CN104483311A - Indicator for simultaneous measurement of calcium, barium and magnesium in silicon-calcium-barium-magnesium by adopting EDTA titration method - Google Patents
Indicator for simultaneous measurement of calcium, barium and magnesium in silicon-calcium-barium-magnesium by adopting EDTA titration method Download PDFInfo
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- CN104483311A CN104483311A CN201410751285.2A CN201410751285A CN104483311A CN 104483311 A CN104483311 A CN 104483311A CN 201410751285 A CN201410751285 A CN 201410751285A CN 104483311 A CN104483311 A CN 104483311A
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Abstract
The invention relates to an indicator for simultaneous measurement of calcium, barium and magnesium in silicon-calcium-barium-magnesium by adopting an EDTA titration method. The indicator is characterized in that when the content of calcium and barium is to be measured, a calcein-alizarin mixed indicator is used; when the content of calcium and magnesium is to be measured, an o-cresolphthalein complexing agent is taken as the indicator; when the content of calcium is to be measured, a calcium indicator is used. The indicator has the advantages that unhooking operation is more convenient and labor-saving; hook closing is more reliable; the indicator is sensitive and rapid; errors caused by inaccurate observation of human eyes at the end point are reduced; EDTA complexometric titration is adopted for simultaneous measurement of calcium, barium and magnesium in the silicon-calcium-barium-magnesium, so that simultaneous measurement of the three elements calcium, barium and magnesium can be implemented in the same solution by just dissolving a sample by one time.
Description
Technical field
The invention belongs to ferroalloy analysis technical field, relate to the indicator of calcium, barium, magnesium in a kind of EDTA complexometry translocation Si-Ca-Ba-Mg.
background technology
Si―Si bond is a kind of new and effective double deoxidizer, desulfurizing agent, is mainly used in deoxidation in molten steel, dephosphorization.It can imitate the impurity in removing steel, changes the character of steel inclusion.Make molten steel purifying, improve the quality of steel.Applications well prospect is had in metallurgical industry.Therefore measure calcium, barium, content of magnesium in Si―Si bond to have a very important role.
The complexometric indicator that EDTA complexometry is commonly used has calcon-carboxylic acid, calcein, o-cresolphthalein complexone, eriochrome black T etc., and the mixed indicator that various indicator is mixed to get in proportion.Different volumetric soiutions, has different ions and proportioning, so also there is difference to different indicator response effects.Thus need to select most suitable indicator to measure its corresponding component.
Summary of the invention
The object of the invention is to solve existing complexometry reaction slower, the impact that some indicator can exist hangover and ossify, make the indicator of selection that terminal variable color can be made sensitive and easily visual color, analysis result just more accurately and reliably, provide calcium barium magnesium indicator in a kind of EDTA titrimetry translocation Si-Ca-Ba-Mg.
Technical scheme of the present invention is as follows:
Calcium barium magnesium indicator in a kind of EDTA titrimetry translocation Si-Ca-Ba-Mg, when measuring calcium barium resultant, selects calcein-alizarin mixed indicator; When measuring calcium magnesium resultant, select o-cresolphthalein complexone as indicator; Measure calcium content, select calcon-carboxylic acid.
The compound method of described calcein-alizarin mixed indicator: take the potassium chloride porphyrize mixing after calcein 1g, alizarin 1g and 100g oven dry;
The compound method of described o-cresolphthalein complexone: 1g o-cresolphthalein complexone and 100g dry after potassium chloride porphyrize mix;
The compound method of described calcon-carboxylic acid: 1g standard calcium indicator and 100g dry after potassium chloride porphyrize mix.
Advantage of the present invention is: sensitive, quick: complexometry reaction is comparatively slow, the impact that some indicator can exist hangover and ossify.And select the indicator in the present invention that colour developing can be made more sensitive, the eye-observation inaccurate error brought when reducing terminal, adopt calcium, barium, magnesium in EDTA complexometry translocation Si-Ca-Ba-Mg, only need carry out once molten sample, just can complete the Simultaneously test of calcium, barium, magnesium three kinds of elements under same solution.
