CN102565038B - Assaying method for Ni content in carbon material - Google Patents
Assaying method for Ni content in carbon material Download PDFInfo
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- CN102565038B CN102565038B CN201010597944.3A CN201010597944A CN102565038B CN 102565038 B CN102565038 B CN 102565038B CN 201010597944 A CN201010597944 A CN 201010597944A CN 102565038 B CN102565038 B CN 102565038B
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000243 solution Substances 0.000 claims abstract description 36
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 20
- 239000012085 test solution Substances 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 13
- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 claims abstract description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004327 boric acid Substances 0.000 claims abstract description 7
- 238000004737 colorimetric analysis Methods 0.000 claims abstract description 3
- 230000004907 flux Effects 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052573 porcelain Inorganic materials 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002835 absorbance Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000004380 ashing Methods 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- FPYYNALBDHWLNB-UHFFFAOYSA-N C(C)O.CC(C(=NO)C)=NO Chemical compound C(C)O.CC(C(=NO)C)=NO FPYYNALBDHWLNB-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 230000004927 fusion Effects 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000000470 constituent Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention relates to an assaying method for Ni content in a carbon material. The assaying method is characterized by comprising the steps of: burning the carbon material with anhydrous sodium carbonate or/and boric acid as a flux, carrying out fusion on ash obtained after burning, leaching with a dilute hydrochloric acid solution to obtain a test solution, reacting nickel and dimethylglyoxime in an alkaline medium in the existence of an oxidant to generate a soluble claret complex, and measuring Ni content by colorimetry. The assaying method for Ni content in the carbon material, provided by the invention, is simple in operation method and high in accuracy.
Description
One, technical field
The present invention relates to the determination and analysis method of Ni content in a kind of carbon materials, especially adopt the method for Ni content in spectrophotometry carbon materials.
Two, background technology
At present, the analytical approach of Ni content in unified carbon materials in industry, to the process of sample, some is more loaded down with trivial details.The determination and analysis method of prior art Ni constituent content mainly adopts the principle of atomic emission spectrum, utilization sees general instrument and reference light spectrogram and analysis mark, the spectrum of electromagnetic radiation is tested oneself evaluation, this method too relies on spectrogram on the one hand, if spectrogram distortion, very large on the impact of result; On the other hand, seldom, for the subtle change of constituent content, corresponding line strength evaluation, than being not reflected, makes measurement result deviation very large for the matrix line of Ni constituent content and element line.Therefore, the active demand that a kind of accuracy Ni method for measuring and analyzing content high, simple to operate is industry is invented.
Three, summary of the invention
Technical matters to be solved by this invention is to provide the determination and analysis method of Ni content in the carbon materials that a kind of method of operating is simple, accuracy is high.
For realizing technical matters of the present invention, concrete technical scheme is: a kind of determination and analysis method of Ni content in carbon materials, with natrium carbonicum calcinatum or/and boric acid makes flux, after ash content after carbon materials calcination is carried out melting, leach test solution with dilute hydrochloric acid solution, in alkaline medium, under oxygenant existence condition, nickel and dimethylglyoxime generate the claret complex compound of solubility, with colorimetric method for determining Ni content.
The further technical scheme of the present invention also comprises high temperature ashing for carbon materials step, takes and be laid in porcelain boat through the carbon materials of grinding in right amount, be placed in high temperature resistance furnace and slowly rise to 750 ~ 900 DEG C by room temperature, at such a temperature calcination 1 ~ 3 hour.
The further technical scheme of the present invention is loaded in platinum crucible by the carbon materials through ashing, adds appropriate natrium carbonicum calcinatum or/and boric acid, 800 ~ 900 DEG C of meltings after stirring.
The further technical scheme of the present invention be by melting after carbon materials cooling, add dissolving with hydrochloric acid, move in volumetric flask and make Sample A.
The further technical scheme of the present invention is the determination and analysis step of Ni content in Sample A:
A, point get 10.00ml Sample A solution in 100ml volumetric flask, add water 50ml, adds 10ml EWNN solution, 10ml sodium hydroxide solution, and 5ml ammonium persulfate solution, mixes;
B, add 2ml dimethylglyoxime ethanolic solution, be diluted with water to scale, mix, place 10 ~ 15 minutes;
In c, companion step (b), sample does blank test;
D, sample in step (b) is put into cuvette, at spectrophotometric wavelength 530nm place, take water as reference, measurement absorbance, deducts the absorption photometric of blank test solution, by quality working curve being found corresponding nickel.
