CN105067605A - Method for continuously determining calcium content and iron content in limestone powder - Google Patents
Method for continuously determining calcium content and iron content in limestone powder Download PDFInfo
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- CN105067605A CN105067605A CN201510438549.3A CN201510438549A CN105067605A CN 105067605 A CN105067605 A CN 105067605A CN 201510438549 A CN201510438549 A CN 201510438549A CN 105067605 A CN105067605 A CN 105067605A
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Abstract
The present invention discloses a method for continuously determining the calcium content and the iron content in limestone powder. The method mainly comprises: separating impurities, determining iron in the filtrate by using an atomic absorption spectrometry method, adding excess EDTA, carrying out back titration on calcium in the filtrate with a CuSO4 standard solution, and finally respectively calculating the calcium content and the iron content in the sample. Compared with the method in the prior art, the method of the present invention has characteristics of simpleness, practicality and accurate and reliable result, and can meet the needs of daily analysis.
Description
Technical field
The invention belongs to analytical chemistry field, be specifically related to a kind of method of calcium and iron content in METHOD FOR CONTINUOUS DETERMINATION agstone.
Background technology
Agstone is a kind of important glaze for electric porcelain raw material, and its composition is comparatively simple, mainly containing calcium oxide, and Fe
2o
3be its objectionable impurities, iron content affects its performance such as color and luster, intensity, therefore must its content of Measurement accuracy before electroceramics batching.To the mensuration of wherein calcium and iron, because the chemical method formality of classics is excessively loaded down with trivial details.Adopt X fluorescence spectrometer to measure Fe, Al content in alumina, although analysis result is accurate, highly sensitive, instrument price is higher, can not meet the needs of routine analysis.
Current calcium can adopt EDTA compleximetry, and iron content can adopt aas determination.Owing to finishing Atomic Absorption Spectrometry test, do not affect and do EDTA complexometry calcium ion, therefore conveniently do the METHOD FOR CONTINUOUS DETERMINATION of iron and calcium content.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the invention provides a kind of simple and practical, the method for calcium and iron content in tie-in Ding Zhang village soil.
Technical scheme: for achieving the above object, the invention provides a kind of method of METHOD FOR CONTINUOUS DETERMINATION agstone calcium and iron content, mainly comprises the following steps:
A () joins iron standard solution, do iron content typical curve.
B () calculates CuSO
4to EDTA standard solution volume ratio K;
(c) tekite limestone flour, the filtrate of preparation removing impurities;
D () uses aas determination iron;
E () adds excessive EDTA, use CuSO
4calcium in standard solution back titration filtrate;
The calcium of (f) difference calculation sample and iron content.
As preferably, in described step (a), join iron standard solution, doing iron content typical curve is:
Accurately take di-iron trioxide 0.2860 gram in beaker, add 1+1 hydrochloric acid 20 milliliters, slowly be heated to di-iron trioxide dissolve completely, quantitatively transfer in 200 milliliters of volumetric flasks after being cooled to 25 DEG C, with deionized water rinsing beaker three times, washing fluid also proceeds in volumetric flask, is finally settled to scale with deionized water, shake up, this solution is containing Fe1.0mg/mL.The iron standard solution getting 5mL1.0mg/mL, in 100mL volumetric flask, is diluted to scale with deionized water, shakes up, and this solution is the iron standard solution of 50 μ g/mL.Draw the iron standard solution 1.0 of 50 μ g/mL, 3.0mL respectively in two 50 milliliters of volumetric flasks with transfer pipet, be diluted to scale with deionized water, shake up, be made into 1.0,3.0 μ g/mL iron standard solution.The operation steps of the instruments such as start when measuring ferric ion in solution, shutdown, standard curve making and sample tests is see the flame method part of " 5100ZL Atomic Absorption Spectrometer working specification ", according to the condition determination of element, absorption measurement is carried out to sample solution and blank solution, record measurement result.
