CN104977270A - Analysis method of carbon element in Mo1 pure molybdenum - Google Patents
Analysis method of carbon element in Mo1 pure molybdenum Download PDFInfo
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- CN104977270A CN104977270A CN201410145679.3A CN201410145679A CN104977270A CN 104977270 A CN104977270 A CN 104977270A CN 201410145679 A CN201410145679 A CN 201410145679A CN 104977270 A CN104977270 A CN 104977270A
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- Prior art keywords
- carbon
- pure molybdenum
- analytical approach
- analysis method
- sulfur
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 52
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 37
- 239000011733 molybdenum Substances 0.000 title claims abstract description 37
- 238000004458 analytical method Methods 0.000 title claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 12
- 239000011593 sulfur Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 239000010937 tungsten Substances 0.000 claims description 9
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 claims description 8
- 239000007769 metal material Substances 0.000 abstract description 4
- 230000004907 flux Effects 0.000 abstract description 3
- AWXLLPFZAKTUCQ-UHFFFAOYSA-N [Sn].[W] Chemical compound [Sn].[W] AWXLLPFZAKTUCQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
An analysis method of carbon element in Mo1 pure molybdenum. The invention relates to the analysis method of carbon element in metal materials, and aims to solve technical problems of high deviation and low accurate degree in an analysis method of the carbon element in Mo1 pure molybdenum in the prior art. The analysis method includes following steps: (1) switching-on and pre-heating a carbon and sulfur analyzer for analyzing carbon elements through an infrared absorption method ; (2) burning an infrared ultralow carbon and sulfur crucible; (3) cooling the burned crucible in a dryer; (4) when the carbon and sulfur analyzer is pre-heated, weighing the Mo1 pure molybdenum, inputting weight values, and adding iron chip and a tungsten-tin flux; and (5) performing measurement according to the analytic methods of the instrument to obtain an analytic result, thereby completing the analysis of the carbon element in the Mo1 pure molybdenum. The analysis method is significantly reduced in deviation and is greatly increased in accuracy. The analysis method is applied in the field of analysis of the carbon element in metal materials.
Description
Technical field
The present invention relates to the analytical approach of carbon in a kind of metal material.
Background technology
The fusing point of the pure molybdenum of Mo1 (Mo1 is a trade mark of pure molybdenum) is high, good heat conductivity, thermal expansivity are little, resistance is little, evaporating pressure is low, and elastic modulus is high, has good heat resistance.But its high temperature oxidation resistance is poor, room temperature ductility is not good.
In the pure molybdenum of Mo1, the analysis of carbon is generally utilize infrared absorption method, adopts carbon and sulfur analytical instrument, uses super low carbon and sulphur crucible, adds tungsten stannum fluxing agent and measure, and its chemical analysis results deviation is comparatively large, and order of accuarcy is lower.
Summary of the invention
The present invention is that the analysis result deviation that the analytical approach that will solve carbon in the pure molybdenum of existing Mo1 exists is large, the technical matters that order of accuarcy is low, thus the analytical approach providing carbon in the pure molybdenum of a kind of Mo1.
In the pure molybdenum of a kind of Mo1 of the present invention, the analytical approach of carbon is carried out according to the following steps:
Step one: carbon and sulfur analytical instrument infrared absorption method being analyzed carbon switches on power, preheating 2 ~ 4h;
Step 2: by low for infrared excess carbon-sulfur crucible at 1000 ~ 1500 DEG C of calcination 20 ~ 30min;
Step 3: the crucible after step 2 calcination is put in exsiccator and cools, cool time is 1 ~ 3h;
Step 4: after carbon and sulfur analytical instrument preheating terminates in step one, take the pure molybdenum of bits shape Mo1 of 0.2 ~ 0.5g, input weight value, adds the iron filings of 0.3 ~ 0.6g and the tungsten stannum fluxing agent of 0.3 ~ 0.6g;
Step 5: measure according to the analytical approach of instrument, record analysis result, namely completes the analysis of carbon in the pure molybdenum of Mo1.
