CN105044275B - The method of testing of alumina content in aluminium metaphosphate - Google Patents
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- 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 29
- DHAHRLDIUIPTCJ-UHFFFAOYSA-K aluminium metaphosphate Chemical compound [Al+3].[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O DHAHRLDIUIPTCJ-UHFFFAOYSA-K 0.000 title claims abstract description 22
- 238000010998 test method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012086 standard solution Substances 0.000 claims abstract description 13
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 claims abstract description 13
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 7
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 7
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 7
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 7
- 229940053652 fluorinse Drugs 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 7
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 28
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 13
- 229960001763 zinc sulfate Drugs 0.000 claims description 13
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 13
- 238000004448 titration Methods 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 8
- 239000012488 sample solution Substances 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 7
- 229960005382 phenolphthalein Drugs 0.000 description 5
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UOFGSWVZMUXXIY-UHFFFAOYSA-N 1,5-Diphenyl-3-thiocarbazone Chemical compound C=1C=CC=CC=1N=NC(=S)NNC1=CC=CC=C1 UOFGSWVZMUXXIY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007716 flux method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- VLYFRFHWUBBLRR-UHFFFAOYSA-L potassium;sodium;carbonate Chemical compound [Na+].[K+].[O-]C([O-])=O VLYFRFHWUBBLRR-UHFFFAOYSA-L 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013102 re-test Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provide a kind of simple to operate, fast and accurately in aluminium metaphosphate alumina content method of testing.The method of testing of alumina content in aluminium metaphosphate, the method are comprised the following steps：1) sample is weighed, adds sodium hydroxide solution complete to sample dissolving, then salt adding acid is to the aobvious acidity of solution；2) disodium ethylene diamine tetraacetate standard liquid is added to shake up, plus several drop phenolphthalein, redness is neutralized to ammoniacal liquor, then be adjusted to a colourless and excessive drop with hydrochloric acid；Plus ammonium acetate, heating is boiled, plus a few drop xylenol orange solution, is titrated to redness with sulfuric acid Zinc standard solution；3) Fluorinse is added, heating is boiled, then is titrated to redness with sulfuric acid Zinc standard solution；4) result is calculated.The present invention adopts the quick dissolved samples of sodium hydroxide solution, high have the advantages that easily operated, the simple and quick, degree of accuracy.
Description
Technical field
The present invention relates to chemical analysis test field, more particularly to a kind of quick dissolving aluminium metaphosphate and accurately test are partially
The method of alumina content in aluminum phosphate.
Background technology
Aluminium metaphosphate is a kind of raw material for manufacturing optical glass, and its purity directly affects the optical property of optical glass.
At present, the detection of aluminium metaphosphate purity is also nothing national standard method of testing, weigh in industry aluminium metaphosphate purity be by test
The content of the content of phosphorus pentoxide or aluminum oxide in aluminium metaphosphate, then the pure of aluminium metaphosphate is become by certain coefficient conversion
Degree.
At present, in aluminium metaphosphate, the test of phosphorus pentoxide content is that the method is accurate using phosphomolybdic acid quinoline gravimetric method
Degree and the degree of accuracy all fine, have the disadvantage that analytical procedure is loaded down with trivial details, analytical cycle is long, the preparation of precipitating reagent using acetone and quinoline this two
Poisonous organic matter is planted, tester brings very big harm to analysis, while also to environment.《Lab technician's reader》
In the aluminium salt that fourth edition (Beijing University of Chemical Technology Liu Zhen chief editor) is provided, the method for testing of alumina content is：Add in aluminum salt solution
A certain amount of and excessive standard EDTA solution, heating boil, and make indicator with xylenol orange after cooling, adjust solution acidity to pH
=5～6, the excessive EDTA of drop is returned with Dithizone.The method degree of accuracy is higher, but for oxygen in test aluminium metaphosphate
Change the content of aluminium, analysis process is more complicated, and analytical cycle is long, and sample needs 900 DEG C of calcinations of mixed flux, agents useful for same
Species and amount ratio larger, these factors can all affect the accuracy of test result.
Content of the invention
The technical problem to be solved be provide a kind of simple to operate, fast and accurately aoxidize in aluminium metaphosphate
The method of testing of aluminium content.
