CN101750467A - Method for analyzing carbonate in limestone - Google Patents

Method for analyzing carbonate in limestone Download PDF

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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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carbonate
magnesium
limestone
calcium
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李春潮
牛利民
管督
罗梅
张继军
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Aluminum Corp of China Ltd
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Aluminum Corp of China Ltd
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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

A kind of method of analyzing carbonate in limestone
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:
Hydrolysis reaction:
Figure G2009102433745D00021
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)
Figure G2009102433745D00031
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.
CN200910243374A 2009-12-18 2009-12-18 Method for analyzing carbonate in limestone Pending CN101750467A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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

Cited By (5)

* Cited by examiner, † Cited by third party
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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Open date: 20100623