Embodiment
1. method summary:
Take sample and (carry out blank test in company with sample) in polytetrafluoroethylene beaker, add nitric acid dissolve sample, drip hydrofluorite and dissolve completely to sample, emit perchloric acid cigarette.Adding hydrochloric acid makes salt dissolve, and is transferred to beaker, drips ammoniacal liquor and is separated.First measure calcium barium resultant, need control ph, eliminate the impact of magnesium with the form precipitated.Measure calcium magnesium resultant, add potassium sulfate and generate the impact that barium sulphate eliminates barium.Finally measure calcium, control ph adds potassium sulfate simultaneously, eliminates the impact of barium magnesium simultaneously.
2. reagent:
The density of nitric acid is 1.42g/mL;
The density of hydrofluorite is 1.15g/mL;
The density of hydrochloric acid is 1.19g/mL;
The density of perchloric acid is 1.67g/mL;
Oxammonium hydrochloride used is solid;
In triethanolamine solution, the volume ratio of triethanolamine and water is 1:4;
The ammoniacal liquor of ammonia spirit to be density be 0.90g/mL mixes with isopyknic water.The concentration of potassium hydroxide solution is 200g/L;
The concentration of ammonium chloride solution is 10g/L;
The concentration of potassium sulfate solution is 100g/L;
The concentration of EDTA standard solution is 0.007mol/L;
The compound method of the ammonia-ammonium chloride buffer solution of pH=10: 67g ammonium chloride is dissolved in 200mL water, adding 570mL density is in the ammoniacal liquor of 0.90g/mL, mixing;
The compound method of calcein-alizarin mixed indicator: take calcein 1g, the potassium chloride porphyrize mixing after alizarin 1g and 100g oven dry;
The compound method of calcon-carboxylic acid: 1g standard calcium indicator and 100g dry after potassium chloride porphyrize mix;
The compound method of calcein: 1g calcein and 100g dry after potassium chloride porphyrize mix;
The compound method of calcein-alizarin mixed indicator: take calcein 1g, the potassium chloride porphyrize mixing after alizarin 1g and 100g oven dry;
The compound method of calcein-thymol blue mixed indicator: take calcein 1g, the potassium chloride porphyrize mixing after thymol blue 1g and 100g oven dry;
The compound method of calcein-phenolphthalein mixed indicator: take calcein 1g, the potassium chloride porphyrize mixing after phenolphthalein 1g and 100g oven dry;
O-cresolphthalein complexone: 1g o-cresolphthalein complexone and 100g dry after potassium chloride porphyrize mix.
The compound method of o-cresolphthalein complexone-thymol blue mixed indicator: take o-cresolphthalein complexone 1g, the potassium chloride porphyrize mixing after thymol blue 1g and 100g oven dry;
Eriochrome black T: 1g eriochrome black T and 100g dry after potassium chloride porphyrize mix.
Acid chromium blue k: 5g/L, prepares with triethanolamine (volume ratio of triethanolamine and water is 1:1).
Naphthol green B: 5g/L, prepares with triethanolamine (volume ratio of triethanolamine and water is 1:1).
3. sample size
Take sample 0.2500g.
4. analytical procedure
Take 0.2500g sample and (carry out blank test in company with sample) in 250mL polytetrafluoroethylene beaker, add 10mL nitric acid (density is 1.42g/mL) dissolved samples, drip hydrofluorite (density is 1.15g/mL) to dissolve completely to sample, add 10mL perchloric acid (density is 1.67g/mL), heating emits perchloric acid cigarette to dry to the greatest extent.Adding hydrochloric acid solution 10mL (density is that the hydrochloric acid of 1.19g/mL mixes with water equal-volume) makes salt dissolve, and is transferred to beaker, drips ammoniacal liquor (ammoniacal liquor of ammonia spirit to be density be 0.90g/mL mixes with isopyknic water) and is separated.Filter in 250mL volumetric flask, shake up after constant volume.
