CN101344489A - Method for measuring calcium constituent in silicon aluminum calcium barium alloy - Google Patents
Method for measuring calcium constituent in silicon aluminum calcium barium alloy Download PDFInfo
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Abstract
The invention discloses a method used for measuring the calcium element in a silicon, aluminum, calcium and barium alloy, which comprises the following steps: a test sample is placed in a beaker, and deionized water is added until the test sample is wet; 9.5 to 10.5 millimeter of nitric acid is added; 1 to 2 millimeter of hydrofluoric acid is titrated; the mixture solution is heated until completely dissolved; perchloric acid is added; the mixture solution is heated until the sample volume is reduced to 1 to 2 millimeter; the mixture solution is naturally cooled; the perchloric acid is further added, and the mixture solution is heated until the sample volume is reduced to 1 to 2 millimeter; the hydrochloric acid and the deionized water are further added; the mixture solution is heated until all salts are dissolved, and the mixture solution is naturally cooled until the temperature is lower than 40 DEG C; the test sample is placed into a volumetric flask with scales and diluted with the deionized water; a mother solution is placed into a trigonal cup, the deionized water, trolamine (1 added by 1), lemery, bitter salt and an calcon-carboxylic acid are added, and the mother solution is adjusted to be red with potassium hydroxide; the potassium hydroxide is further added; EDTA is titrated until an end point that the mother solution becomes blue; and an analyzing result is computed. The method does not need precipitation separation and filtration, and has the acute end point without intermediate color and improved measuring accuracy.
Description
Technical field
The present invention relates to the analytical chemistry field, more belong to the analytical approach that adopts the EDTA direct titrimetric method to measure the calcium constituent in the silicon aluminum calcium barium alloy.
Background technology
At present, the detection method of calcium in the silicon aluminum calcium barium alloy generally all adopts ammoniacal liquor separation of iron and aluminium, and ammonium persulfate separates manganese, and glazier's salt precipitation barium is indicator with the calcon-carboxylic acid, the EDTA titration.This method complex operation, analytical cycle is long, the cost height.
People are in order to improve the work efficiency of analyzing and testing, around the ultimate analysis in the silicon aluminum calcium barium alloy has been made extensive work and certain effect is arranged, in " mensuration of barium, calcium in the silicon aluminum calcium barium alloy " literary composition of delivering in " Chemical Engineer " periodical of publishing in February, 2003, the method that only needs molten sample once just barium, calcium content can be measured is simultaneously disclosed.By analysis, though this method can be measured barium, calcium content simultaneously, its deficiency is: the one, and owing to the perchloric acid of 20 milliliters of disposable addings, make the calcium in the solution discharge insufficient; The 2nd, the metachromasia of solution terminal point is slow, has intermediate color to exist; The 3rd, because the potassium hydroxide of 20 milliliters of disposable addings, make the pH value instability of solution, reappearance is relatively poor; The 4th, because the hydrofluorite that adds is more, environment there is pollution; The 5th, need filter.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide calcium constituent time in a kind of assay determination silicon aluminum calcium barium alloy short, calcium discharges fully, the analytical approach of the calcium constituent in the mensuration silicon aluminum calcium barium alloy that pH value is stable, the assay determination accuracy rate is high of the metachromasia sensitivity of solution terminal point, solution.
