CN104977385A - Method for continuous determination of calcium oxide and magnesium oxide content of limestone and dolomite - Google Patents
Method for continuous determination of calcium oxide and magnesium oxide content of limestone and dolomite Download PDFInfo
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- CN104977385A CN104977385A CN201510323064.XA CN201510323064A CN104977385A CN 104977385 A CN104977385 A CN 104977385A CN 201510323064 A CN201510323064 A CN 201510323064A CN 104977385 A CN104977385 A CN 104977385A
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Abstract
The invention discloses a method for continuous determination of calcium oxide and magnesium oxide content of limestone and dolomite. The method comprises adding a limestone or dolomite sample into a Teflon plastic beaker, preparing a blank contrast without the limestone or dolomite sample, respectively adding hydrochloric acid and nitric acid-hydrofluoric acid into the beakers to dissolve the sample, adding perchloric acid into the beakers to produce smoke, adding hydrochloric acid into the breakers, carrying out salt heating dissolution, transferring the reagents into a big volumetric flask, carrying out dilution until the liquid level reaches to the scale and metered volume is obtained, dividing each solution in the sample and blank contrast into two parts with the same amount, orderly adding appropriate amounts of triethanolamine, water, hydroxylamine hydrochloride, a potassium hydroxide solution and calcein into one part in the sample and blank contrast, carrying out titration by an EDTA standard solution until the fluorescent green color disappears, recording the volume, calculating calcium oxide content, orderly adding appropriate amounts of triethanolamine, water, hydroxylamine hydrochloride, an ammonia-ammonium chloride buffer solution and an eriochrome black T indicator into the other part in the sample and blank contrast, carrying out titration by an EDTA standard solution until the prunosus color is changed into a blue color, recording the volume and calculating magnesium oxide content.
Description
Technical field
The present invention relates to fire resisting material field, particularly relate to calcium oxide, magnesian method for continuously measuring in a kind of volumetric determination lime stone, rauhkalk.
Background technology
Lime and lime stone are used as building materials in a large number, are also the important source material of much industry.Lime stone directly can be processed into building stones and be fired into unslaked lime, and lime has unslaked lime and white lime.The principal ingredient of unslaked lime is CaO, and general in block, pure be white, containing being light gray or faint yellow during impurity.The unslaked lime moisture absorption or add water and just become lime hydrate, lime hydrate is also white lime, and its principal ingredient is Ca (OH)
2.White lime through being deployed into calcimine, lime paste, lime mortar etc., as coating material and brick and tile bonding agent.Cement is by the mixing such as lime stone and clay, obtains through high-temperature calcination.Glass, by mixing such as lime stone, silica sand, soda ash, obtains through high-temperature fusion.Ironmaking lime masonry flux, removing gangue.Steel-making unslaked lime does slag making materials, except the objectionable impurities such as desulfuration, phosphorus.(principal ingredient is CaC to calcium carbide
2) be that unslaked lime and coke react obtained in electric furnace.Soda ash is through multistep reaction obtained (Sol dimension method) with raw materials such as lime stone, salt, ammonia.Lime hydrate and soda ash reaction is utilized to make caustic soda (causticizing process).Pure lime hydrate and chlorine reaction is utilized to obtain bleaching.The chemical process of lime stone is utilized to make the important calcium salts such as lime chloride, calcium nitrate, calcium sulfite.Lime hydrate can be temporarily rigid except what anhydrate, as water softening agent.Lime stone burns is processed into purer powder lime carbonate, is used as the inserts of rubber, plastics, paper, toothpaste, cosmetics etc.The soda-lime that lime and caustic soda are made, as the absorbing agent of carbon dioxide.Unslaked lime is used as drying agent and sanitizer.Agriculturally, the agricultural chemicals such as lime sulfur mixture, Bordeaux mixture is prepared with unslaked lime.Use in soil white lime can sweetening of the soil acidity, improve soil structure, supply needed for plant calcium element.Use lime brush trunk, can protect trees.