The present invention solves the technical scheme that adopted of technical problem：The method of testing of alumina content in aluminium metaphosphate,
The method is comprised the following steps：
1) sample of 0.2g～0.4g drying is weighed, and the sodium hydroxide solution of 10mL～20mL 100g/L is added to sample
Product dissolving completely, then plus 10mL～20mL 6mol/L hydrochloric acid to the aobvious acidity of solution；
2) 20mL～40mL 0.05mol/L disodium ethylene diamine tetraacetate standard liquid is added to shake up, plus several drop phenolphthalein, use ammonia
Water is neutralized to redness, then is adjusted to a colourless and excessive drop with hydrochloric acid；Plus 60% ammonium acetate of 10mL～20mL, heating boils, plus 2
Drop～3 drips xylenol orange solution, is titrated to redness with sulfuric acid Zinc standard solution；
3) 30mL～40mL 50g/L Fluorinse is added, heating is boiled, then is titrated to sulfuric acid Zinc standard solution red
Color is terminal；
4) result is calculated
In formula：
The numerical value of V zinc sulfate standard titration solution volume, unit are milliliter (mL)；
The exact value of c zinc sulfate standard titration solution concentration, unit are mole per liter (mol/L)；
The numerical value of m sample quality, unit are gram (g)；
The numerical value of 1/2nd alundum (Al2O3) molal weight of M, unit are gram per mole (g/mol).
Step 1) described weigh 0.2～0.4g and be accurate to 0.0001g.
Step 1) described dry be through 105～110 DEG C dry.
Step 1) sample for weighing 0.2～0.4g drying should be placed in beaker.
Step 1) addition 10mL～20mL 100g/L sodium hydroxide solution after, then on electric furnace heat a few minutes.
Step 2) and step 3) described to heat time for boiling be 3min～5min.
The invention has the beneficial effects as follows：The present invention is for the aluminium metaphosphate for being insoluble in water and acid, there is provided one kind hydrogen-oxygen
The method for changing the quick dissolved samples of sodium solution, with respect to conventional hybrid flux fusing sample, temperature height, time length, is difficult to leach
The shortcomings of, the method has the advantages that easily operated, the simple and quick, degree of accuracy is high, test result indicate that, the method accurately may be used
Lean on, favorable reproducibility, precision is high, is conducive to utilization and extention.
Specific embodiment
In the aluminium metaphosphate of the present invention, the method for testing of alumina content, comprises the following steps：
1) sample of the 0.2g～0.4g (being accurate to 0.0001g) through 105 DEG C～110 DEG C drying is weighed in 250mL beaker,
Add the sodium hydroxide solution of 10mL～20mL 100g/L to sample dissolving completely, then plus 10mL～20mL 6mol/L hydrochloric acid extremely
The aobvious acidity of solution；
2) 20mL～40mL 0.05mol/L disodium ethylene diamine tetraacetate standard liquid (EDTA) is added to shake up, plus several drop phenol
Phthalein, is neutralized to redness with ammoniacal liquor, then is adjusted to a colourless and excessive drop with hydrochloric acid；Plus 10mL～20mL60% ammonium acetate, heating boils
Boiling 3min～5min is removed, and drop～3 drips xylenol orange solution plus 2, is titrated to redness with sulfuric acid Zinc standard solution；
3) 30mL～40mL 50g/L Fluorinse is added, heating is boiled 3min～5min and removed, then uses zinc sulfate mark
Quasi- solution is titrated to red for terminal；
4) result is calculated
In formula：
The numerical value of V zinc sulfate standard titration solution volume, unit are milliliter (mL)；
The exact value of c zinc sulfate standard titration solution concentration, unit are mole per liter (mol/L)；
The numerical value of m sample quality, unit are gram (g)；
The numerical value of 1/2nd alundum (Al2O3) molal weight of M, unit are gram per mole (g/mol)
[M(1/2Al2O3)=51] (numerical value of 1/2nd alundum (Al2O3) molal weights, represented with mathematical expression).
