CN104749319A - Rapid analysis method of calcium in coal gangue - Google Patents
Rapid analysis method of calcium in coal gangue Download PDFInfo
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- CN104749319A CN104749319A CN201310752117.0A CN201310752117A CN104749319A CN 104749319 A CN104749319 A CN 104749319A CN 201310752117 A CN201310752117 A CN 201310752117A CN 104749319 A CN104749319 A CN 104749319A
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Abstract
The invention relates to a rapid analysis method of calcium in coal gangue. Hydroxylamine hydrochloride, triethanolamine and L-cysteine are sequentially added, a reducing agent and a masking agent are utilized to eliminate interference without separation, and the content of the calcium in coal gangue can be directly titrated, and the method has the advantages of rapidness, accuracy, good reproducibility and the like; and all results have high accuracy and precision.
Description
Technical field
The present invention relates to the rapid analysis of calcium in a kind of gangue, be specifically related to the rapid analysis of calcium content in a kind of EDTA standard solution direct titration gangue.
Background technology
Gangue is the solid waste of mining and discharging in coal washing process, is a kind of black gray expandable rock lower, harder than coal with a kind of carbon content of coal seam association in coalification course.Its principal ingredient is Al
2o
3, SiO
2, also contain the Fe that quantity does not wait in addition
2o
3, CaO, MgO, Na
2o, K
2o, P
2o
5, SO
3with micro-rare element (gallium, vanadium, titanium, cobalt).
At present, in gangue, the conventional analysis assay method of calcium content is: take gangue sample and be placed in silver crucible, put into high temperature furnace, pre-burning 15 ~ 20min under the high temperature of 700 ~ 750 DEG C, take out, let cool, add NaOH, rise from low temperature, melting 30min under the high temperature of 700 ~ 750 DEG C, middle taking-up shake 1 time, takes out cooling, crucible is put into the 300mL beaker having filled about 100mL boiling water, cover surface plate, electric furnace suitably heats, after frit leaches completely, take out crucible, rinse crucible and lid with water.Under agitation once add 30mL hydrochloric acid, then add 2 ~ 5mL nitric acid, clean crucible and lid with hot hydrochloric acid (1+5).Solution is heated to the 2 ~ 3min that boils, after cooling, moves into volumetric flask constant volume, divide and get aliquot solution, the content of calcium in EDTA standard solution direct titration gangue.Analyze and measure process tedious, complex operation step.
Summary of the invention
The object of the present invention is to provide a kind of by adding oxammonium hydrochloride successively, triethanolamine, Cys, the rapid analysis of calcium content in EDTA standard solution direct titration gangue.
For achieving the above object, the present invention is by the following technical solutions:
A rapid analysis for calcium in gangue, comprises the following steps:
Gangue sample is pre-burning 15 ~ 20min under the high temperature of 700 ~ 750 DEG C, take 0.5 ± 0.1g sample in tetrafluoroethene beaker, to add 5mL red fuming nitric acid (RFNA) after water-wet, heating for dissolving 5 ~ 10min, be cooled to 20 ~ 60 DEG C, add 2 ~ 3mL perchloric acid and 5mL hydrofluorite, heating for dissolving, be evaporated to and emit perchloric acid opium, be cooled to 20 ~ 60 DEG C, add 5mL hydrofluorite, be evaporated to and emit opium, the 2mL concentrated sulphuric acid is added after cooling, heating for dissolving, being evaporated to sulfuric acid cigarette emits to the greatest extent, after taking off cooling, add 1 ~ 2mL hydrochloric acid 1+1 and 20mL water, dissolved salts is boiled in heating, move into after cooling in 100mL volumetric flask, clean beaker and constant volume,
Divide and get 20.00mL sample solution in beaker, add water rare to 50mL, add 0.2 ~ 0.3g oxammonium hydrochloride successively, 5 ~ 10mL triethanolamine 1+4,5 ~ 10mL concentration is the Cys of 10g/L, adds the potassium hydroxide solution that 10mL concentration is 200g/L, add 0.1 ~ 0.2g calcon, solution presents claret, is titrated to pure blue, is terminal with EDTA standard solution.