Oil is the lifeline of economy, and the lifeblood of national power development, who has oil, and who just has the development of 21 century.Deposit oil, participating in the transaction of petroleum futures market, is not only economic activity, but for the consideration of strategic development target.Therefore controlling petroleum resources is one of factors of outburst the war in Iraq.In state-owned sentence archaism, bread is the staff of life, and God's will is also.Lime stone is exactly the grain of cement industry, is the lifeblood of manufacture of cement.As long as cement mill produces, be unable to do without lime stone with regard to a moment, who has occupied limestone resource, and who has just occupied the development of cement industry.The war that current China cement production enterprise is contended for markets, be alternatively contention limestone resource war, therefore consortium using the limestone resource that takes advantage as one of measure realizing self-growth strategy.
Lime stone is the precious resources lime stone that purposes is extremely wide is the trade name of ls as raw mineral materials.Ls is on history of human civilization, wide in occurring in nature distribution with it, be easy to the feature that obtains and be widely used.Long production history is had as important building materials, in modern industry, lime stone is the primary raw material manufacturing cement, lime, calcium carbide, it is indispensable flux limestone in metallurgical industry, fat lime stone, after superfine grinding, is widely used in the manufacture of the products such as papermaking, rubber, paint, coating, medicine, cosmetics, feed, sealing, bonding, polishing.According to incompletely statistics, the lime stone that manufacture of cement consumes and building stone, lime production, flux for metallurgy, the ratio that calcium carbonate superfine powder consumes the summation of lime stone is 1: 3.Ls is non-renewable resources, and along with the continuous progress of science and technology and the development of nanometer technology, the application of lime stone also will be widened further.
Rauhkalk component molecules formula is CaCO
3, MgCO
3.Theoretical composition: CaO 30.4%, MgO 21.9%, CO
247.7%.Normal containing impurity such as silicon, aluminium, iron, titaniums.
Rauhkalk is carbonate mineral, has ferrodolomite and mangandolomite respectively.Its crystal structure, as kalzit, is often rhombohedron.Can slowly blebbing during chance cold dilute hydrochloric acid.Some rauhkalks irradiate at cathode ray and issue Exocarpium Citri Rubrum coloured light.Rauhkalk is the main mineral constituent of composition pierite and dolomitic limestone.Rauhkalk can be used for building materials, pottery, glass and fire resistive material, chemical industry and agricultural, environmental protection, the field such as energy-conservation.The main flux being used as basic refractory and blast furnace ironmaking; Produce calcium magnesium phosphate and preparing magnesium sulfate; And produce the batching of glass and pottery.Purposes is allocated in tire glaze in addition as flux.Some ancient kilns in the north, are everlasting in tire glaze add rauhkalk as determined kiln etc., also add rauhkalk in some color glaze in Jing Dezhen.
As basic solvent conventional in blast furnace process, be a kind of typical carbonate mineral, its principal ingredient is calcium carbonate, magnesium carbonate and a small amount of silica impurity, therefore carries out calcium oxide in lime stone, rauhkalk, magnesium oxide Accurate Determining is significant.
The xrf analysis that development in recent years is got up, achieves the instrumentation of rauhkalk sample analysis, but because of its apparatus expensive, strong to standard specimen dependence, analysis cost is improved greatly, needs the igloss carrying out sample in advance to measure simultaneously, have impact on its analysis speed, make it apply and be subject to certain limitation.Chemical analysis major part adopts platinum crucible, owing to using platinum crucible, analysis cost is improved, has higher requirement to daily management.
Summary of the invention
For overcoming the above problems, the invention provides a kind of operating process short, cost is low, and fast, efficient, accurately, good stability, is easy to the analytical approach of calcium oxide, content of magnesia in the mensuration lime stone of grasp, rauhkalk.Solve existing analytical approach long flow path, cost high problem.
