 80ml of water, adding different amounts of aluminum chloride solution (100 g/L), stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 5min (continuously stirring and keeping the original volume), taking down, filtering with slow filter paper, transferring all precipitate onto the filter paper, washing with boiling acetic acid solution (5%) until the filtrate is free of chloride ions (checked with 10g/L silver nitrate solution), and washing with hot water until the filtrate is neutral. Putting the precipitate and filter paper into a constant-weight platinum crucible, ashing on an electric furnace, moving into a high-temperature furnace with the temperature of 900 ℃, burning for 30min, taking out, putting into a dryer, cooling to room temperature, and weighing.
The corresponding measurements with the addition of 0, 10, 20, 30, 40, 50, 100ml of aluminium chloride solution (100 g/L) are: 58.90%, 4.32%, 4.36%, 4.30%, 4.22%, 4.42%, 4.46%, the results of the assay can be seen: the measurement result is stable when more than 10ml of aluminum chloride solution is added, and the measurement result is basically independent of the content of alumina without adding the aluminum chloride solution.
Example 5
The same sample as in example 1 was used.
Weighing 0.5000g of sample, placing the sample in a 300ml beaker, adding 80ml of water and 20ml of aluminum chloride solution (100 g/L), stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for different times (stirring and keeping the original volume), taking down, filtering with slow filter paper, transferring all the precipitate onto the filter paper, washing with boiling acetic acid solution (5%) until the filtrate is free of chloride ions (checked with 10g/L silver nitrate solution), and washing with hot water until the filtrate is neutral. Putting the precipitate and filter paper into a constant-weight platinum crucible, ashing on an electric furnace, transferring into a high-temperature furnace at the temperature of 900 ℃, burning for 30min, taking out, putting into a dryer, cooling to room temperature, and weighing.
The measurement results for boiling times of 2, 5, 10, 15, 20min are: 4.24%, 4.30%, 4.34%, 4.40%, the assay results were stable.
Example 6
The same sample as in example 1 was used.
Weighing 0.5000g of sample, placing the sample in a 300ml beaker, adding 100ml of water and 30ml of aluminum chloride solution (100 g/L), stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 5min (continuously stirring and keeping the original volume), taking down, filtering with slow filter paper, transferring all precipitate onto the filter paper, washing with boiling acetic acid solution (5%) until the filtrate is free of chloride ions (detected by 10g/L silver nitrate solution), and washing with hot water until the filtrate is neutral. And putting the precipitate and filter paper into a constant-weight platinum crucible, incinerating on an electric furnace, respectively burning at different temperatures, taking out, putting into a dryer, cooling to room temperature, and weighing.
The ignition temperatures are 700, 800, 900, 1000 and 1050 ℃, and the corresponding measurement results are as follows: 5.82%, 4.26% and 4.26%, and the result is stable when the ignition temperature is higher than 800 ℃.
Example 7
The same sample as in example 1 was used.
Weighing 0.5000g of sample, placing the sample in a 300mi beaker, adding different amounts of water and 20ml of aluminum chloride solution (100 g/L), stirring with a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 5min (stirring continuously and keeping the original volume), taking down, filtering with slow filter paper, transferring all the precipitate onto the filter paper, washing with boiling acetic acid solution (5%) until the filtrate is free of chloride ions (checked with 10g/L silver nitrate solution), and washing with hot water until the filtrate is neutral. Putting the precipitate and filter paper into a constant-weight platinum crucible, ashing on an electric furnace, transferring into a high-temperature furnace with the temperature of 900 ℃, burning for 30min, taking out, putting into a dryer, cooling to room temperature, and weighing.
The volumes of water added were 30, 60, 80, 100, 150ml corresponding to the assay results: 4.20%, 4.26%, 4.24%, 4.16%, 4.08%, the volume of water added is between 30 and 150 ml.
Claims (1)
1. A method for measuring alumina in cryolite comprises the steps of preparing a reagent, finely grinding a sample, weighing the sample, dissolving the sample, washing a precipitate, burning the precipitate, cooling the precipitate and weighing; characterized in that the determination steps comprise:
a. preparing a reagent: preparing an aluminum chloride solution with the concentration of 50-300 g/L; acetic acid solution with weight concentration of 2-10 percent; silver nitrate solution with the concentration of 10 g/L;
b. grinding the sample until the sample passes through a 74-micron sieve, drying the sample in an oven at 105-110 ℃ for 2 hours, and placing the sample in a dryer to cool the sample to room temperature;
c. and (3) dissolving: weighing 0.5-1 g of sample, placing the sample in a beaker, adding 50-150 ml of water and 10-100 ml of aluminum chloride solution with the concentration of 50-200 g/L, stirring by using a glass rod to uniformly distribute the sample at the bottom of the beaker, heating and boiling for 2-20 min, and taking down;
d. washing process, ignition of precipitate, cooling and weighing of precipitate: filtering with filter paper, transferring all the precipitate onto the filter paper, washing with boiling 2-10% acetic acid solution until the filtrate is free of chloride ions, and washing with hot water to neutrality; putting the precipitate and filter paper into a constant-weight platinum crucible, ashing the platinum crucible on an electric furnace, then moving the platinum crucible into a high-temperature furnace with the temperature of 850-1050 ℃, burning the platinum crucible for 30min, taking out the platinum crucible, putting the platinum crucible into a dryer, cooling the platinum crucible to room temperature, and weighing the platinum crucible;
e. the content of alumina in cryolite is calculated according to the following formula:
in the formula: m is 1 -amount of precipitate after subtraction of blank, g;
m 0 sample size, g.
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| CN106062541A (en) * | 2015-02-04 | 2016-10-26 | 俄罗斯工程技术中心 | Method for determining the composition and cryolite ratio of solid samples of potassium-containing electrolyte in aluminium production by XRD |
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| CN104215541B (en) * | 2013-08-27 | 2016-09-14 | 芜湖东旭光电装备技术有限公司 | Efficiently, high purity aluminium oxide content and the method for impurity content are accurately detected |
| CN104280306A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting content of silicon dioxide and aluminum oxide in glass |
| CN104634774B (en) * | 2015-03-03 | 2017-08-29 | 四川西冶新材料股份有限公司 | The assay method of ice crystal content in welding material |
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| US6220748B1 (en) * | 1999-01-15 | 2001-04-24 | Alcoa Inc. | Method and apparatus for testing material utilizing differential temperature measurements |
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Cited By (2)
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| CN106062541A (en) * | 2015-02-04 | 2016-10-26 | 俄罗斯工程技术中心 | Method for determining the composition and cryolite ratio of solid samples of potassium-containing electrolyte in aluminium production by XRD |
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