Rapid analysis as above, preferably, the concentration of described EDTA standard solution is about 0.01mol/L.
Rapid analysis as above, preferably, the computing formula of described calcium content is:
CaO(wt％)＝Vf
CaO/2m (I)
EDTA standard solution volume is consumed, mL during V-titration calcium amount;
F
caOthe quality of-suitable with the 1.00mLEDTA standard solution calcium oxide represented with milligram, mg/mL;
M-takes the quality of sample, g.
Beneficial effect of the present invention is: first gangue dissolves with red fuming nitric acid (RFNA) by the inventive method, adds the carbon in perchloric acid removing solution, adds the silicon in hydrofluorite removing solution, adds evaporate to dryness solution after sulfuric acid, add hydrochloric acid subsequently and make solid rapid solution.Add oxammonium hydrochloride, as reductive agent, reductive agent high-valence state metallic ion.Add triethanolamine (1+4) and Cys (10g/L), as screening agent, other metallic ion of screening agent.Subsequently with calcon, as indicator, with the titration of EDTA standard solution.The method does not need to adopt hexamethylenetetramine-cupferron precipitate and separate interference element, can direct titration, and result is stablized, and recovery testu proves measurement result accurately and reliably.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but following embodiment is only limitted to explain the present invention, and protection scope of the present invention should comprise the full content of claim, is not limited only to the present embodiment.
The reagent used in embodiment is:
Red fuming nitric acid (RFNA) (ρ=1.42g/ml), commercially available;
The concentrated sulphuric acid (ρ=1.84g/ml), commercially available;
Hydrochloric acid (1+1), concentrated hydrochloric acid and water are 1: 1 solution configured according to volume ratio;
Triethanolamine (1+4), triethanolamine and water are 1: 4 solution configured according to volume ratio;
EDTA concentration of standard solution is about 0.01mol/L.
Embodiment 1
Take 0.5000g sample (gangue sample is pre-burning 15 ~ 20min under the high temperature of 700 ~ 750 DEG C) in 100mL tetrafluoroethene beaker, to add 5mL red fuming nitric acid (RFNA) after water-wet, electric furnace dissolves 5 ~ 10min, take off slightly cold, add 2mL perchloric acid, 5mL hydrofluorite (for the first time), heating for dissolving, be evaporated to and emit perchloric acid opium, take off slightly cold, add 5mL hydrofluorite (for the second time), be evaporated to and emit opium, the 2mL concentrated sulphuric acid is added after taking off cooling, heating for dissolving, being evaporated to sulfuric acid cigarette emits to the greatest extent, after taking off cooling, add 2mL hydrochloric acid (1+1) and 20mL water heating boil dissolved salts, take off cooling, do not need to be separated, move in 100mL volumetric flask, clean beaker and constant volume.
Divide and get 20.00mL sample solution in 250mL beaker, add water rare to 50mL, add 0.2g oxammonium hydrochloride successively, 5mL triethanolamine (1+4), 5mL Cys (10g/L), add 10mL potassium hydroxide solution (200g/L), add 0.1g calcon, with EDTA standard solution (f
cao=0.6722mg/mL) be titrated to pure blue, be terminal.Consume EDTA standard solution 1.64mL, calculate through formula (I), in gangue, the massfraction of calcium is 1.10%.
Embodiment 2
Take 0.4993g sample (gangue sample is pre-burning 15 ~ 20min under the high temperature of 700 ~ 750 DEG C) in 100mL tetrafluoroethene beaker, to add 5mL red fuming nitric acid (RFNA) after water-wet, electric furnace dissolves 5 ~ 10min, take off slightly cold, add 2mL perchloric acid, 5mL hydrofluorite (for the first time), heating for dissolving, be evaporated to and emit perchloric acid opium, take off slightly cold, add 5mL hydrofluorite (for the second time), be evaporated to and emit opium, the 2mL concentrated sulphuric acid is added after taking off cooling, heating for dissolving, being evaporated to sulfuric acid cigarette emits to the greatest extent, after taking off cooling, add 1mL hydrochloric acid (1+1) and 20mL water heating boil dissolved salts, take off cooling, do not need to be separated, move in 100mL volumetric flask, clean beaker and constant volume.
