CN101750467A - Method for analyzing carbonate in limestone - Google Patents
Method for analyzing carbonate in limestone Download PDFInfo
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- CN101750467A CN101750467A CN200910243374A CN200910243374A CN101750467A CN 101750467 A CN101750467 A CN 101750467A CN 200910243374 A CN200910243374 A CN 200910243374A CN 200910243374 A CN200910243374 A CN 200910243374A CN 101750467 A CN101750467 A CN 101750467A
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- Prior art keywords
- carbonate
- magnesium
- limestone
- calcium
- add
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- 239000006028 limestone Substances 0.000 title claims abstract description 57
- 235000019738 Limestone Nutrition 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 37
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 28
- 239000011777 magnesium Substances 0.000 claims abstract description 31
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 27
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011575 calcium Substances 0.000 claims abstract description 27
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 20
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 19
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 19
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 16
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000000796 flavoring agent Substances 0.000 claims description 4
- 235000019634 flavors Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 abstract description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000001514 detection method Methods 0.000 abstract 1
- 229910052634 enstatite Inorganic materials 0.000 abstract 1
- 229910052909 inorganic silicate Inorganic materials 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910021534 tricalcium silicate Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 15
- 238000004090 dissolution Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910017625 MgSiO Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910004283 SiO 4 Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000011978 dissolution method Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- -1 rauhkalk Chemical compound 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 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
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for analyzing carbonate in limestone, which relates to an improvement on a method for detecting carbonate content in limestone. The method is characterized by comprising the following detection steps: heating and dissolving a limestone sample by adopting NH4Cl solution, filtering the solution, adding hydrochloric acid solution into the solution to fix volume, measuring calcium and magnesium by adopting EDTA complexometry respectively, or measuring magnesium by adopting an atomic absorption method, and working out the contents of calcium carbonate and magnesium carbonate through the measured quantities of the calcium and the magnesium. The method for analyzing the carbonate in the limestone is characterized in that after the limestone is dissolved in the NH4Cl solution, the phase composition is changed into Ca3SiO5, MgSiO3, SiO2 and Mg3Ca(SiO4)2, so the NH4Cl can selectively dissolve the carbonate in the limestone and dissolve out the carbonate qualitatively. The method of the invention can selectively and qualitatively dissolve the components of the carbonate in the limestone, and is a reliable method for accurately detecting the contents of the calcium carbonate and the magnesium carbonate in the limestone.
Description
Technical field
A kind of method of analyzing carbonate in limestone relates to a kind of improvement that is used to detect the carbonate in limestone content method.
Background technology
Lime stone is the important raw material of industry, usually needs to detect carbonate in limestone content when control lime stone quality.The sample dissolution method that detects the carbonate composition has following type and characteristics.
High-temperature melting method: add solid flux, behind the tekite lime stone sample, can be prepared into solution to be measured under the high temperature,, can calculate lime carbonate in the lime stone, magnesium carbonate content by detecting calcium, the magnesium density in the solution.Major defect is this sample treatment, and the calcium that exists with other form in the lime stone, magnesium are all calculated by lime carbonate, magnesium carbonate, causes the testing result of lime carbonate, magnesium carbonate higher.
The direct dissolution method of mineral acid: hydrochloric acid commonly used directly dissolves the lime stone specimen preparation and becomes solution to be measured, by detecting calcium, the magnesium density in the solution, can calculate lime carbonate in the lime stone, magnesium carbonate content.This method and high-temperature melting method have similar shortcoming, only cause the testing result of lime carbonate, magnesium carbonate higher few.Wherein, patent: a kind of measurement lime stone CaCO
3, MgCO
3Promptly there is this shortcoming in the method for composition (classification number: G01N2l/79 (2006.01) I).
The direct dissolution method of organic acid or strong acid weak base salt: have bibliographical information to dissolve carbonate in fluorite, the wollastonite respectively, do not see the report that is used to dissolve carbonate in limestone with acetate, aluminium choride etc.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of can effective selectivity, quantitatively dissolve carbonate in limestone, accurately detect the method for carbonate in limestone analysis on Content carbonate in limestone.
Order of the present invention is to be achieved through the following technical solutions.
A kind of method of analyzing carbonate in limestone is characterized in that its testing process step comprises employing NH
4Cl solution heating for dissolving lime stone sample, filter, add the hydrochloric acid solution constant volume, adopt the method for EDTA complexometry to measure calcium and magnesium respectively, or use aas determination magnesium, converse lime carbonate and magnesium carbonate content with calcium and the magnesium amount that records.
A kind of method of analyzing carbonate in limestone of the present invention is characterized in that the concrete operations step of the molten sample process of lime stone is:
(1) take by weighing the 0.25g sample and place the 150mL beaker, add 1.6g~4g ammonium chloride, add hot water to the about 30mL~80mL of volume, heat little boil-off separating, volume reduces to add hot water;
(2) to be evaporatedly going out when no ammonia is hidden in the water vapor, is neutral with test paper check pH value, stops to dissolve;
(3) go in the 250mL volumetric flask with quick filter paper filtering, and add 10mL~35mL hydrochloric acid, constant volume;
(4) adopt the method for EDTA complexometry to measure calcium and magnesium respectively, or use aas determination magnesium, calculate lime carbonate in the lime stone, magnesium carbonate content with calcium and the magnesium amount that records.