Realize the technical measures of above-mentioned purpose:
A kind of method of measuring calcium constituent in the silicon aluminum calcium barium alloy, its step:
1) the materials sample of 0.1～1.0 gram places polytetrafluoroethylene beaker, and it is moistening to sample to add deionized water;
2) add 9.5～10.5 milliliters in nitric acid;
3) drip 1～2 milliliter in hydrofluorite;
4) heat until sample at electric hot plate and dissolve fully;
5) add 4.5～5.5 milliliters in perchloric acid;
6) under 170～190 ℃ of conditions, be heated to volume of sample and narrow down to 1～2 milliliter;
7) naturally cool to 25～35 ℃;
8) add 4.5～5.5 milliliters in perchloric acid, and under 170～190 ℃ of conditions, be heated to volume of sample and narrow down to 1～2 milliliter;
9) add 9.5～10.5 milliliters of hydrochloric acid, 45～55 milliliters of deionized waters;
10) under 100-120 ℃ condition, be heated to the salt dissolving, take off, adopt the natural cooling mode that sample is cooled to be lower than 40 ℃;
11) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake evenly mother liquor preparation end with deionized water;
12) get mother liquor and place triangle cup or beaker for 20～30 milliliters, and add 5 milliliters in magnesium sulphate, calcon-carboxylic acid 0.1～0.2 gram of 10 milliliters of glazier's salts, 5% (mass concentration) of no more than 50 milliliters of deionized water, 20 milliliters of triethanolamines (1+1), 10% (mass concentration) respectively, and be that the potassium hydroxide of 200 grams per liters is adjusted to redness with solution with volume mass concentration;
13) adding 10 ml volumes mass concentrations again is the potassium hydroxide of 200 grams per liters;
14) adopting EDTA titration to blueness is that terminal point finishes.
15) calculating of analysis result: the mass percent (%) that is calculated as follows calcium:
In the formula: C---the concentration mol/L of EDTA standard titration solution;
V---liquid consumes the volume of EDTA standard titration solution, ml;
M---divide the test portion amount of getting test solution, g;
40.08---molal weight, g/mol.
The present invention is compared with prior art: do not need to adopt ammoniacal liquor separation of iron, aluminium, ammonium persulfate separates manganese, directly adopts triethanolamine to shelter compositions such as iron, aluminium, manganese; Do not need precipitate and separate, reduced operation link, lowered Measurement Uncertainty; Sulfate precipitation barium is eliminated the interference of barium, need not filter; Add a spot of magnesium sulphate, make the terminal point acumen, improved the accuracy of measuring.
Embodiment
The calculating of the analysis result of following examples: the mass percent (%) that all calculates calcium according to following formula:
Embodiment 1
A kind of method of measuring calcium constituent in the silicon aluminum calcium barium alloy, its step:
1) sample that (the YSB14612 Ca:9.25%) 0.1000 that materials restrains places polytetrafluoroethylene beaker, and it is moistening to sample to add deionized water;
2) add 10 milliliters in nitric acid;
3) drip 1 milliliter in hydrofluorite;
4) heat until sample at electric hot plate and dissolve fully;
5) add 4.5 milliliters in perchloric acid;
6) under 170 ℃ of conditions, be heated to volume of sample and narrow down to 2 milliliters;
7) naturally cool to 25 ℃;
8) add 4.5 milliliters in perchloric acid, and under 170 ℃ of conditions, be heated to volume of sample and narrow down to 2 milliliters;
9) add 10 milliliters of hydrochloric acid, 50 milliliters of deionized waters;
10) under 100 ℃ condition, be heated to the salt dissolving, take off and adopt the natural cooling mode that sample is cooled in 38 ℃;
11) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake evenly mother liquor preparation end with deionized water;
12) get mother liquor and place triangle cup or beaker for 20 milliliters, and add 5 milliliters in magnesium sulphate, calcon-carboxylic acid 0.1 gram of 10 milliliters of glazier's salts, 5% (mass concentration) of no more than 50 milliliters of deionized water, 20 milliliters of triethanolamines (1+1), 10% (mass concentration) respectively, and be that 10 milliliters of potassium hydroxide of 200 grams per liters are adjusted to redness with solution with volume mass concentration;
13) adding 10 milliliters volume mass concentration again is the potassium hydroxide of 200 grams per liters;
14) adopting EDTA titration to the blueness of 0.005 mol is that terminal point finishes, and the titration volume of EDTA is 9.25 milliliters.