Divide and get 20.00mL sample solution in 250mL beaker, add water rare to 50mL, add 0.2g oxammonium hydrochloride successively, 10mL triethanolamine (1+4), 5mL Cys (10g/L), add 10mL potassium hydroxide solution (200g/L), add 0.2g calcon, with EDTA standard solution (f
cao=0.6722mg/mL) be titrated to pure blue, be terminal.Consume EDTA standard solution 2.32mL, calculate through formula (I), in gangue, the massfraction of calcium is 1.56%.
Embodiment 3
Take 0.5026g sample (gangue sample is pre-burning 15 ~ 20min under the high temperature of 700 ~ 750 DEG C) in 100mL tetrafluoroethene beaker, to add 5mL red fuming nitric acid (RFNA) after water-wet, electric furnace dissolves 5 ~ 10min, take off slightly cold, add 3mL perchloric acid, 5mL hydrofluorite (for the first time), heating for dissolving, be evaporated to and emit perchloric acid opium, take off slightly cold, add 5mL hydrofluorite (for the second time), be evaporated to and emit opium, the 2mL concentrated sulphuric acid is added after taking off cooling, heating for dissolving, being evaporated to sulfuric acid cigarette emits to the greatest extent, after taking off cooling, add 2mL hydrochloric acid (1+1) and 20mL water heating boil dissolved salts, take off cooling, do not need to be separated, move in 100mL volumetric flask, clean beaker and constant volume.
Divide and get 20.00mL sample solution in 250mL beaker, add water rare to 50mL, add 0.3g oxammonium hydrochloride successively, 5mL triethanolamine (1+4), 10mL Cys (10g/L), add 10mL potassium hydroxide solution (200g/L), add 0.1g calcon, with EDTA standard solution (f
cao=0.6722mg/mL) be titrated to pure blue, be terminal.Consume EDTA standard solution 3.26mL, calculate through formula (I), in gangue, the massfraction of calcium is 2.18%.
Embodiment 4 sample recovery testu
Method of the present invention is adopted to carry out recovery testu to the calcium in gangue 1#, 2#, 3# respectively.Experimental result shows, the recovery (experimental result refers to table 1) between 98.2 ~ 101.0% of calcium, illustrates the measurement result of the inventive method accurately and reliably.
Table 1 sample recovery testu
Embodiment 5 Precision Experiment
The method described in embodiment 1 is adopted to carry out Precision Experiment to the calcium in gangue 4#, 5#, 6# respectively.Experiment replicate determination 6 times (n=6), the data recorded are made Mathematical Statistics Analysis, and relative standard deviation is (experimental result refers to table 2) in 1.4 ~ 2.6% scopes, illustrates that the measurement result precision of the inventive method is good.
Table 2 Precision Experiment
Claims (3)
1. the rapid analysis of calcium in gangue, it is characterized in that, the method comprises the following steps:
Gangue sample is pre-burning 15 ~ 20min under the high temperature of 700 ~ 750 DEG C, take 0.5 ± 0.1g sample in tetrafluoroethene beaker, to add 5mL red fuming nitric acid (RFNA) after water-wet, heating for dissolving 5 ~ 10min, be cooled to 20 ~ 60 DEG C, add 2 ~ 3mL perchloric acid and 5mL hydrofluorite, heating for dissolving, be evaporated to and emit perchloric acid opium, be cooled to 20 ~ 60 DEG C, add 5mL hydrofluorite, be evaporated to and emit opium, the 2mL concentrated sulphuric acid is added after cooling, heating for dissolving, being evaporated to sulfuric acid cigarette emits to the greatest extent, after taking off cooling, add 1 ~ 2mL hydrochloric acid 1+1 and 20mL water, dissolved salts is boiled in heating, move into after cooling in 100mL volumetric flask, clean beaker and constant volume,
Divide and get 20.00mL sample solution in beaker, add water rare to 50mL, add 0.2 ~ 0.3g oxammonium hydrochloride successively, 5 ~ 10mL triethanolamine 1+4,5 ~ 10mL concentration is the Cys of 10g/L, adds the potassium hydroxide solution that 10mL concentration is 200g/L, add 0.1 ~ 0.2g calcon, solution presents claret, is titrated to pure blue, is terminal with EDTA standard solution.
