CN104458637A - Method for testing ultra-low carbon and sulphur content in plain carbon steel-low alloy steel - Google Patents
Method for testing ultra-low carbon and sulphur content in plain carbon steel-low alloy steel Download PDFInfo
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Abstract
The invention relates to a method for testing ultra-low carbon and sulphur content in plain carbon steel-low alloy steel. The method is characterized by comprising the following steps: processing samples into crumbs by using a planing machine; weighing fluxing agents and pouring into a crucible; putting into an infrared carbon-sulphur detector for analyzing; taking the crucible out after analysis, putting into a drier and cooling; correcting an instrument in a standardization mode; weighing the samples into the crucible; putting the crucible on a crucible tray of a high-frequency infrared carbon-sulphur detector; pressing a start key; automatically closing a furnace head of the instrument; heating the samples in oxygen flow by virtue of a high frequency furnace; respectively producing carbon and sulphur into CO2, CO and SO2; performing dust filtration and dehumidification on oxygen serving as carrier gas; introducing the oxygen into an SO2 infrared absorption cell for testing sulphur and SO2 gas; performing desulfuration and introducing into CO and CO2 infrared absorption cell for testing content of carbon. The method has the advantages that a method for testing the ultra-low carbon and sulphur in plain carbon steel-low alloy steel by means of infrared absorption is built, and the method is correct in analysis result, high in accuracy and short in time.
Description
Technical field
The present invention relates to the mensuration of Ultra-low carbon, sulfur content in a kind of steel, particularly one measures Ultra-low carbon and sulfur content method in straight carbon steel-low alloy steel, belongs to technical field of analytical chemistry.
background technology
Along with the fast development of production, scientific research, current steel-making presents the trend of diversification, and the scale of smelting ultralow-carbon, sulphur strengthens day by day, and this just proposes quite high requirement to the detection of Ultra-low carbon, sulphur.
At present, although there has been national standard method GB/T20123-2006, sensing range C:0.005 ~ 4.3 at%, S:0.0005 of the method ~ 0.33 at%, can not meet analysis carbon, sulfur content being less than to the product of 0.001 at%.
And national standard method GB/T20126-2006, although sensing range C:0.0003 ~ 0.01 at%, S:0.0005 of the method ~ 0.33 at%, analysis carbon, sulfur content being less than to the product of 0.001 at% can be met.But need at muffle furnace (420 DEG C) pre-service 5 ~ 10min before Specimen Determination; Tungsten particle needs at 450 DEG C of muffle furnace heating 10min; Tin grain then to need in ultrasonic cleaner, with watery hydrochloric acid cleaning more than 5min, then to use after water rinse, drying, complex operation, extends analysis time.
In addition, although there is spark emission spectroscopic method to measure ultralow-carbon report in steel, analysis condition is harsh, and cost is high.
Summary of the invention
The object of the invention is to be intended to overcome the above problems, provide a kind of and adopt Ultra-low carbon and sulfur content method in infrared absorption determining straight carbon steel-low alloy steel.
the technical solution adopted for the present invention to solve the technical problems:
1. sample planer is processed into bits shape;
2. will consider shape sample to be worth doing to clean with ether in ultrasonic cleaner, and after ether volatilization, load rapidly in drying, clean vial and cover tightly;
3. take flux in crucible, be placed in infrared C-S analyzer analysis, after analysis, exsiccator is put in crucible taking-up and cool;
4. standardization corrects: according to specimen types and content selection analysis passage, and analyze with selected standard specimen (close with sample to be tested content), when three times assay value is no more than tolerance, undertaken a bit by instrumentation code or multiple spot standardization correction (sample content should be less than selected standard specimen content);
The standard specimen that alternative one is of the same type with tested sample or benchmark are analyzed, and assay value, within the scope of tolerance, can carry out sample analysis.Otherwise, again do standardization and correct;
5. take in sample and above-mentioned steps crucible, be put in by crucible on the crucible tray of high frequency infrared ray carbon sulphur analyser, by start key, the burner of instrument closes automatically, and sample is through coreless induction furnace heating in oxygen stream, and carbon and sulphur content do not generate CO
2, CO and SO
2, be that carrier gas is through filtering dirt and after dehumidifying, entering SO with oxygen
2cell for infrared absorption, measures sulphur.Measure SO
2after gas, after desulfurization, enter CO, CO
2cell for infrared absorption, measures carbon content.