Because the thing phase composition mainly contains kalzit (CaCO in the lime stone
3), aragonite (CaCO
3), rauhkalk (CaCO
3MgCO
3), magnesite (MgCO
3), silicate (elements such as calcium, magnesium, iron, aluminium, sodium), also have trace quartz, amorphous silica, pyrite, calcium sulphate, calcium phosphate etc.Therefore mineral acid solubilized kalzit, aragonite, rauhkalk, magnesite and part silicate etc. can not select mineral acid.When selecting ammonium chloride (NH
4Cl) time, ammonium chloride only reacts with kalzit, aragonite, rauhkalk, magnesite (being commonly referred to as carbonate) under proper condition, does not all react mutually with other thing.Select strong acid weak base salt based on reaction mechanism be: carry out hydrolysis reaction earlier and constantly produce H
+And weak base, H
+Constantly dissolve with carbonate reaction again.Key reaction is as follows:
Acid and reactant salt: CaCO
3(MgCO
3)+2H
+=Ca
2+(Mg
2+)+CO
2↑+H
2O
A kind of method of analyzing carbonate in limestone of the present invention, lime stone is through NH
4After the Cl solution dissolution process, the thing phase composition becomes Ca
3SiO
5, MgSiO
3, SiO
2, Mg
3Ca (SiO
4)
2, NH is described
4Carbonate in the Cl energy selective dissolution lime stone, and quantitatively stripping.The composition of method alternative of the present invention, quantitative dissolving carbonate in limestone is for the content that accurately detects lime carbonate, magnesium carbonate in the lime stone provides reliable method.
Embodiment
A kind of method of analyzing carbonate in limestone, its testing process step comprise employing NH
4Cl solution heating for dissolving lime stone sample, filter, add the hydrochloric acid solution constant volume, adopt the method for EDTA complexometry to measure calcium and magnesium (or using aas determination magnesium) respectively, the content that converses lime carbonate and magnesium carbonate with the calcium that records and magnesium amount.。
The condition and the step of specific operation process are as follows:
1) ammonium chloride: solid
Hydrochloric acid: 6mol/L
2) lime stone sample granularity: less than 74 μ m
3) sample dissolution: take by weighing about 0.25g sample and place the 150mL beaker, add 1.6g~4g ammonium chloride, add hot water to the about 30mL~80mL of volume, heat little boil-off separating, volume reduces to add hot water.To be evaporated when going out in the water vapor no ammonia flavor (is neutral with test paper check pH value) stop to dissolve.Go in the 250mL volumetric flask with quick filter paper filtering, and add 10mL~35mL hydrochloric acid, constant volume.Adopt the method for EDTA complexometry to measure calcium and magnesium (or using aas determination magnesium) respectively, the content that converses lime carbonate and magnesium carbonate with the calcium that records and magnesium amount.
The foundation of determining of concrete operations condition:
(1) the ammonium chloride addition is determined: claim 0.25g lime stone sample, dissolves carbonate is complete when adding 1.6g~4g ammonium chloride, therefore selects 1.6g~4g ammonium chloride addition.
(2) liquor capacity is determined: volume is too little and too mostly be unfavorable for solubilizing reaction and operation, determines to claim that 0.25g lime stone sample dissolution volume is 30mL~80mL.
(3) heating-up temperature and time are determined: the temperature height helps the discharge of fast reaction speed and gas, keep during for the ease of the operation dissolving solution little boil just passable.Dissolution time does not react according to the lime stone sample and fixed or do not get rid of (available pH test paper check) till the ammonia, claims the 0.25g lime stone sample dissolution time more than 30min.
(4) selectivity, quantitative dissolved carbon hydrochlorate.
Confirm that through material phase analysis the thing phase composition is CaCO in the undressed lime stone
3, CaCO
3MgCO
3, Ca
3SiO
5, MgSiO
3, SiO
2, Mg
3Ca (SiO
4)
2Lime stone is through NH
4After Cl handled, the thing phase composition became Ca
3SiO
5, MgSiO
3, SiO
2, Mg
3Ca (SiO
4)
2, NH is described
4Carbonate in the Cl energy selective dissolution lime stone, and quantitatively stripping.
With the sample of known lime stone composition, after the NH4Cl processing, the composition that detects in the solution compares, and iron, aluminium all do not detect, and the silicon value of detecting is less than 0.05%.Illustrate that other thing is close insoluble the carbonate of NH4Cl in the dissolving lime stone, selectivity is fine.
(5) dissolved carbon hydrochlorate repeated experiment: measurement project: CaCO
3, dissolving number of times (n=8)
Dissolving repeats performance and satisfies conventional requirement.