2. rapid analysis as claimed in claim 1, it is characterized in that, the concentration of described EDTA standard solution is about 0.01mol/L.
3. rapid analysis as claimed in claim 1 or 2, it is characterized in that, the computing formula of described calcium content is:
CaO(wt％)＝Vf
CaO/2m (I)
EDTA standard solution volume is consumed, mL during V-titration calcium amount;
F
caOthe quality of-suitable with the 1.00mLEDTA standard solution calcium oxide represented with milligram, mg/mL;
M-takes the quality of sample, g.
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| CN201310752117.0A CN104749319A (en) | 2013-12-31 | 2013-12-31 | Rapid analysis method of calcium in coal gangue |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931382A (en) * | 2015-07-09 | 2015-09-23 | 中蓝连海设计研究院 | Determination method for coal content in pyrite |
| CN106841511A (en) * | 2015-12-03 | 2017-06-13 | 北京有色金属研究总院 | The rapid analysis method of calcium, magnesium in a kind of iron ore |
Citations (5)
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|---|---|---|---|---|
| GB1424427A (en) * | 1973-04-11 | 1976-02-11 | Dow Chemical Co | Determination of calcium |
| JPS61108964A (en) * | 1984-11-01 | 1986-05-27 | Osaka Soda Co Ltd | Quantitative determination of trace calcium in aqueous solution |
| CN101344489A (en) * | 2008-09-02 | 2009-01-14 | 武汉钢铁(集团)公司 | Method for measuring calcium constituent in silicon aluminum calcium barium alloy |
| CN101701914A (en) * | 2009-10-29 | 2010-05-05 | 江西稀有金属钨业控股集团有限公司 | Analysis detection method for calcium element in ore |
| CN102636485A (en) * | 2012-03-28 | 2012-08-15 | 云南磷化集团有限公司 | Method for measuring content of calcium oxide in iron ores |
-
2013
- 2013-12-31 CN CN201310752117.0A patent/CN104749319A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1424427A (en) * | 1973-04-11 | 1976-02-11 | Dow Chemical Co | Determination of calcium |
| JPS61108964A (en) * | 1984-11-01 | 1986-05-27 | Osaka Soda Co Ltd | Quantitative determination of trace calcium in aqueous solution |
| CN101344489A (en) * | 2008-09-02 | 2009-01-14 | 武汉钢铁(集团)公司 | Method for measuring calcium constituent in silicon aluminum calcium barium alloy |
| CN101701914A (en) * | 2009-10-29 | 2010-05-05 | 江西稀有金属钨业控股集团有限公司 | Analysis detection method for calcium element in ore |
| CN102636485A (en) * | 2012-03-28 | 2012-08-15 | 云南磷化集团有限公司 | Method for measuring content of calcium oxide in iron ores |
Non-Patent Citations (1)
| Title |
|---|
| 赵树宝等: "EDTA络合滴定法测定铁矿石中钙和镁", 《冶金分析》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931382A (en) * | 2015-07-09 | 2015-09-23 | 中蓝连海设计研究院 | Determination method for coal content in pyrite |
| CN106841511A (en) * | 2015-12-03 | 2017-06-13 | 北京有色金属研究总院 | The rapid analysis method of calcium, magnesium in a kind of iron ore |
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