15) as calculated, the content of calcium is 9.27%
Embodiment 2
A kind of method of measuring calcium constituent in the silicon aluminum calcium barium alloy, its step:
1) sample that (the YSB14612 Ca:9.25%) 0.2800 that materials restrains places polytetrafluoroethylene beaker, and it is moistening to sample to add deionized water;
2) add 10 milliliters in nitric acid;
3) drip 1 milliliter in hydrofluorite;
4) heat until sample at electric hot plate and dissolve fully;
5) add 4.5 milliliters in perchloric acid;
6) under 180 ℃ of conditions, be heated to volume of sample and narrow down to 1.5 milliliters;
7) naturally cool to 25 ℃;
8) add 4.5 milliliters in perchloric acid, and under 180 ℃ of conditions, be heated to volume of sample and narrow down to 1.5 milliliters;
9) add 10 milliliters of hydrochloric acid, 50 milliliters of deionized waters;
10) under 100 ℃ condition, be heated to the salt dissolving, take off and adopt the natural cooling mode that sample is cooled to be lower than 35 ℃;
11) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake evenly mother liquor preparation end with deionized water;
12) get mother liquor and place triangle cup or beaker for 20 milliliters, and add 5 milliliters in magnesium sulphate, calcon-carboxylic acid 0.15 gram of 10 milliliters of glazier's salts, 5% (mass concentration) of no more than 50 milliliters of deionized water, 20 milliliters of triethanolamines (1+1), 10% (mass concentration) respectively, and be that the potassium hydroxide of 200g/L is adjusted to redness for 10 milliliters with solution with volume mass concentration;
13) adding 10 milliliters volume mass concentration again is 200 grams per liter potassium hydroxide;
14) adopting EDTA titration to the blueness of 0.01 mol is that terminal point finishes, and the titration volume of EDTA is 12.93 milliliters.
15) as calculated, the content of calcium is 9.25%
Embodiment 3
A kind of method of measuring calcium constituent in the silicon aluminum calcium barium alloy, its step:
1) sample that (YSB14612Ca:9.25%) 0.6 that materials restrains places polytetrafluoroethylene beaker, and it is moistening to sample to add deionized water;
2) add 10.5 milliliters in nitric acid;
3) drip 1.5 milliliters in hydrofluorite;
4) heat until sample at electric hot plate and dissolve fully;
5) add 5.0 milliliters in perchloric acid;
6) under 185 ℃ of conditions, be heated to volume of sample and narrow down to 1.3 milliliters;
7) naturally cool to 28 ℃;
8) add 5.0 milliliters in perchloric acid, and under 190 ℃ of conditions, be heated to volume of sample and narrow down to 1.3 milliliters;
9) add 9.5 milliliters of hydrochloric acid, 50 milliliters of deionized waters;
10) under 110 ℃ of conditions, be heated to dissolving fully, take off, adopt the natural cooling mode that sample is cooled to 30 ℃;
11) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake evenly mother liquor preparation end with deionized water;
12) get mother liquor and place the triangle cup for 25 milliliters, and add 5 milliliters in magnesium sulphate, calcon-carboxylic acid 0.1 gram of 10 milliliters of glazier's salts, 5% concentration of 50 milliliters of deionized waters, 20 milliliters of triethanolamines (1+1), 10% concentration respectively, and be that 10 milliliters of potassium hydroxide of 200g/L are adjusted to redness with solution with volume mass concentration;
13) add 10 milliliters of potassium hydroxide that volume mass concentration is 200g/L again;
14) adopting EDTA titration to the blueness of 0.01 mol is that terminal point finishes, and the titration volume of EDTA is 34.60mL
15) as calculated, the content of calcium is 9.24%.