Divide and get 50mL filtrate in 250mL beaker, add oxammonium hydrochloride (solid) 0.2g, triethanolamine solution (volume ratio of triethanolamine and water is 1:4) is sheltered interfering ion, add potassium sulfate solution (concentration is 100g/L) 10mL, (67g ammonium chloride is dissolved in 200mL water to add 10mL ammonia-ammonium chloride buffer solution, adding 570mL density is in the ammoniacal liquor of 0.90g/mL, mixing) control ph is 10, add indicator a little, with EDTA standard solution (concentration is for 0.007mol/L) titration, its EDTA consumption is V (Ca+Mg).
Divide and get 50mL filtrate in 250mL beaker, add oxammonium hydrochloride (solid) 0.2g, triethanolamine (volume ratio of triethanolamine and water is 1:4) is sheltered interfering ion, add potassium sulfate solution (concentration is 100g/L) 10mL, add potassium hydroxide solution (concentration is 200g/L) 40mL, control ph is 12, add indicator a little, with EDTA standard solution (concentration is for 0.007mol/L) titration, its EDTA consumption is V
ca.
Divide and get 50mL filtrate in 250mL beaker, add oxammonium hydrochloride (solid) 0.2g, triethanolamine (volume ratio of triethanolamine and water is 1:4) is sheltered interfering ion, adding potassium hydroxide solution (concentration is 200g/L) 40mL control ph is 12, add indicator a little, with EDTA standard solution (concentration is for 0.007mol/L) titration, its EDTA consumption is V
(Ca+Ba).
5. Analysis result calculation:
In above-mentioned formula: the concentration of c---EDTA standard solution, mol/L;
V
ca---in titration sample solution during calcium consume the volume of EDTA standard solution, mL;
V
ca+Ba---in titration sample solution when calcium, barium consume the volume of EDTA standard solution, mL;
V
ca+Mg---in titration sample solution when calcium, magnesium consume the volume of EDTA standard solution, mL;
M---sample mass, g;
K---sample divides liquid proportional, divides and get 50mL, so K=1/5 in the present embodiment from 250mL sample solution;
V
01---in titration blank solution during calcium consume the volume of EDTA standard solution, mL;
V
02---in titration blank solution when calcium, barium consume the volume of EDTA standard solution, mL;
V
03---in titration blank solution when calcium, magnesium consume the volume of EDTA standard solution, mL;
M
ca---the molal weight (40.08g/mol) of calcium;
M
ba---the molal weight (137.33g/mol) of barium;
M
mg---the molal weight (24.30g/mol) of magnesium.
6. sample analysis contrast
6.1 measure calcium barium resultant
Table 1 measures the contrast of calcium barium resultant indicator
| Indicator | Terminal variable color | Endpoint situation |
| Calcon-carboxylic acid | Red---pure blue | Terminal trails |
| Calcein | Fluorescein---orange | Not obvious |
| Calcein+thymol blue | Fluorescence green---bluish violet | Better |
| Calcein+alizarin | Fluorescence green---claret | Obviously |
| Calcein+phenolphthalein | Fluorescence green---red | Not obvious |
6.2 measure calcium magnesium resultant
Table 2 measures the contrast of calcium magnesium resultant indicator
| Indicator | Terminal variable color | Endpoint situation |
| O-cresolphthalein complexone | Red---brilliant white | Obviously |
| O-cresolphthalein complexone+thymol blue | Red---blue | Not obvious |
| Eriochrome black T | Claret---pure blue | Terminal trails |
| Acid chromium blue k+naphthol green B | Claret---blue-green | Better |
6.3 measure calcium content
Table 3 measures the contrast of calcium content indicator
| Indicator | Terminal variable color | Endpoint situation |
| Calcon-carboxylic acid | Red---blue | Obviously |
| Calcein | Fluorescein---orange | Not obvious |
| Calcein+thymol blue | Fluorescence green---bluish violet | Better |
| Calcein+alizarin | Fluorescence green---claret | Better |
| Calcein+phenolphthalein | Fluorescence green---red | Better |
6.4 indicator are selected
When measuring calcium barium resultant, final choice calcein-alizarin mixed indicator.Using alizarin as contrast colot, comparatively significantly terminal variable color can be observed.Alizarin is in rose-red in alkaline solution, and after mixing with calcein indicator, terminal is disappeared by fluorescence green, goes to claret, more easily observes.And alizarin is colour-fast in highly basic, also not by adsorption of magnesium hydroxide.