For reaching above-mentioned purpose, the method for continuously measuring of calcium oxide, content of magnesia in a kind of lime stone of the present invention, rauhkalk, comprises the following steps:
In polytetrafluoroethylplastic plastic beaker, one adds quality is m lime stone or rauhkalk sample, another does not add as blank, add hydrochloric acid respectively afterwards, nitrate acid and hydrofluoric acid dissolves, add perchloric acid smoked, cigarette emits only, test solution dries up, add hydrochloric acid heating for dissolving salt afterwards again, test solution is transferred to respectively in Large Copacity bottle, be diluted to scale fixed molten, each solution divides again the solution two parts getting equivalent, be placed in four and large beaker volume is equal large beaker respectively above, portion in sample and blank adds triethanolamine successively, water, oxammonium hydrochloride, hydro-oxidation potassium solution, calcein is appropriate, being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, write down volume and be respectively V
caand V
01, another part in sample and blank adds triethanolamine, water, oxammonium hydrochloride, ammonification-ammonium chloride buffer solution successively, and it is appropriate to add chromium black T indicator, and being titrated to aubergine with the EDTA standard solution that concentration is C, to become blueness be terminal, writes down volume and be respectively V
(Mg+Ca)and V
02,
The calcium oxide content obtained is W
caO%=C (V
ca-V
01) M
caO100/m K × 1000;
The magnesian content obtained is W
mgO%=C (V
(Mg+Ca)-V
ca-(V
02-V
01) M
mgO100/m K × 1000;
In formula: M
caO: the molal weight of calcium oxide, g/mol;
M
mgO: magnesian molal weight, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V
ca: in sample, calcium consumes the volume of EDTA standard solution, mL;
V
01: the blank volume consuming EDTA standard solution during titration calcium, mL;
V
(Mg+Ca): calcium magnesium resultant consume the volume of EDTA standard solution, mL;
V
02: the blank volume consuming EDTA standard solution during titration calcium magnesium resultant, mL.
Wherein said concentration of hydrochloric acid is 65%.
Wherein said concentration of nitric acid is 67%.
Wherein said hydrofluoric acid concentration is 40%.
Wherein said perchloric acid concentration is 70%.
Wherein said triethanolamine concentrations is 12%.
Wherein said potassium hydroxide solution concentration is 20%.
The invention difference from existing technology is that the present invention achieves following technique effect:
1) fast, efficiently, low cost: the method substantially reduces operating process, has saved medicine, has reduced testing cost, improve production efficiency.
2) accurately, stable: adopt this method, be separated interference element twice with ammoniacal liquor, both measurement results are the same.Ensure that measurement result is stablized, data are accurate.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1. method summary: adopt hydrochloric acid (65%) in polytetrafluoroethylplastic plastic beaker, nitric acid (67%)-hydrofluorite (40%) dissolved samples, adds perchloric acid smoked, and cigarette emits only, and one lights a cigarette cannot see, and test solution dries up.Add 10mL hydrochloric acid (65%), heating for dissolving salt.Test solution is transferred in 250mL volumetric flask, be diluted to scale fixed molten.Divide and get 50mL solution two parts, be placed in two 250mL beakers respectively, portion adds 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), calcein is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Another part adds 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 10mL ammonia-ammonium chloride buffer solution (pH=10), add chromium black T indicator appropriate, being titrated to aubergine with EDTA standard solution, to become blueness be terminal.
2. reagent:
2.1 nitric acid (67%)
2.2 hydrofluorite (40%)
2.3 perchloric acid (70%)
2.4 hydrochloric acid (65%)
2.5 oxammonium hydrochlorides (solid)
2.6 triethanolamines (12%)
2.7 potassium hydroxide solutions (20%)
2.8 calcein indicator: 1g calcein and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
2.9EDTA standard solution C (EDTA)=0.01783mol/L
2.10 ammonia-ammonium chloride buffer solution (PH=10): 67g ammonium chloride is dissolved in 200mL water, adds 570mL strong aqua, is diluted to 1000mL. with water
2.11 chromium black T indicators: 1g eriochrome black T and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
3. sampling and sample preparation: get sample preparation standard according to fire resistive material and carry out sample and produce.