Preferred as another kind, in described step (b), calculate CuSO
4as follows to the method for EDTA standard solution volume ratio K: pipette volume be the EDTA standard solution of A in Erlenmeyer flask, add suitable quantity of water, the acetic acid-ammonium acetate buffer of pH=4.5, methylene red salt indicator, use CuSO
4standard solution drops to grass green and appears as terminal, writes down CuSO
4volume V
k, by K=A/V
kcalculating K; Wherein A is positive count.
Preferred as another kind, in described step (c), tekite limestone flour, the method of the filtrate of preparation removing impurities is as follows: with parts by weight, take 0.5 part of agstone (taking front 110 DEG C of dryings 2 hours) and 1-3 part mixed flux in container, stir evenly, after 880 DEG C of melting 20-40 minutes, peel off sample bead and put into beaker in tall form, add hydrochloric acid, heating stirring and dissolving is extracted, constant volume, shake up, for subsequent use.
Further preferably, described mixed flux is that 1 part of Anhydrous potassium carbonate or natrium carbonicum calcinatum and 1-5 part borax anhydrous mix porphyrize, to obtain final product.
Preferred as another kind, in described step (d), as follows by the method for aas determination iron:
Sample to be measured is swayed evenly, ensure that sample is representative.Get appropriate sample to pour in beaker, if sample is muddy, containing insoluble object or impurity, available qualitative filter paper is filled in beaker.Little by little, marginally add 1+1 hydrochloric acid, or 3mol/LNaOH solution tests its pH value with PH test paper simultaneously, make its pH value reach 3 ~ 4.If the material having other insoluble generates, filter with qualitative filter paper, shake up.See the flame method part of " 5100ZL Atomic Absorption Spectrometer working specification ", according to the condition determination of element, absorption measurement is carried out to sample solution and blank solution, record measurement result, if institute's test sample product solution concentration exceeds the scope of typical curve, reply sample solution quantitatively dilutes.
Preferred as another kind, in described step (e), add excessive EDTA, use CuSO
4in standard solution back titration filtrate, the method for calcium is as follows:
Get step (d) measure iron content after solution, add excessive EDTA standard solution, boil, drip 0.2% p-nitrophenol, then drip 1+1 ammoniacal liquor, then the hydrochloric acid dripping 1+1 is adjusted to yellow disappearance, make pH=4.2, boil 3 minutes, be cooled to room temperature.Add the acetic acid-ammonium acetate buffer solution of PH=4.5, and drip the Nitroso R salt indicator of 0.2%, use CuSO
4solution drops to solution and becomes grass green, and writing down and consuming volume is V2.
In described step (f), calcium and the iron content formula of the inventive method calculation sample are as follows:
Fe
2o
3content reference standard curve
001"/>
In formula: TCaO represents the buffer solution at pH=4.5 respectively, with the respective titer under the Nitroso R salt indicator condition of 0.2%, refer to the quality of the measured matter that the vs (standard solution) of every 1mL volumetric molar concentration is suitable.Computing formula is: TB/A=mA/VB (B index liquid, A refers to measured object, and unit is g/mL).
Beneficial effect: the present invention is relative to prior art, and method simple practical, result accurately and reliably, can meet the needs of routine analysis.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Following examples agents useful for same purity is pure for analyzing, and water used is redistilled water, and related solution is formulated as follows:
The EDTA standard solution of 0.01mol/L: take 3.8g disodium ethylene diamine tetraacetate on analytical balance, is dissolved in 100mL deionized water, and low-grade fever is transferred in 500mL reagent bottle, then added 400mL deionized water, shake up after dissolving.If any muddiness, should filter.With CaCO
3for primary standard substance demarcates EDTA solution.
The CuSO4 standard solution of 0.03mol/L: 7.5g copper sulphate (CuSO
45H2O) water-soluble, add 0.8mL sulfuric acid, proceed in 1L tubualted bottle, be diluted with water to 1L, shake up.Demarcate with the EDTA standard solution of 0.01mol/L.
Acetic acid-ammonium acetate buffer (pH4.5): get ammonium acetate 7.7g, the 50mL that adds water adds glacial acetic acid 6mL and makes into 100mL with appropriate water, to obtain final product after dissolving.