The present invention includes following beneficial effect:
The analysis of carbon in the pure molybdenum of Mo1 of the present invention, use the crucible after high temperature sintering, the potpourri of iron filings and tungsten stannum fluxing agent is as flux, so not only effectively can reduce the blank value of crucible, make the abundant melting of material, carbon discharges well, and deviation obviously reduces, and accuracy improves greatly.
Embodiment
Embodiment one: in the pure molybdenum of a kind of Mo1 of present embodiment, the analytical approach of carbon is carried out according to the following steps:
Step one: carbon and sulfur analytical instrument infrared absorption method being analyzed carbon switches on power, preheating 2 ~ 4h;
Step 2: by low for infrared excess carbon-sulfur crucible at 1000 ~ 1500 DEG C of calcination 20 ~ 30min;
Step 3: the crucible after step 2 calcination is put in exsiccator and cools, cool time is 1 ~ 3h;
Step 4: after carbon and sulfur analytical instrument preheating terminates in step one, take the pure molybdenum of bits shape Mo1 of 0.2 ~ 0.5g, input weight value, adds the iron filings of 0.3 ~ 0.6g and the tungsten stannum fluxing agent of 0.3 ~ 0.6g;
Step 5: measure according to the analytical approach of instrument, record analysis result, namely completes the analysis of carbon in the pure molybdenum of Mo1.
Present embodiment comprises following beneficial effect:
The analysis of carbon in the pure molybdenum of present embodiment Mo1, use the crucible after high temperature sintering, the potpourri of iron filings and tungsten stannum fluxing agent is as flux, so not only effectively can reduce the blank value of crucible, make the abundant melting of material, carbon discharges well, and deviation obviously reduces, and accuracy improves greatly.
Embodiment two: present embodiment and embodiment one are unlike preheating 3h in step one.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: in step 2 by low for infrared excess carbon-sulfur crucible at 1200 ~ 1500 DEG C of calcination 25 ~ 30min.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: in step 2 by low for infrared excess carbon-sulfur crucible at 1350 DEG C of calcination 25min.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: in step 3, cool time is 2h.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are unlike the pure molybdenum of bits shape Mo1 that takes 0.2g in step 4.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are unlike the iron filings that add 0.3g in step 4.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven are unlike the tungsten stannum fluxing agent that adds 0.3g in step 4.Other is identical with one of embodiment one to seven.
By following verification experimental verification beneficial effect of the present invention:
Test one: in the pure molybdenum of a kind of Mo1 of this test, the analytical approach of carbon realizes according to the following steps:
Step one: carbon and sulfur analytical instrument infrared absorption method being analyzed carbon switches on power, preheating 3h;
Step 2: by low for infrared excess carbon-sulfur crucible at 1350 DEG C of calcination 25min;
Step 3: the crucible after step 2 calcination is put in exsiccator and cools, cool time is 2h;
Step 4: after carbon and sulfur analytical instrument preheating terminates in step one, take the pure molybdenum of bits shape Mo1 of 0.2g, input weight value, adds the iron filings of 0.3g and the tungsten stannum fluxing agent of 0.3g;
Step 5: measure according to the analytical approach of instrument, record analysis result, namely completes the analysis of carbon in the pure molybdenum of Mo1.
Use former method and the inventive method to carry out chemical analysis test to entering factory's starting material, result is as shown in table 1:
Table 1
As shown in Table 1, in the sample that the present invention records, carbon content is all low than former method, and in the pure molybdenum of Mo1 that records of the present invention carbon element content closer to the analytical test report of national non-ferrous metal and electronic material Institute of Analysis, illustrate and use the deviation of the inventive method to carbon analysis in the pure molybdenum of Mo1 obviously to reduce, accuracy improves greatly.