Embodiment 4
A kind of method of measuring calcium constituent in the silicon aluminum calcium barium alloy, its step:
1) sample that (the YSB14612 Ca:9.25%) 1.0 that materials restrains places polytetrafluoroethylene beaker, and it is moistening to sample to add deionized water;
2) add 10.5 milliliters in nitric acid;
3) drip 2.0 milliliters in hydrofluorite;
4) heat until sample at electric hot plate and dissolve fully;
5) add 5.5 milliliters in perchloric acid;
6) under 190 ℃ of conditions, be heated to volume of sample and narrow down to 1.0 milliliters;
7) naturally cool to 30 ℃;
8) add 5.5 milliliters in perchloric acid, and under 190 ℃ of conditions, be heated to volume of sample and narrow down to 1.0 milliliters;
9) add 9.5 milliliters of hydrochloric acid, 55 milliliters of deionized waters;
10) under 120 ℃ of conditions, be heated to dissolving fully, take off, adopt the natural cooling mode that sample is cooled to 28 ℃;
11) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake evenly mother liquor preparation end with deionized water;
12) get mother liquor and place the triangle cup for 30 milliliters, and add 5 milliliters in magnesium sulphate, calcon-carboxylic acid 0.1 gram of 10 milliliters of glazier's salts, 5% concentration of 50 milliliters of deionized waters, 20 milliliters of triethanolamines (1+1), 10% concentration respectively, and be that 10 milliliters of potassium hydroxide of 200g/L are adjusted to redness with solution with volume mass concentration;
13) add 10 milliliters of potassium hydroxide that 10 ml volumes mass concentrations are 200g/L again;
14) adopting EDTA titration to the blueness of 0.02mol/L is that terminal point finishes, and the titration volume of EDTA is 34.6mL.
15) as calculated, the content of calcium is 9.26%.
As follows through testing its result:
1, the precision of method experiment: chosen two standard models, each sample measurement 11 times calculates its relative standard deviation (RSD).Statistics sees Table 1.
The measurement result of calcium (%) in table 1 blank reagent solution
The data of table 1 as can be seen, the relative standard deviation of this analytical approach is less than 1%, the reappearance of analysis result is fine.
2, the accuracy of method experiment (reclaiming experiment): that selects to produce is numbered YSB14610 and two standard models of YSB14613, adds the standard solution of the calcium of certain content, press the sample analysis step and operates, and carries out recovery test, and measurement result sees Table 2.
Table 2 recovery test measurement result (%)
By the data of table 2 as can be seen, the recovery can satisfy the requirement of detection fully between 98.1%-101.4%.
Claims (1)
1, a kind of method of measuring calcium constituent in the silicon aluminum calcium barium alloy, its step:
1) the materials sample of 0.1～1.0 gram places polytetrafluoroethylene beaker, and it is moistening to sample to add deionized water;
2) add 9.5～10.5 milliliters in nitric acid;
3) drip 1～2 milliliter in hydrofluorite;
4) heat until sample at electric hot plate and dissolve fully;
5) add 4.5～5.5 milliliters in perchloric acid;
6) under 170～190 ℃ of conditions, be heated to volume of sample and narrow down to 1～2 milliliter;
7) naturally cool to 25～35 ℃;
8) add 4.5～5.5 milliliters in perchloric acid, and under 170～190 ℃ of conditions, be heated to volume of sample and narrow down to 1～2 milliliter;
9) add 9.5～10.5 milliliters of hydrochloric acid, 45～55 milliliters of deionized waters;
10) under 100-120 ℃ condition, be heated to the salt dissolving, take off, adopt the natural cooling mode that sample is cooled to be lower than 40 ℃;
11) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake evenly mother liquor preparation end with deionized water;
12) get mother liquor and place triangle cup or beaker for 20～30 milliliters, and add 5 milliliters in magnesium sulphate, calcon-carboxylic acid 0.1～0.2 gram of 10 milliliters of glazier's salts, 5% (mass concentration) of no more than 50 milliliters of deionized water, 20 milliliters of triethanolamines (1+1), 10% (mass concentration) respectively, and be that the potassium hydroxide of 200 grams per liters is adjusted to redness with solution with volume mass concentration;
13) adding 10 ml volumes mass concentrations again is the potassium hydroxide of 200 grams per liters;
14) adopting EDTA titration to blueness is that terminal point finishes.
15) calculating of analysis result: the mass percent (%) that is calculated as follows calcium:
In the formula: C---the concentration mol/L of EDTA standard titration solution;
V---test solution consumes the volume of EDTA standard titration solution, ml;
M---divide the test portion amount of getting test solution, g;
40.08---the molal weight of calcium, g/mol.
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