0.2% methylene red salt indicator solution: take 0.2g indicator and be dissolved in the ethanol of 100mL60%.PH color change interval 4.4-6.2.
1+1 hydrochloric acid: the distilled water adding 1 volume in beaker, the method entering water with acid adds the concentrated hydrochloric acid of 1 volume again under glass bar stirs in beaker.
1+1 ammoniacal liquor: prepare containing ammonia 25-28% industrial ammonia and distilled water volume ratio 1:1.
0.2% p-nitrophenyl phenol solution: take 0.2g p-nitrophenol indicator and be dissolved in ethanol, and dilute 100mL.
The major experimental instrument used is as follows:
High frequency fusion machine: German Herzog company high frequency fusion machine, model: HAG-M-HF.
Atomic Absorption Spectrometer, PE5100ZL.
A method for METHOD FOR CONTINUOUS DETERMINATION agstone calcium and iron content, mainly comprises the following steps:
A () joins iron standard solution, do iron content typical curve: accurately take di-iron trioxide 0.2860 gram in beaker, add 1+1 hydrochloric acid 20 milliliters, slowly be heated to di-iron trioxide dissolve completely, quantitatively transfer in 200 milliliters of volumetric flasks after being cooled to 25 DEG C, with deionized water rinsing beaker three times, washing fluid also proceeds in volumetric flask, finally be settled to scale with deionized water, shake up, obtain the iron standard solution containing Fe1.0mg/mL; Get the iron standard solution of 5mL containing 1.0mg/mL in 100mL volumetric flask, be diluted to scale with deionized water, shake up, obtain the iron standard solution containing 50 μ g/mL; Draw iron standard solution 1.0mL, 3.0mL of 50 μ g/mL respectively in two 50 milliliters of volumetric flasks with transfer pipet, be diluted to scale with deionized water, shake up, be made into 1.0 μ g/mL, 3.0 μ g/mL iron standard solution respectively; The operation steps of the instruments such as start when measuring ferric ion in solution, shutdown, standard curve making and sample tests is see the flame method part of " 5100ZL Atomic Absorption Spectrometer working specification ", according to the condition determination of element, absorption measurement is carried out to sample solution and blank solution, record measurement result.
B () calculates CuSO
4to EDTA standard solution volume ratio K: pipette volume be the EDTA standard solution of A in Erlenmeyer flask, add suitable quantity of water, the acetic acid-ammonium acetate buffer of pH=4.5, methylene red salt indicator, use CuSO
4standard solution drops to grass green and appears as terminal, writes down CuSO
4volume V
k, by K=A/V
kcalculating K; Wherein A is positive count.
(c) tekite limestone flour, the filtrate of preparation removing impurities: tekite limestone flour, the method for filtrate of preparation removing impurities is as follows: with parts by weight, takes 0.5 part of agstone and 1-3 part mixed flux in container, stir evenly, after 880 DEG C of melting 20-40 minutes, peel off sample bead and put into beaker in tall form, add hydrochloric acid, heating stirring and dissolving is extracted, constant volume, shakes up, for subsequent use.Described mixed flux is that 1 weight portion Anhydrous potassium carbonate or natrium carbonicum calcinatum and 1-5 weight portion borax anhydrous mix porphyrize, to obtain final product.
D () uses aas determination iron: swayed sample to be measured evenly, getting appropriate sample pours in beaker, if sample is muddy, containing insoluble object or impurity, available qualitative filter paper is filled in beaker, drip 1+1 hydrochloric acid, or 3mol/LNaOH solution tests its pH value with PH test paper simultaneously, makes its pH value reach 3 ~ 4; If the material having other insoluble generates, filter with qualitative filter paper, shake up; By the flame method part of " 5100ZL Atomic Absorption Spectrometer working specification ", according to the condition determination of element, absorption measurement is carried out to sample solution and blank solution, record measurement result, if institute's test sample product solution concentration exceeds the scope of typical curve, reply sample solution quantitatively dilutes.