4. sample weighting amount: take sample 0.2500g
5. analytical procedure:
Specimen test: take sample m0.2500g in polytetrafluoroethylene beaker, add 10mL hydrochloric acid (65%), add 10mL hydrofluorite (40%), dissolved samples on electric hot plate, after sample major part is dissolved, add 5mL nitric acid (67%), add 5mL perchloric acid (70%), continue to be heated to perchloric acid smoked, perchloric acid cigarette emits only, cannot see one to light a cigarette, take off, add hydrochloric acid (65%) 10mL, heating for dissolving salt, test solution is transferred in 250mL volumetric flask, be diluted to scale fixed molten.From 250mL volumetric flask, divide and get 50mL solution two parts, be placed in two 250mL beakers respectively, portion adds 50mL triethanolamine (12%), and (first adds, to first the interference element such as iron and aluminium be sheltered), add 50mL water, add oxammonium hydrochloride and (add the object of oxammonium hydrochloride a little, play further masking action equally, addition general about 0.5 gram both passable.), (as buffer solution, calcium and EDTA complexing require that pH value is greater than 12, add the pH value of potassium hydroxide (20%) guarantee system to add 30mL potassium hydroxide solution (20%).), calcein indicator is appropriate, and (in order to titration end-point is sharp, terminal is good-looking.), being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Meter lower volume is V
ca.Another part adds 50mL triethanolamine (12%), adds 50mL water, adds oxammonium hydrochloride a little, add 10mL ammonia-ammonium chloride buffer solution (pH=10), add chromium black T indicator appropriate, being titrated to aubergine with EDTA standard solution, to become blueness be terminal, and meter lower volume is V
(Mg+Ca).
Blank test: in polytetrafluoroethylene beaker, add 10mL hydrochloric acid (65%), add 10mL hydrofluorite (40%), dissolved samples on electric hot plate, after sample major part is dissolved, add 5mL nitric acid (67%), add 5mL perchloric acid (70%), continue to be heated to perchloric acid smoked, perchloric acid cigarette emits only, cannot see one to light a cigarette, take off, add hydrochloric acid (65%) 10mL, heating for dissolving salt, test solution is transferred in 250mL volumetric flask, be diluted to scale fixed molten.Divide and get 50mL solution two parts, be placed in two 250mL beakers respectively, portion adds 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), calcein indicator is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Meter lower volume is V
01.Another part adds 50mL triethanolamine (12%), adds 50mL water, adds oxammonium hydrochloride a little, add 10mL ammonia-ammonium chloride buffer solution (pH=10), add network T indicator appropriate, being titrated to aubergine with EDTA standard solution, to become blueness be terminal, and meter lower volume is V
02.
6. Analysis result calculation:
W
CaO％＝C(V
Ca-V
01)M
CaO100/m K×1000；
W
MgO％＝C(V
(Mg+Ca)-V
Ca-(V
02-V
01)M
MgO100/m K×1000；
In formula: M
caO: the molal weight (g/mol) of calcium oxide;
M
mgO: magnesian molal weight (g/mol);
M: sample mass (g);
K: sample divides liquor ratio (50/250=1/5);
C:EDTA concentration of standard solution (mol/L);
V
ca: in sample, calcium consumes the volume (mL) of EDTA standard solution;
V
01: the blank volume (mL) consuming EDTA standard solution during titration calcium;
V
(Mg+Ca): calcium magnesium resultant consume the volume (mL) of EDTA standard solution;
V
02: the blank volume (mL) consuming EDTA standard solution during titration calcium magnesium resultant.
7. standard specimen analysis of control:
Accuracy:
As can be seen from the above table: the data measuring gained, accurately, and operating process is short, fast, efficiently.
8. conclusion:
Calcium oxide in rauhkalk, lime stone, magnesian content can be determined continuously accurately by the inventive method.Substantially reduce the running time, reduce energy consumption.Make determination data accurately and reliably, application obtains good effect aborning.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (7)
1. the method for continuously measuring of calcium oxide, content of magnesia in lime stone, rauhkalk, is characterized in that comprising the following steps:
In polytetrafluoroethylplastic plastic beaker, one adds quality is m lime stone or rauhkalk sample, another does not add as blank, add hydrochloric acid respectively afterwards, nitrate acid and hydrofluoric acid dissolves, add perchloric acid smoked, cigarette emits only, test solution dries up, add hydrochloric acid heating for dissolving salt afterwards again, test solution is transferred to respectively in Large Copacity bottle, be diluted to scale fixed molten, each solution divides again the solution two parts getting equivalent, be placed in four and large beaker volume is equal large beaker respectively above, portion in sample and blank adds triethanolamine successively, water, oxammonium hydrochloride, hydro-oxidation potassium solution, calcein is appropriate, being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, write down volume and be respectively V
caand V
01, another part in sample and blank adds triethanolamine, water, oxammonium hydrochloride, ammonification-ammonium chloride buffer solution successively, and it is appropriate to add chromium black T indicator, and being titrated to aubergine with the EDTA standard solution that concentration is C, to become blueness be terminal, writes down volume and be respectively V
(Mg+Ca)and V
02,
The calcium oxide content obtained is W
caO%=C (V
ca-V
01) M
caO100/m K × 1000;
The magnesian content obtained is W
mgO%=C (V
(Mg+Ca)-V
ca-(V
02-V
01) M
mgO100/m K × 1000;
In formula: M
caO: the molal weight of calcium oxide, g/mol;
M
mgO: magnesian molal weight, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V
ca: in sample, calcium consumes the volume of EDTA standard solution, mL;
V
01: the blank volume consuming EDTA standard solution during titration calcium, mL;
V
(Mg+Ca): calcium magnesium resultant consume the volume of EDTA standard solution, mL;
V
02: the blank volume consuming EDTA standard solution during titration calcium magnesium resultant, mL.