5) accuracy validation：
For same sample, using the method retest 6 times, its result is as follows：
| 1 | 2 | 3 | 4 | 5 | 6 | |
| Al2O3(%) | 19.81 | 19.78 | 19.83 | 19.76 | 19.82 | 19.84 |
Found out by test result, collimation is good, precision is high, the inventive method is described accurately, reliable.
The method have the advantages that：
1) device of sample dissolution is simple.Conventional method is melted using platinum crucible, relatively costly, and the present invention can be using burning
Cup sample dissolution, reduces cost.
2) agents useful for same amount species and consumption are reduced.Conventional method is using the mixing of 8～10g sodium carbonate-potassium carbonate-borax
Solvent melts sample in 900 DEG C of Muffle furnaces, and the present invention only can dissolve sample with a kind of sodium hydroxide solution, if on electric furnace
Heating a few minutes dissolve faster, and the condition of sample dissolution is substantially reduced, and has saved the energy, reduces production cost.
3) transfer of sample solution is physically easier to perform.Traditional flux method will add hydrochloric acid and leach frit, here with boiling water
During operating personnel must carry protective articles, with anti-scald, present invention sodium hydroxide solution sample dissolution, quickly, safety.
4) more rapidly, analysis result is more accurate for analysis test process.Analysis program is reduced, analysis efficiency is improve, greatly
The accuracy of measurement result is improve greatly.
Embodiment 1：
1) sample of the 0.2g (being accurate to 0.0001g) through 105 DEG C of drying is weighed in beaker, add the hydrogen of 10mL100g/L
Sodium hydroxide solution is complete to sample dissolving；Plus 10mL 6mol/L hydrochloric acid is to the aobvious acidity of solution；
2) add 20mL 0.05mol/L disodium ethylene diamine tetraacetate standard liquid, plus 2 and phenolphthalein is dripped, be neutralized to ammoniacal liquor red
Color, then a colourless and excessive drop is adjusted to hydrochloric acid；Plus 60% ammonium acetate of 10mL, heating boils 3min and removes, drop xylenol of plus 2
Orange solution, is titrated to redness with sulfuric acid Zinc standard solution；
3) Fluorinse of 30mL 50g/L is added, and heating is boiled 3min and removed, then is titrated with sulfuric acid Zinc standard solution
To red for terminal；
4) result is calculated
In formula：
The numerical value of V zinc sulfate standard titration solution volume, unit are milliliter (mL)；
The exact value of c zinc sulfate standard titration solution concentration, unit are mole per liter (mol/L)；
The numerical value of m sample quality, unit are gram (g)；
The numerical value of M alundum (Al2O3) molal weight, unit are gram per mole of (g/mol) [M (1/2Al2O3)=51].
Embodiment 2：
1) sample of the 0.3g (being accurate to 0.0001g) through 105 DEG C of drying is weighed in beaker, add the hydrogen of 15mL100g/L
Sodium hydroxide solution is complete to sample dissolving；Plus 15mL 6mol/L hydrochloric acid is to the aobvious acidity of solution；
2) add 30mL 0.05mol/L disodium ethylene diamine tetraacetate standard liquid, plus 2 and phenolphthalein is dripped, be neutralized to ammoniacal liquor red
Color, then a colourless and excessive drop is adjusted to hydrochloric acid；Plus 60% ammonium acetate of 15mL, heating boils 3min and removes, drop xylenol of plus 3
Orange solution, is titrated to redness with sulfuric acid Zinc standard solution；
3) Fluorinse of 35mL 50g/L is added, and heating is boiled 4min and removed, then is titrated with sulfuric acid Zinc standard solution
To red for terminal；
4) result is calculated
In formula：
The numerical value of V zinc sulfate standard titration solution volume, unit are milliliter (mL)；
The exact value of c zinc sulfate standard titration solution concentration, unit are mole per liter (mol/L)；
The numerical value of m sample quality, unit are gram (g)；
The numerical value of M alundum (Al2O3) molal weight, unit are gram per mole of (g/mol) [M (1/2Al2O3)=51].