E, be calculated as follows Ni content:
M in formula
1: the quality of the nickel checked in by working curve, ug; v
1: divide the volume getting test solution, ml; V: the cumulative volume of test solution, ml; M: the quality taking carbon materials, g.
The further technical scheme of the present invention is described EWNN solution concentration is 100g/L.
The further technical scheme of the present invention is described concentration of sodium hydroxide solution is 100g/L.
The further technical scheme of the present invention is described ammonium persulfate solution concentration is 50g/L.
The further technical scheme of the present invention is described dimethylglyoxime ethanol solution concentration is 10g/L.
The invention has the beneficial effects as follows:
1, assay method usable range of the present invention is wide, comprises mensuration and the analysis of nickel content in all carbon materialses such as petroleum coke, charcoal block, pitch.
2, the method for the invention does not need to carry out the pre-service such as filtering to sample, measures after can directly adding corresponding reagent.
3, the method for the invention is easy and simple to handle, developing time is short, and the deviation of measurement result is little.
Four, embodiment
The specific embodiment of the present invention is described in detail below in conjunction with concrete experimental data.
The present invention needs the instrument and equipment used: disc grinder, high temperature furnace, balance (0.1mg), porcelain boat, platinum crucible (with cover, 30ml), spectrophotometer, graduated cylinder.
The configuration of main agents and sample:
1, natrium carbonicum calcinatum.
2, boric acid.
3, hydrochloric acid, 3mol/L.
4, EWNN solution, 100g/ml.
5, sodium hydroxide solution, 100g/ml.
6, dimethylglyoxime ethanolic solution, 10g/ml.
7, ammonium persulfate solution, 50g/ml, now with the current.
8, the preparation of Sample A: a, get tested carbon materials sample m in disk grinding alms bowl, be ground into powder; B, accurately to take through air dried ground sample 2.0000g (m), be put in porcelain boat, pave; C, porcelain boat is put on porcelain boat frame, frame is put in high temperature box furnace fire door, fire door is left the gap into air, slowly rise to 750 ~ 900 DEG C by room temperature, calcination 1 ~ 3 hour at such a temperature (pitch should keep about 20 minutes at cold stage when burning); D, take out porcelain boat cooling, the ash content in porcelain boat is swept in the platinum crucible that 2.5g natrium carbonicum calcinatum and 0.5g boric acid are housed, carefully stirs, cover and to be placed in 800 ~ 900 DEG C of high temperature furnaces melting 20 minutes; E, the crucible having melted sample is taken out cooling from high temperature furnace, add the hydrochloric acid 30ml of 3mol/L, sample is all dissolved, as do not dissolved completely, being placed on electric furnace and boiling a few minutes; F, move in 100ml volumetric flask by the test solution cooling of dissolving, clean crucible, washing lotion moves in volumetric flask, and constant volume, shakes up and make Sample A; G, companion Sample A do blank test.
9, the preparation of nickel typical shelf solution: take 1.0000g nickel, be placed in 400ml beaker, cover surface plate, add 50ml hydrochloric acid (1+1), drip appropriate hydrogen peroxide, slow heating makes nickel dissolve completely, boils several minutes with the hydrogen peroxide of decomposing excessive, cooling, solution is moved in 1000ml volumetric flask, be diluted to scale with water, mix, this solution 1ml is containing 1.0mg nickel.
10, the preparation of nickel standard solution: pipette 20.00ml nickel typical shelf solution in 1000ml volumetric flask, be diluted with water to scale, mix, this solution 1ml contains 20ug nickel.
11, the drafting of working curve:
Pipette 0,1.00,2.00,3.00,4.00,5.00ml nickel standard solution is in one group of 100ml volumetric flask, respectively add about 50ml water, mix, add 2ml dimethylglyoxime ethanolic solution, be diluted with water to scale, mix, place 10 ~ 15 minutes, make reference with standard blank, measure absorbance at spectrophotometer 530nm place, with nickel quality for horizontal ordinate, absorbance is ordinate, drawing curve.
Concrete determination step and analytical approach:
Divide and materials solution A 10.00ml in 100ml volumetric flask, add water about 50ml, adds 10ml EWNN solution, 10ml sodium hydroxide solution, 5ml ammonium persulfate solution, mixes, and adds 2ml dimethylglyoxime ethanolic solution, be diluted with water to scale, mix, place 10 ~ 15 minutes.
Blank test is done in company with above-mentioned test solution.
Above-mentioned test solution is put into cuvette, at spectrophotometric wavelength 530nm place, take water as reference, measures absorbance, deducts the absorption photometric of blank test solution, by quality working curve being found corresponding nickel.