2. the method for continuously measuring of calcium oxide, content of magnesia in lime stone according to claim 1, rauhkalk, is characterized in that: described concentration of hydrochloric acid is 65%.
3. the method for continuously measuring of calcium oxide, content of magnesia in lime stone according to claim 1, rauhkalk, is characterized in that: described concentration of nitric acid is 67%.
4. the method for continuously measuring of calcium oxide, content of magnesia in lime stone according to claim 1, rauhkalk, is characterized in that: described hydrofluoric acid concentration is 40%.
5. the method for continuously measuring of calcium oxide, content of magnesia in lime stone according to claim 1, rauhkalk, is characterized in that: described perchloric acid concentration is 70%.
6. the method for continuously measuring of calcium oxide, content of magnesia in lime stone according to claim 1, rauhkalk, is characterized in that: described triethanolamine concentrations is 12%.
7. the method for continuously measuring of calcium oxide, content of magnesia in lime stone according to claim 1, rauhkalk, is characterized in that: described potassium hydroxide solution concentration is 20%.
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| CN105606762A (en) * | 2016-02-26 | 2016-05-25 | 内蒙古包钢钢联股份有限公司 | Measuring method for content of calcium oxide and magnesium oxide in open-hearth furnace slag, converter slag and electric furnace slag |
| CN105651931A (en) * | 2016-02-26 | 2016-06-08 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of calcium oxide and magnesium oxide in refined slag |
| CN105651930A (en) * | 2016-02-26 | 2016-06-08 | 内蒙古包钢钢联股份有限公司 | Method for determining calcium content of iron-calcium cored wire |
| CN105738362A (en) * | 2016-02-26 | 2016-07-06 | 内蒙古包钢钢联股份有限公司 | Method for measuring contents of calcium oxide and magnesia in iron ore |
| CN105738559A (en) * | 2016-02-26 | 2016-07-06 | 内蒙古包钢钢联股份有限公司 | Method for measuring calcium oxide and magnesium oxide content of tundish covering agent |
| CN105758852A (en) * | 2016-02-26 | 2016-07-13 | 内蒙古包钢钢联股份有限公司 | Determining method for content of calcium in high-calcium line |
| CN105784532A (en) * | 2016-04-15 | 2016-07-20 | 内蒙古包钢钢联股份有限公司 | Continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate |
| CN105911049A (en) * | 2016-04-13 | 2016-08-31 | 内蒙古包钢钢联股份有限公司 | Method for determining calcium oxide in rare earth concentrate |
| CN105910949A (en) * | 2016-04-15 | 2016-08-31 | 内蒙古包钢钢联股份有限公司 | Determination method for rare earth oxide in rare earth concentrate |
| CN106404992A (en) * | 2016-08-26 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium oxide and magnesium oxide in lime |
| CN106404763A (en) * | 2016-08-26 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium oxide and magnesium oxide in desulfurizing agent |
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| CN112067608A (en) * | 2020-09-04 | 2020-12-11 | 长沙矿冶研究院有限责任公司 | Method for measuring content of calcium oxide in scheelite |
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| CN106404763A (en) * | 2016-08-26 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium oxide and magnesium oxide in desulfurizing agent |
| CN106404993A (en) * | 2016-08-29 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Measuring method of magnesium oxide in magnesium refractory material |
| CN112067608A (en) * | 2020-09-04 | 2020-12-11 | 长沙矿冶研究院有限责任公司 | Method for measuring content of calcium oxide in scheelite |
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