(6) dissolving lime carbonate recovery test: take by weighing lime carbonate (analyzing pure) 0.1514g, 0.2143g, 0.2481g NH respectively
4Solution after Cl handles records the lime carbonate recovery (%) and is respectively 99.57,99.63,99.56, and NH is described
4Cl dissolving lime carbonate is fine.
Embodiment 1
Take by weighing lime stone sample 0.2500 gram, place the 150mL beaker, add 3g ammonium chloride, add hot water to the about 50mL of volume, heat little boil-off separating, volume reduces to add hot water.To be evaporated when going out in the water vapor no ammonia flavor (is neutral with test paper check pH value) stop to dissolve.Go in the 250mL volumetric flask with quick filter paper filtering, and add 30mL hydrochloric acid (6mol/L), constant volume.After measuring the concentration of calcium, magnesium in the solution, calculate lime carbonate 87.98% in the lime stone, magnesium carbonate 2.49%.
Embodiment 2
Take by weighing lime stone sample 0.2500 gram, place the 150mL beaker, add 3g ammonium chloride, add hot water to the about 50mL of volume, heat little boil-off separating, volume reduces to add hot water.To be evaporated when going out in the water vapor no ammonia flavor (is neutral with test paper check pH value) stop to dissolve.Go in the 250mL volumetric flask with quick filter paper filtering, and add 30mL hydrochloric acid (6mol/L), constant volume.After measuring the concentration of calcium, magnesium in the solution, calculate lime carbonate 95.35% in the lime stone, magnesium carbonate 1.38%.
Claims (2)
1. a method of analyzing carbonate in limestone is characterized in that its testing process step comprises employing NH
4Cl solution heating for dissolving lime stone sample, filter, add the hydrochloric acid solution constant volume, adopt the method for EDTA complexometry to measure calcium and magnesium respectively, or use aas determination magnesium, the content that converses lime carbonate and magnesium carbonate with the calcium that records and magnesium amount.
2. a kind of method of analyzing carbonate in limestone according to claim 1 is characterized in that the concrete operations step of the molten sample process of lime stone is:
(1) take by weighing the 0.25g sample and place the 150mL beaker, add 1.6g~4g ammonium chloride, add hot water to the about 30mL~80mL of volume, heat little boil-off separating, volume reduces to add hot water;
(2) to be evaporated when going out in the water vapor no ammonia flavor, be neutral with test paper check pH value, stop to dissolve;
(3) go in the 250mL volumetric flask with quick filter paper filtering, and add 10mL~35mL hydrochloric acid, constant volume;
(4) adopt the method for EDTA complexometry to measure calcium and magnesium respectively, or use aas determination magnesium, calculate lime carbonate in the lime stone, magnesium carbonate content with calcium and the magnesium amount that records.
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CN200910243374A CN101750467A (en) | 2009-12-18 | 2009-12-18 | Method for analyzing carbonate in limestone |
Applications Claiming Priority (1)
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CN200910243374A CN101750467A (en) | 2009-12-18 | 2009-12-18 | Method for analyzing carbonate in limestone |
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Publication Number | Publication Date |
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CN101750467A true CN101750467A (en) | 2010-06-23 |
Family
ID=42477759
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103323451A (en) * | 2013-06-08 | 2013-09-25 | 四川汉龙新材料有限公司 | Determination method of marble and fluorite content in electrode coating |
CN104090063A (en) * | 2014-07-24 | 2014-10-08 | 湖南水口山有色金属集团有限公司 | Method for detecting purity of slaked lime |
CN104198486A (en) * | 2014-09-23 | 2014-12-10 | 中蓝连海设计研究院 | Method for measuring content of calcium carbonate in gypsum |
CN104843756A (en) * | 2015-03-26 | 2015-08-19 | 龙岩紫云化学科技有限公司 | Decomposition method of carbonatite |
CN116183597A (en) * | 2022-11-10 | 2023-05-30 | 长沙矿冶院检测技术有限责任公司 | Method for measuring content of calcium fluoride in ore |
-
2009
- 2009-12-18 CN CN200910243374A patent/CN101750467A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103323451A (en) * | 2013-06-08 | 2013-09-25 | 四川汉龙新材料有限公司 | Determination method of marble and fluorite content in electrode coating |
CN104090063A (en) * | 2014-07-24 | 2014-10-08 | 湖南水口山有色金属集团有限公司 | Method for detecting purity of slaked lime |
CN104198486A (en) * | 2014-09-23 | 2014-12-10 | 中蓝连海设计研究院 | Method for measuring content of calcium carbonate in gypsum |
CN104843756A (en) * | 2015-03-26 | 2015-08-19 | 龙岩紫云化学科技有限公司 | Decomposition method of carbonatite |
CN116183597A (en) * | 2022-11-10 | 2023-05-30 | 长沙矿冶院检测技术有限责任公司 | Method for measuring content of calcium fluoride in ore |
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