Described flux is the mixing of tin grain and tungsten powder;
Measurement range of the present invention: C:0.0003 ~ 0.050at%; S:0.0003 ~ 0.010at%
The invention has the beneficial effects as follows:
Set up a kind of method that infrared absorption measures Ultra-low carbon, sulphur in straight carbon steel, alloy steel.The present invention with ether washed samples 5min in ultrasonic cleaner, will guarantee that analysis result is more accurate by sample; Flux and crucible, after carbon and sulfur analytical instrument calcination, make the blank value of carbon sulphur all about 0.00004, can ensure that the Monitoring lower-cut of analytical approach is low like this, are applicable to the content analyzing super low carbon and sulphur in steel.It is 0.0003 at% that the Monitoring lower-cut carbon of method analyzes lower limit, Sulfur Analysis lower limit is 0.0003 at%, precision and the accuracy of analysis result meet the requirement of GB/T20126-2006 national standard. the relative GB/T20126-2006 national standard of the method, shorten analysis time, practical in actual production and scientific research.
Embodiment
the measurement range of 1 method
This method provides and adopt Ultra-low carbon, sulfur content in infrared absorption determining straight carbon steel, low alloy steel.
This method is applicable to the mensuration of Ultra-low carbon, sulfur content in straight carbon steel, low alloy steel.
Measurement range: C:0.0003 ~ 0.050 at %; S:0.0003 ~ 0.010 at%
2 key instruments and reagent
Japan produces CS-820V2 Infrared Carbon and Sulphur Determination instrument at the field that rises abruptly;
Ultrasonic cleaner (Kunshan Gao De plant equipment company limited)
Infrared special super low carbon and sulphur crucible (god of fire's board, the sharp crucible porcelain factory of gold of Hunan Liling city);
Acicular Sn grain flux: the massfraction of carbon containing and sulphur should be less than 0.0005% respectively;
Tungsten flux: the massfraction of carbon containing and sulphur should be less than 0.0005% respectively;
Straight carbon steel, low alloy steel standard specimen;
Magnesium perchlorate, plasticity alkali: all anhydrous, nothing oil;
Absolute ether;
Oxygen: purity > 99.99%
Power gas: pressurized air, nitrogen, must be anhydrous without oil.
Electronic balance: precision ± 0.0001g.
3. concrete implementation step:
Sample planer is processed into bits shape by step 1.;
Bits shape sample is cleaned 5min with ether by step 2. in ultrasonic cleaner, after ether volatilization, loads rapidly in drying, clean vial and covers tightly;
Step 3. takes 0.2g tin grain+1.5g tungsten powder flux in crucible, is placed in infrared C-S analyzer analysis, after analysis, exsiccator is put in crucible taking-up and cools;
Step 4. standardization corrects:
According to specimen types and content selection analysis passage, and analyze with selected standard specimen (close with sample to be tested content), when three times assay value is no more than tolerance, undertaken a bit by instrumentation code or multiple spot standardization correction (sample content should be less than selected standard specimen content).
The standard specimen that alternative one is of the same type with tested sample or benchmark are analyzed, and assay value, within the scope of tolerance, can carry out sample analysis.Otherwise, again do standardization and correct.
Crucible described in step 3 is placed in high frequency infrared ray carbon sulphur analyser by step 5., sample weight is set to 1.000g, measure in same passage, the enough number of times of replication (5-6 times) obtain low and more consistent reading, with recording three times minimum readings, compute mean value, in input instrument, instrument can carry out the electronic compensation of blank value when measuring sample.
Step 6. takes in 0.5 ~ 0.6g sample and step 3 crucible, is put in by crucible on the crucible tray of high frequency infrared ray carbon sulphur analyser, and by start key, the burner of instrument closes automatically, and sample is through coreless induction furnace heating in oxygen stream, and carbon and sulphur content do not generate CO
2(wherein part generates CO) and SO
2, be that carrier gas is through filtering dirt and after dehumidifying, entering SO with oxygen
2cell for infrared absorption, measures sulphur.Measure SO
2after gas, after desulfurization, enter CO, CO
2cell for infrared absorption, measures carbon content.
Specific embodiment is:
one, determine by experiment infrared carbon sulfur analyzer correlation parameter and to measure time influence factor.
1. coreless induction furnace exports setting
| Coreless induction furnace exports setting | mA | s |
| Step 1 | 0～175 | 5 |
| Step 2 | 175～175 | 50 |
When analysis straight carbon steel, low alloy steel, coreless induction furnace exports in range of set value.Sample not only decomposes completely, the recovery is high, and the power of coreless induction furnace can be avoided too high and reduce serviceable life of higher-order of oscillation pipe.