E () adds excessive EDTA, use CuSO
4calcium in standard solution back titration filtrate: add excessive EDTA, use CuSO
4in standard solution back titration filtrate, the method for calcium is as follows: get step (d) measure iron content after solution, add excessive EDTA standard solution, boil, drip 0.2% p-nitrophenol, then drip 1+1 ammoniacal liquor, then the hydrochloric acid dripping 1+1 is adjusted to yellow disappearance, makes pH=4.2, boil 3 minutes, be cooled to 25 DEG C; Add the acetic acid-ammonium acetate buffer solution of PH=4.5, and drip the Nitroso R salt indicator of 0.2%, use CuSO
4solution drops to solution and becomes grass green, and writing down and consuming volume is V2.
The calcium of (f) difference calculation sample and iron content:
Calcium and the iron content formula of the inventive method calculation sample are as follows:
Fe
2o
3content reference standard curve
002"/>
In formula: TCaO represents the buffer solution at pH=4.5 respectively, with the respective titer under the Nitroso R salt indicator condition of 0.2%, refer to the quality of the measured matter that the vs of every 1mL volumetric molar concentration is suitable; Computing formula is: T
b/A=m
a/ VB, wherein B index liquid, A refers to measured object, and unit is g/mL.
Iron content % | Calcium content % | |
Standard value | 0.08 | 56.48 |
1st time | 0.08 | 56.50 |
2nd time | 0.08 | 56.45 |
3rd time | 0.08 | 56.48 |
Absolute error | 0.00 | 0.05 |
Relative error | 0 | 0.09% |
Adopt the method for Xray fluorescence spectrometer | 0.06 | 56.40 |
Conclusion: adopt Xray fluorescence spectrometer testing stone limestone flour, although test process is simple to operation, the method in measurement result degree of accuracy patent not like this.
Claims (8)
1. a method for METHOD FOR CONTINUOUS DETERMINATION agstone calcium and iron content, is characterized in that, mainly comprises the following steps:
A () joins iron standard solution, do iron content typical curve;
B () calculates CuSO
4to EDTA standard solution volume ratio K;
(c) tekite limestone flour, the filtrate of preparation removing impurities;
D () uses aas determination iron;
E () adds excessive EDTA, use CuSO
4calcium in standard solution back titration filtrate;
The calcium of (f) difference calculation sample and iron content.
2. the method for a kind of METHOD FOR CONTINUOUS DETERMINATION agstone calcium according to claim 1 and iron content, it is characterized in that, in described step (a), join iron standard solution, doing iron content typical curve method is: accurately take di-iron trioxide 0.2860 gram in beaker, add 1+1 hydrochloric acid 20 milliliters, slowly be heated to di-iron trioxide dissolve completely, quantitatively transfer in 200 milliliters of volumetric flasks after being cooled to 25 DEG C, with deionized water rinsing beaker three times, washing fluid also proceeds in volumetric flask, finally be settled to scale with deionized water, shake up, obtain the iron standard solution containing Fe1.0mg/mL, get the iron standard solution of 5mL containing 1.0mg/mL in 100mL volumetric flask, be diluted to scale with deionized water, shake up, obtain the iron standard solution containing 50 μ g/mL, draw iron standard solution 1.0mL, 3.0mL of 50 μ g/mL respectively in two 50 milliliters of volumetric flasks with transfer pipet, be diluted to scale with deionized water, shake up, be made into 1.0 μ g/mL, 3.0 μ g/mL iron standard solution respectively, the operation steps of the instruments such as start when measuring ferric ion in solution, shutdown, standard curve making and sample tests is see the flame method part of " 5100ZL Atomic Absorption Spectrometer working specification ", according to the condition determination of element, absorption measurement is carried out to sample solution and blank solution, record measurement result.
3. the method for a kind of METHOD FOR CONTINUOUS DETERMINATION agstone calcium according to claim 1 and iron content, is characterized in that, in described step (b), calculate CuSO
4as follows to the method for EDTA standard solution volume ratio K: pipette volume be the EDTA standard solution of A in Erlenmeyer flask, add suitable quantity of water, the acetic acid-ammonium acetate buffer of pH=4.5, methylene red salt indicator, use CuSO
4standard solution drops to grass green and appears as terminal, writes down CuSO
4volume V
k, by K=A/V
kcalculating K; Wherein A is positive count.
