CN104458631A - Method for determining carbon and sulfur in material through repeatedly using crucible - Google Patents
Method for determining carbon and sulfur in material through repeatedly using crucible Download PDFInfo
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- CN104458631A CN104458631A CN201310431260.XA CN201310431260A CN104458631A CN 104458631 A CN104458631 A CN 104458631A CN 201310431260 A CN201310431260 A CN 201310431260A CN 104458631 A CN104458631 A CN 104458631A
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Abstract
The invention discloses a method for determining carbon and sulfur in a material through repeatedly using a crucible. The method is characterized in that the crucible is repeatedly used to determine the content of carbon in the material 5-6 times on the premise that the content of carbon or sulfur element in the material accords with an analysis error requirement; or the crucible is repeatedly used to determine the content of sulfur in the material 2-3 times. The used crucible is stored in different areas of a drier according to the use frequency, and the used crucible is used to correct an infrared absorption carbon and sulfur instrument in next time use in order to ensure the test accuracy and precision; the method realizes the repeated use of the crucible, and reduces the discard amount of the crucible; and the method reduces the use amount of a flux, reduces the energy consumption, the test cost and the environmental pollution rate, and is in favor of protecting the environment.
Description
Technical field
the present invention relates to a kind of method repeatedly using carbon and sulphur in crucible mensuration material, belong to measuring for materials field.
Background technology
carbon, sulfur content in experimental determination metal or other material, adopt infrared absorption spectrometry mostly.The porcelain crucible used in the method is commercially available 25 × 25mm crucible, after crucible is bought, needs first crucible to be placed in muffle furnace calcination in 1000 DEG C ~ 1200 DEG C temperature ranges and naturally cools to normal temperature after 4 hours, be stored in exsiccator for subsequent use.Before detection, also need to take out crucible from exsiccator, infrared absorption carbon sulphur instrument carries out correction test by software program and working specification to detecting instrument, after instrumental correction is good, then carries out specimen test.After crucible often used once, the working curve of instrument will change.In order to ensure the accuracy measured and accuracy.Therefore test crucible in prior art only to use once, whether damage and all pass into disuse, cause waste.The Disabled slag that simultaneously discarded crucible and the rear sample of the interior test of crucible are formed all can form certain pollution to the physical environment of surrounding.
Summary of the invention
the object of the invention is to, provide a kind of and repeatedly use the method that crucible measures carbon and sulphur in material, reduce the discarded amount of crucible, to save experimentation cost, also can reduce discarded crucible and Disabled slag to the impact of the physical environment of surrounding simultaneously.
technical scheme of the present invention:
a kind of method repeatedly using carbon and sulphur in crucible mensuration material, the method is divided into 6 regions by the exsiccator depositing crucible, commercially available crucible is left in 0 region for subsequent use after treatment, first time is when testing, take the crucible left in 0 region to test, after first time test, used crucible leaves in 1 region for subsequent use after treatment; When second time is tested, take the crucible left in 1 region and test, after second time test, used crucible leaves in 2 regions for subsequent use after treatment; By that analogy, it is for subsequent use that each used crucible leaves next region in, and the crucible can only taking a region during test next time is tested; Last time used crucible should be adopted before each official test to carry out correction test to infrared absorption carbon sulphur instrument, when guarantee in material of measuring and monitoring the growth of standing timber carbon or sulfur content meet analytical error require, reuse crucible and to measure in material carbon content 5 ~ 6 times; Or reuse crucible and to measure in material sulfur content 2 ~ 3 times.
in preceding method, describedly process is carried out to commercially available crucible be: commercially available crucible to be placed in muffle furnace calcination in 1000 ~ 1200 DEG C of temperature ranges and to naturally cool to normal temperature after 4 hours, put into exsiccator 0 region for subsequent use.
in preceding method, describedly process is carried out to used crucible be: by used crucible from after infrared absorption carbon sulphur instrument takes off, first be placed in anti-scald refrigeratory and cool 10 ~ 20 minutes, then blow clean with the grit of hair-dryer by crucible outer wall, then put into exsiccator respective regions for subsequent use.
in preceding method, described correction test takes standard substance 0.2 ~ 0.5g and the special tungsten particle 1.0 ~ 1.5g of determination of carbon and sulfur carries out correction test by official test code to infrared absorption carbon sulphur instrument, and write down the consumption of standard substance used and the special tungsten particle of determination of carbon and sulfur.
in preceding method, when taking correction test during described official test, the consumption of standard substance and the special tungsten particle of determination of carbon and sulfur is placed on corrected infrared absorption carbon sulphur instrument and tests.
in preceding method, after described official test, after infrared absorption carbon sulphur instrument takes off crucible, should crucible be examined, if having slag to spill or break, then discard this crucible or use again after this crucible is processed.
compared with prior art, the present invention, by used crucible is deposited in the different region of exsiccator by access times, when next time uses, adopts used crucible to correct infrared absorption carbon sulphur instrument, to guarantee accuracy, the precision of test; Achieve reusing of crucible, not only decrease the learies of crucible; Decrease the use amount of flux simultaneously, reduce energy consumption, experimentation cost and the pollution speed to environment, favorable environment is protected.