Embodiment 3：
1) sample of the 0.4g (being accurate to 0.0001g) through 110 DEG C of drying is weighed in 250mL beaker, add 20mL
The sodium hydroxide solution of 100g/L is complete to sample dissolving；Plus 20mL 6mol/L hydrochloric acid is to the aobvious acidity of solution；
2) add 40mL 0.05mol/L disodium ethylene diamine tetraacetate standard liquid, plus 3 and phenolphthalein is dripped, be neutralized to ammoniacal liquor red
Color, then a colourless and excessive drop is adjusted to hydrochloric acid；Plus 60% ammonium acetate of 20mL, heating boils 5min and removes, drop xylenol of plus 2
Orange solution, is titrated to redness with sulfuric acid Zinc standard solution；
3) Fluorinse of 40mL 50g/L is added, and heating is boiled 5min and removed, then is titrated with sulfuric acid Zinc standard solution
To red for terminal；
4) result is calculated
In formula：
The numerical value of V zinc sulfate standard titration solution volume, unit are milliliter (mL)；
The exact value of c zinc sulfate standard titration solution concentration, unit are mole per liter (mol/L)；
The numerical value of m sample quality, unit are gram (g)；
The numerical value of M alundum (Al2O3) molal weight, unit are gram per mole of (g/mol) [M (1/2Al2O3)=51].
Claims (6)
1. in aluminium metaphosphate alumina content method of testing, it is characterised in that the method is comprised the following steps：
1) sample of 0.2g～0.4g drying is weighed, adds the sodium hydroxide solution of 10mL～20mL 100g/L molten to sample
Solution completely, then plus 10mL～20mL 6mol/L hydrochloric acid to the aobvious acidity of solution；
2) 20mL～40mL 0.05mol/L disodium ethylene diamine tetraacetate standard liquid is added to shake up, plus several drop phenolphthalein, with ammoniacal liquor
With to red, then a colourless and excessive drop is adjusted to hydrochloric acid；Plus 60% ammonium acetate of 10mL～20mL, heating boils, drop～3 of plus 2
Drop xylenol orange solution, is titrated to redness with sulfuric acid Zinc standard solution；
3) 30mL～40mL 50g/L Fluorinse is added, heating is boiled, then redness is titrated to sulfuric acid Zinc standard solution be
Terminal；
4) result is calculated
In formula：
The numerical value of V zinc sulfate standard titration solution volume, unit are milliliter (mL)；
The exact value of c zinc sulfate standard titration solution concentration, unit are mole per liter (mol/L)；
The numerical value of m sample quality, unit are gram (g)；
The numerical value of 1/2nd alundum (Al2O3) molal weight of M, unit are gram per mole (g/mol).
2. in aluminium metaphosphate as claimed in claim 1 alumina content method of testing, it is characterised in that step 1) title
Take 0.2～0.4g and be accurate to 0.0001g.
3. in aluminium metaphosphate as claimed in claim 1 alumina content method of testing, it is characterised in that step 1) baking
Dry dried through 105～110 DEG C.
4. in aluminium metaphosphate as claimed in claim 1 alumina content method of testing, it is characterised in that step 1) title
The sample for taking 0.2～0.4g drying should be placed in beaker.
5. in aluminium metaphosphate as claimed in claim 1 alumina content method of testing, it is characterised in that step 1) described plus
After entering the sodium hydroxide solution of 10mL～20mL 100g/L, then heat a few minutes on electric furnace.
6. in aluminium metaphosphate as claimed in claim 1 alumina content method of testing, it is characterised in that step 2) and step
3) time that the heating is boiled is 3min～5min.
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| CN107677565A (en) * | 2017-10-31 | 2018-02-09 | 贵州开磷质量检测中心有限责任公司 | A kind of method for determining available phosphorus content in MAP and Diammonium phosphate (DAP) |
| CN109187530A (en) * | 2018-11-13 | 2019-01-11 | 衡阳市大宇锌业有限公司 | Zinc, aluminum content tests method in a kind of industry ZnSO4 |
| CN111579714A (en) * | 2020-06-28 | 2020-08-25 | 成都光明光电股份有限公司 | Method for measuring content of copper oxide in copper metaphosphate |
| CN113740200B (en) * | 2021-08-31 | 2024-09-24 | 广西产研院新型功能材料研究所有限公司 | Method for detecting component content in aluminum tripolyphosphate |
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