4. the method for a kind of METHOD FOR CONTINUOUS DETERMINATION agstone calcium according to claim 1 and iron content, is characterized in that, in described step (c), tekite limestone flour, the method for filtrate of preparation removing impurities is as follows: with parts by weight, takes 0.5 part of agstone and 1-3 part mixed flux in container, stir evenly, after 880 DEG C of melting 20-40 minutes, peel off sample bead and put into beaker in tall form, add hydrochloric acid, heating stirring and dissolving is extracted, constant volume, shakes up, for subsequent use.
5. the method for a kind of METHOD FOR CONTINUOUS DETERMINATION agstone calcium according to claim 3 and iron content, is characterized in that, described mixed flux is that 1 weight portion Anhydrous potassium carbonate or natrium carbonicum calcinatum and 1-5 weight portion borax anhydrous mix porphyrize, to obtain final product.
6. the method for a kind of METHOD FOR CONTINUOUS DETERMINATION agstone calcium according to claim 1 and iron content, it is characterized in that, in described step (d), as follows by the method for aas determination iron: sample to be measured to be swayed evenly, getting appropriate sample pours in beaker, if sample is muddy, containing insoluble object or impurity, available qualitative filter paper is filled in beaker, drip 1+1 hydrochloric acid, or 3mol/LNaOH solution tests its pH value with PH test paper simultaneously, its pH value is made to reach 3 ~ 4; If the material having other insoluble generates, filter with qualitative filter paper, shake up; By the flame method part of " 5100ZL Atomic Absorption Spectrometer working specification ", according to the condition determination of element, absorption measurement is carried out to sample solution and blank solution, record measurement result, if institute's test sample product solution concentration exceeds the scope of typical curve, reply sample solution quantitatively dilutes.
7. the method for a kind of METHOD FOR CONTINUOUS DETERMINATION agstone calcium according to claim 1 and iron content, is characterized in that, in described step (e), adds excessive EDTA, uses CuSO
4in standard solution back titration filtrate, the method for calcium is as follows: get step (d) measure iron content after solution, add excessive EDTA standard solution, boil, drip 0.2% p-nitrophenol, then drip 1+1 ammoniacal liquor, then the hydrochloric acid dripping 1+1 is adjusted to yellow disappearance, makes pH=4.2, boil 3 minutes, be cooled to 25 DEG C 25 DEG C; Add the acetic acid-ammonium acetate buffer solution of PH=4.5, and drip the Nitroso R salt indicator of 0.2%, use CuSO
4solution drops to solution and becomes grass green, and writing down and consuming volume is V2.
8. the method for a kind of METHOD FOR CONTINUOUS DETERMINATION agstone calcium according to claim 1 and iron content, is characterized in that, in described step (f), calcium and the iron content formula of the inventive method calculation sample are as follows:
fe 2 o 3 content reference standard curve
In formula: TCaO represents the buffer solution at pH=4.5 respectively, with the respective titer under the Nitroso R salt indicator condition of 0.2%, refer to the quality of the measured matter that the vs of every 1mL volumetric molar concentration is suitable; Computing formula is: T
b/A=m
a/ VB, wherein B index liquid, A refers to measured object, and unit is g/mL.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106918591A (en) * | 2015-12-28 | 2017-07-04 | 立邦涂料(中国)有限公司 | The assay method of iron tramp in a kind of inner and external wall putty for building and powdered whiting |
CN106918591B (en) * | 2015-12-28 | 2020-01-17 | 立邦涂料(中国)有限公司 | Method for measuring iron impurities in interior and exterior wall putty for building and heavy calcium carbonate |
CN116990249A (en) * | 2023-09-26 | 2023-11-03 | 北京挑战农业科技有限公司 | Method for measuring content of ferrous ions in liquid and application thereof |
CN116990249B (en) * | 2023-09-26 | 2024-01-30 | 北京挑战农业科技有限公司 | Method for measuring content of ferrous ions in liquid and application thereof |
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Application publication date: 20151118 |