Be calculated as follows the mass percentage of nickel:
In formula, m
1: the quality of the nickel checked in by working curve, ug; v
1: divide the volume getting test solution, ml; V: the cumulative volume of test solution, ml; M: the quality taking carbon materials, g.
Laboratory monitoring tolerance: %
| ω(Ni) | Tolerance |
| 0.0010～0.0050 | 0.0005 |
| 0.0050～0.0100 | 0.0010 |
| 0.0100～0.0500 | 0.0050 |
Claims (1)
1. the determination and analysis method of Ni content in a carbon materials, it is characterized in that, with natrium carbonicum calcinatum or/and boric acid makes flux, after ash content after carbon materials calcination is carried out melting, leach test solution with dilute hydrochloric acid solution, in alkaline medium, under oxygenant existence condition, nickel and dimethylglyoxime generate the claret complex compound of solubility, with colorimetric method for determining Ni content; In described carbon materials, the determination and analysis method of Ni content also comprises high temperature ashing for carbon materials step, take and be laid in porcelain boat through the carbon materials of grinding in right amount, be placed in high temperature roaster and slowly rise to 750 ~ 790 DEG C by room temperature, at such a temperature calcination 1 ~ 2 hour; Carbon materials through ashing is loaded in platinum crucible, adds appropriate natrium carbonicum calcinatum or/and boric acid, 800 ~ 900 DEG C of meltings after stirring;
By the carbon materials cooling after melting, add dissolving with hydrochloric acid, move in volumetric flask and make Sample A; In Sample A, the determination and analysis step of Ni content is:
A, point get 10.00ml Sample A solution in 100ml volumetric flask, add water 50ml, adds 10ml EWNN solution, 10ml sodium hydroxide solution, and 5ml ammonium persulfate solution, mixes;
B, add 2ml dimethylglyoxime ethanolic solution, be diluted with water to scale, mix, place 10 ~ 15 minutes;
In c, companion step b, sample does blank test;
D, sample in step b being put into cuvette, at spectrophotometric wavelength 530nm place, take water as reference, measures absorbance, deducts the absorption photometric of blank test solution, by quality working curve being found corresponding nickel;
E, be calculated as follows Ni content:
M in formula
1: the quality of the nickel checked in by working curve, g; v
1: divide the volume getting test solution, ml; V: the cumulative volume of test solution, ml; M: the quality taking carbon materials, g;
Described EWNN solution concentration is 100g/L; Described concentration of sodium hydroxide solution is 100g/L; Described ammonium persulfate solution concentration is 50g/L; Described dimethylglyoxime ethanol solution concentration is 10g/L.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101408506A (en) * | 2007-10-11 | 2009-04-15 | 上海电气电站设备有限公司 | Method for measuring iron and nickel contents in cobalt-base alloy welding wire by flame atomic absorption method |
| CN101864524A (en) * | 2009-04-15 | 2010-10-20 | 中国科学院过程工程研究所 | Clean production technology for processing low-grade laterite-nickel ore by sodium carbonate alkali fusion |
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| CN101225470B (en) * | 2008-01-31 | 2010-06-09 | 曹国华 | Method for extracting nickel and cobalt from lateritic nickel by hydrochloric acid process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101408506A (en) * | 2007-10-11 | 2009-04-15 | 上海电气电站设备有限公司 | Method for measuring iron and nickel contents in cobalt-base alloy welding wire by flame atomic absorption method |
| CN101864524A (en) * | 2009-04-15 | 2010-10-20 | 中国科学院过程工程研究所 | Clean production technology for processing low-grade laterite-nickel ore by sodium carbonate alkali fusion |
Non-Patent Citations (1)
| Title |
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| 光度法测定铁矿石中钴、镍;崔东艳 等;《山东冶金》;20101220;第32卷(第6期);39-42页 * |
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Address after: Taoyuan County in Hunan province Changde city 415700 disk town Chuangyuan Industrial Park Patentee after: Suntown Technology Group Corporation Address before: Sheng Tong Industrial Park No. 109 Venus Road 410200 in Hunan province Changsha City Patentee before: Suntown Technology Group Corporation |
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Effective date of registration: 20171222 Address after: 252100 Xin Fa Hope Industrial Park, Chiping County, Liaocheng City, Shandong Patentee after: Shandong Xin hair Huayuan Aluminum Co., Ltd. Address before: Taoyuan County in Hunan province Changde city 415700 disk town Chuangyuan Industrial Park Patentee before: Suntown Technology Group Corporation |
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