When measuring calcium magnesium resultant, final choice o-cresolphthalein complexone is as indicator.After adding indicator, solution is for pink, shoals gradually, finally occurs brilliant white, more easily observe close to color during terminal.And add thymol blue when carrying out contrast colot, close to the blue gradual change of terminal, make end point mutation not obvious on the contrary.
Measure calcium content, finally select calcon-carboxylic acid.Terminal becomes pure blue from redness, bright-colored, and variable color is sharp.When selecting calcein as indicator, terminal is not obvious, and result is often on the low side.And after adding contrast colot agent, terminal is comparatively obvious relatively before.
6.5 measurement result
According to the present invention the indicator selected measure Si―Si bond sample, its measurement result is as following table:
Table 4: each element determination result
Test figure shows, three kinds of selected indicator are for EDTA translocation Ca, and Ba, Mg tri-kinds of element effects are better, and data accuracy is high.
7. conclusion
By to above several mensuration calcium barium resultant, calcium magnesium resultant, the contrast of the indicator of calcium content, find to select a kind of suitable indicator can well improve the hangover of terminal and ossify, make the prominent more obvious of terminal, variable color is sharper, and then improves the accuracy of analysis result.
Claims (4)
1. a calcium barium magnesium indicator in EDTA titrimetry translocation Si-Ca-Ba-Mg, is characterized in that: when measuring calcium barium resultant, select calcein-alizarin mixed indicator; When measuring calcium magnesium resultant, select o-cresolphthalein complexone as indicator; Measure calcium content, select calcon-carboxylic acid.
2. calcium barium magnesium indicator in EDTA titrimetry translocation Si-Ca-Ba-Mg according to claim 1, is characterized in that: the compound method of described calcein-alizarin mixed indicator: take the potassium chloride porphyrize mixing after calcein 1g, alizarin 1g and 100g oven dry.
3. calcium barium magnesium indicator in EDTA titrimetry translocation Si-Ca-Ba-Mg according to claim 1, is characterized in that: the compound method of described o-cresolphthalein complexone: 1g o-cresolphthalein complexone and 100g dry after potassium chloride porphyrize mix.
4. calcium barium magnesium indicator in EDTA titrimetry translocation Si-Ca-Ba-Mg according to claim 1, is characterized in that: the compound method of described calcon-carboxylic acid: 1g standard calcium indicator and 100g dry after potassium chloride porphyrize mix.
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| CN104807793A (en) * | 2015-04-29 | 2015-07-29 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium wire |
| CN104819977A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium alloy |
| CN104819978A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-aluminum-calcium-barium alloy |
| CN104820061A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium-barium alloy |
| CN104833675A (en) * | 2015-05-20 | 2015-08-12 | 内蒙古包钢钢联股份有限公司 | Determination method of content of calcium oxide in iron ore |
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| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
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| CN104819977A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium alloy |
| CN104819978A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-aluminum-calcium-barium alloy |
| CN104820061A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium-barium alloy |
| CN104833675A (en) * | 2015-05-20 | 2015-08-12 | 内蒙古包钢钢联股份有限公司 | Determination method of content of calcium oxide in iron ore |
| CN104964976A (en) * | 2015-06-12 | 2015-10-07 | 内蒙古包钢钢联股份有限公司 | Method of measuring calcium hydroxide content in slaked lime |
| CN105092569A (en) * | 2015-08-21 | 2015-11-25 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of calcium hydroxide in carbide slag |
| CN105158405A (en) * | 2015-08-21 | 2015-12-16 | 内蒙古包钢钢联股份有限公司 | Method for continuously determining content of calcium oxide and magnesium oxide in bentonite |
| CN105092569B (en) * | 2015-08-21 | 2019-06-04 | 内蒙古包钢钢联股份有限公司 | The measuring method of calcium hydroxide content in carbide slag |
| 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 |
| 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 |
| CN109358056A (en) * | 2018-12-26 | 2019-02-19 | 西南铝业（集团）有限责任公司 | A method of 7050 zinc in aluminium alloy contents of measurement |
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