Embodiment
the present invention is described in further detail for structure example below, but not as any limitation of the invention.
Embodiment
a kind of method repeatedly using carbon and sulphur in crucible mensuration material, the method is divided into 6 regions by the exsiccator depositing crucible, commercially available crucible is left in 0 region for subsequent use after treatment, first time is when testing, take the crucible left in 0 region to test, after first time test, used crucible leaves in 1 region for subsequent use after treatment; When second time is tested, take the crucible left in 1 region and test, after second time test, used crucible leaves in 2 regions for subsequent use after treatment; By that analogy, it is for subsequent use that each used crucible leaves next region in, and the crucible can only taking a region during test next time is tested; Last time used crucible should be adopted before each official test to carry out correction test to infrared absorption carbon sulphur instrument, when guarantee in material of measuring and monitoring the growth of standing timber carbon or sulfur content meet analytical error require, reuse crucible and to measure in material carbon content 5 ~ 6 times; Or reuse crucible and to measure in material sulfur content 2 ~ 3 times.Describedly process is carried out to commercially available crucible be: commercially available crucible to be placed in muffle furnace calcination in 1000 ~ 1200 DEG C of temperature ranges and to naturally cool to normal temperature after 4 hours, put into exsiccator 0 region for subsequent use.Describedly process is carried out to used crucible be: by used crucible from after infrared absorption carbon sulphur instrument takes off, first be placed in anti-scald refrigeratory and cool 10 ~ 20 minutes, blow clean with the grit of hair-dryer by crucible outer wall again, then put into exsiccator respective regions for subsequent use.Described correction test takes standard substance 0.2 ~ 0.5g and the special tungsten particle 1.0 ~ 1.5g of determination of carbon and sulfur carries out correction test by official test code to infrared absorption carbon sulphur instrument, and write down the consumption of standard substance used and the special tungsten particle of determination of carbon and sulfur.When taking correction test during described official test, the consumption of standard substance and the special tungsten particle of determination of carbon and sulfur is placed on corrected infrared absorption carbon sulphur instrument and tests.After official test, after infrared absorption carbon sulphur instrument takes off crucible, should crucible be examined, if having slag to spill or break, then discard this crucible or use again after this crucible is processed.
during concrete enforcement, reacted crucible will be tested, and take off from infrared absorption carbon sulphur instrument and process, put into special exsiccator respective regions stand-by; With standard substance (sample) compensation line linearity curve; Repeatedly use crucible to test, general available crucible measures carbon content 5 ~ 6 times, and available crucible measures sulfur content 2 ~ 3 times.Measure and monitor the growth of standing timber material carbon, sulfur content of institute meets analytical error requirement.Concrete operation step is as follows:
1, reacted crucible will be tested, and take off from infrared absorption carbon sulphur instrument, be placed in anti-scald refrigeratory and cool 10min ~ 20min, stand-by with putting into special exsiccator respective regions (0 ~ 5) after hair-dryer removing outer wall grit.
2, from special exsiccator, crucible is taken out, infrared absorption carbon sulphur instrument carries out correction test by software program and working specification, and [wherein selection standard material (sample) the test portion amount that takes is 0.2g ~ 0.5g, and the special tungsten particle of added determination of carbon and sulfur is 1.0g ~ 1.5g.], correct to test findings and standard value error analyzing in allowed band.
3, instrumental correction good after, carry out specimen test.Test crucible is got with correction test same area, and alleged test portion amount and the special tungsten particle of added determination of carbon and sulfur and correction test consumption are about etc.
when 4, at every turn taking off crucible from infrared absorption carbon sulphur instrument, observe crucible: if having slag to spill or break, then discard this crucible, otherwise process crucible to be placed in next region of special exsiccator stand-by.
5, test by 1-4 step cycle.