Claims (8)
1. the analytical approach of carbon in the pure molybdenum of Mo1, is characterized in that the analytical approach of carbon in the pure molybdenum of Mo1 is carried out according to the following steps:
Step one: carbon and sulfur analytical instrument infrared absorption method being analyzed carbon switches on power, preheating 2 ~ 4h;
Step 2: by low for infrared excess carbon-sulfur crucible at 1000 ~ 1500 DEG C of calcination 20 ~ 30min;
Step 3: the crucible after step 2 calcination is put in exsiccator and cools, cool time is 1 ~ 3h;
Step 4: after carbon and sulfur analytical instrument preheating terminates in step one, take the pure molybdenum of bits shape Mo1 of 0.2 ~ 0.5g, input weight value, adds the iron filings of 0.3 ~ 0.6g and the tungsten stannum fluxing agent of 0.3 ~ 0.6g;
Step 5: measure according to the analytical approach of instrument, record analysis result, namely completes the analysis of carbon in the pure molybdenum of Mo1.
2. the analytical approach of carbon in the pure molybdenum of a kind of Mo1 according to claim 1, is characterized in that preheating 3h in step one.
3. the analytical approach of carbon in the pure molybdenum of a kind of Mo1 according to claim 1, to is characterized in that low for infrared excess carbon-sulfur crucible in step 2 at 1200 ~ 1500 DEG C of calcination 25 ~ 30min.
4. the analytical approach of carbon in the pure molybdenum of a kind of Mo1 according to claim 1, to is characterized in that low for infrared excess carbon-sulfur crucible in step 2 at 1350 DEG C of calcination 25min.
5. the analytical approach of carbon in the pure molybdenum of a kind of Mo1 according to claim 1, is characterized in that in step 3, cool time is 2h.
6. the analytical approach of carbon in the pure molybdenum of a kind of Mo1 according to claim 1, is characterized in that the pure molybdenum of bits shape Mo1 taking 0.2g in step 4.
7. the analytical approach of carbon in the pure molybdenum of a kind of Mo1 according to claim 1, is characterized in that the iron filings adding 0.3g in step 4.
8. the analytical approach of carbon in the pure molybdenum of a kind of Mo1 according to claim 1, is characterized in that the tungsten stannum fluxing agent adding 0.3g in step 4.
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| CN201410145679.3A CN104977270A (en) | 2014-04-10 | 2014-04-10 | Analysis method of carbon element in Mo1 pure molybdenum |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108746103A (en) * | 2018-05-10 | 2018-11-06 | 石钢京诚装备技术有限公司 | The minimizing technology of residual carbon sulphur in carbon-sulfur crucible |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2697559Y (en) * | 2004-03-04 | 2005-05-04 | 武汉钢铁(集团)公司 | Ceramic curcible pre-treatment furnace for nifrared carbon sulphur analysis |
| US20090173884A1 (en) * | 2008-01-08 | 2009-07-09 | Sumco Techxiv Corporation | Method and apparatus for measuring spectroscopic absorbance |
| CN103196863A (en) * | 2013-03-21 | 2013-07-10 | 内蒙古包钢钢联股份有限公司 | Method for determining contents of carbon and sulfur in iron alloy by using infrared absorption method with calibration of different reference materials |
-
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- 2014-04-10 CN CN201410145679.3A patent/CN104977270A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2697559Y (en) * | 2004-03-04 | 2005-05-04 | 武汉钢铁(集团)公司 | Ceramic curcible pre-treatment furnace for nifrared carbon sulphur analysis |
| US20090173884A1 (en) * | 2008-01-08 | 2009-07-09 | Sumco Techxiv Corporation | Method and apparatus for measuring spectroscopic absorbance |
| CN103196863A (en) * | 2013-03-21 | 2013-07-10 | 内蒙古包钢钢联股份有限公司 | Method for determining contents of carbon and sulfur in iron alloy by using infrared absorption method with calibration of different reference materials |
Non-Patent Citations (3)
| Title |
|---|
| 王立新: "《冶金仪器分析技术与应用》", 30 September 2010, 化学工业出版社 * |
| 田英炎 等: "综论碳和硫的红外光谱法", 《21实际材料高速分析 第三届全国高速分析学术交流会论文集》 * |
| 裘立奋: "《现代难熔金属和稀散金属分析》", 31 January 2007, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108746103A (en) * | 2018-05-10 | 2018-11-06 | 石钢京诚装备技术有限公司 | The minimizing technology of residual carbon sulphur in carbon-sulfur crucible |
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