Claims (6)
1. one kind repeatedly uses the method that crucible measures carbon and sulphur in material, it is characterized in that: the method is divided into 6 regions by the exsiccator depositing crucible, commercially available crucible is left in 0 region for subsequent use after treatment, first time is when testing, take the crucible left in 0 region to test, after first time test, used crucible leaves in 1 region for subsequent use after treatment; When second time is tested, take the crucible left in 1 region and test, after second time test, used crucible leaves in 2 regions for subsequent use after treatment; By that analogy, it is for subsequent use that each used crucible leaves next region in, and the crucible can only taking a region during test next time is tested; Last time used crucible should be adopted before each official test to carry out correction test to infrared absorption carbon sulphur instrument, when guarantee in material of measuring and monitoring the growth of standing timber carbon or sulfur content meet analytical error require, reuse crucible and to measure in material carbon content 5 ~ 6 times; Or reuse crucible and to measure in material sulfur content 2 ~ 3 times.
2. method according to claim 1, is characterized in that: describedly carry out process to commercially available crucible and be: commercially available crucible to be placed in muffle furnace calcination in 1000 ~ 1200 DEG C of temperature ranges and to naturally cool to normal temperature after 4 hours, put into exsiccator 0 region for subsequent use.
3. method according to claim 1, it is characterized in that: describedly process is carried out to used crucible be: by used crucible from after infrared absorption carbon sulphur instrument takes off, first be placed in anti-scald refrigeratory and cool 10 ~ 20 minutes, blow clean with the grit of hair-dryer by crucible outer wall again, then put into exsiccator respective regions for subsequent use.
4. method according to claim 1, it is characterized in that: described correction test takes standard substance 0.2 ~ 0.5g and the special tungsten particle 1.0 ~ 1.5g of determination of carbon and sulfur carries out correction test by official test code to infrared absorption carbon sulphur instrument, and write down the consumption of standard substance used and the special tungsten particle of determination of carbon and sulfur.
5. method according to claim 1, is characterized in that: when taking correction test during described official test, the consumption of standard substance and the special tungsten particle of determination of carbon and sulfur is placed on corrected infrared absorption carbon sulphur instrument and tests.
6. method according to claim 5, is characterized in that: after described official test, after infrared absorption carbon sulphur instrument takes off crucible, should examine crucible, if having slag to spill or break, then discard this crucible or use after processing this crucible again.
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| CN201310431260.XA CN104458631B (en) | 2013-09-22 | 2013-09-22 | It is a kind of to repeatedly use the method that crucible determines carbon and sulfur in material |
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| CN201310431260.XA CN104458631B (en) | 2013-09-22 | 2013-09-22 | It is a kind of to repeatedly use the method that crucible determines carbon and sulfur in material |
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| CN104458631B CN104458631B (en) | 2017-03-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105466880A (en) * | 2015-12-26 | 2016-04-06 | 首钢总公司 | Sample pretreatment method for measuring contents of sulfur in dolomite and limestone |
| CN108414470A (en) * | 2018-04-10 | 2018-08-17 | 中国航发北京航空材料研究院 | A kind of method of ultra-low sulfur in measurement wrought superalloy |
| CN112326584A (en) * | 2020-10-19 | 2021-02-05 | 本钢板材股份有限公司 | Method for detecting sulfur and carbon in steel |
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| CN101495680A (en) * | 2006-06-23 | 2009-07-29 | Rec斯坎沃佛股份有限公司 | Reusable crucibles and method of manufacturing them |
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| CN101495680A (en) * | 2006-06-23 | 2009-07-29 | Rec斯坎沃佛股份有限公司 | Reusable crucibles and method of manufacturing them |
| CN103266294A (en) * | 2013-03-07 | 2013-08-28 | 贵阳嘉瑜光电科技咨询中心 | Method of repeatedly using molybdenum crucible in HEM crystal growth |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105466880A (en) * | 2015-12-26 | 2016-04-06 | 首钢总公司 | Sample pretreatment method for measuring contents of sulfur in dolomite and limestone |
| CN108414470A (en) * | 2018-04-10 | 2018-08-17 | 中国航发北京航空材料研究院 | A kind of method of ultra-low sulfur in measurement wrought superalloy |
| CN108414470B (en) * | 2018-04-10 | 2020-11-13 | 中国航发北京航空材料研究院 | Method for measuring ultralow sulfur content in wrought superalloy |
| CN112326584A (en) * | 2020-10-19 | 2021-02-05 | 本钢板材股份有限公司 | Method for detecting sulfur and carbon in steel |
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| CN104458631B (en) | 2017-03-29 |
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