2. the sample weighting amount of sample
Sample weighting amount controls at 0.3 ~ 0.8g, and the recovery of carbon sulphur is all higher, and along with the increase of sample weighting amount, analysis precision is more and more higher.But along with the increase of sample weighting amount, pollution level suffered by stove itself will have increasing in various degree, show as sample itself and very easily splash occurs, strengthen the contaminated chance of air path part, there is different losses to electric elements etc. simultaneously, reduce serviceable life of instrument itself, it is high for being suitable for the sample complete recovery of not only burning between 500mg ~ 600mg therefore to consider shape sample analysis Chao Di Tan ﹑ sulphur general control to be worth doing, therefore determines that sample weighting amount is 0.5 ~ 0.6 g.
The setting of comparison level
3. when comparison level is 1at%, CO
2release profiles time delay; When comparison level is 2 ~ 5at%, CO
2not only smooth but also the symmetrical and not time delay of release profiles.SO
2release profiles rough when comparison level is 1 ~ 4at%, the signal difference of release is described, and release profiles is smooth when comparison level is 5%.Therefore, comparison level for alternatives 5% is more excellent condition.
4. the shortest integral time
The shortest integral time 20 ~ 30s, sample decomposes not exclusively, CO
2, SO
2release, the recovery is lower, causes analysis result on the low side.The shortest integral time 45 ~ 50s, although sample decomposes completely, some hangover, causes unnecessary analysis time delay.So the shortest integral time is chosen as 35 ~ 40s, not only sample decomposes completely, and CO
2, SO
2release, the recovery is higher.
5. the requirement of oxygen purity
Oxygen is used in molten sample process, providing oxygenant for combustion reaction and carrying analytical gas as carrier gas.When measuring super low carbon and sulphur sample, in oxygen, the methane of trace can oxidized generation carbon dioxide and water in high-frequency melting temperature, the carbon of instrument and the signal base line of sulphur can be made to fluctuate, impact analysis result.Therefore, when analyzing super low carbon and sulphur sample, the high purity oxygen using purity to be greater than 99.99 ﹪ can address this problem.Or instrument has oxygen purifying device.
two, the elimination of crucible and reagent blank
The blank of analysis environments and crucible and reagent directly affects the Monitoring lower-cut of the super low carbon and sulphur in straight carbon steel, low alloy steel, and the blank reducing crucible and reagent measures the most important research of super low carbon and sulphur in straight carbon steel, low alloy steel.
Embodiment 1
Crucible and flux all not calcinations, directly take the flux of different amount in crucible, be put in by crucible on the crucible tray of high frequency infrared ray carbon sulphur analyser, by start key, the burner of instrument closes automatically, carries out mensuration crucible and reagent blank.The results are shown in Table 1.
Embodiment 2
By crucible calcination 4h in the muffle furnace of 1300 DEG C, put into exsiccator after slightly cold and cool; Acicular Sn grain flux, tungsten flux, copper flux is calcination 0.5h in the muffle furnace of 200 DEG C; Then take different fluxs in crucible, be put in by crucible on the crucible tray of high frequency infrared ray carbon sulphur analyser, by start key, the burner of instrument closes automatically, measures.The results are shown in Table 1.
Embodiment 3
By crucible calcination 4h in the muffle furnace of 1300 DEG C, put into exsiccator after slightly cold and cool; Acicular Sn grain flux, tungsten flux, copper flux is calcination 2h in the muffle furnace of 400 DEG C; Take different fluxs in crucible, be put in by crucible on the crucible tray of high frequency infrared ray carbon sulphur analyser, by start key, the burner of instrument closes automatically, measures.The results are shown in Table 1.
Embodiment 4
Take a certain amount of flux in crucible, be placed in infrared C-S analyzer analysis, after analysis, exsiccator is put in crucible taking-up and cool, again crucible is put on the crucible tray of high frequency infrared ray carbon sulphur analyser, by start key, the burner of instrument closes automatically, measures.The results are shown in Table 1.
The blank value at ﹪ of table 1 crucible and flux
Can be found out by the result of table 1: acicular Sn grain flux, tungsten flux, copper flux be calcination 0.5h and acicular Sn grain flux, tungsten flux, copper flux blank value approximately equal after calcination 2h in the muffle furnace of 400 DEG C in the muffle furnace of 200 DEG C; Flux and crucible are after carbon and sulfur analytical instrument calcination, and the blank value of carbon sulphur, all about 0.00004, can ensure that the Monitoring lower-cut of analytical approach is low like this, are applicable to the content analyzing super low carbon and sulphur in steel.
three, the selection of flux addition
Although the magnetic conductivity of straight carbon steel, low alloy steel is comparatively strong, in order to reduce fusing point during burning, making sample be easy to burning, and improving the release rate of carbon in sample, sulphur, must by adding suitable flux.The object adding flux is in order to " lighting " sample, makes sample oxidation within a short period of time.
Flux and crucible by after described method process, then take a certain amount of sample in crucible, and identical instrument parameter arranges lower bioassay standard sample (ingot iron 300, C:0.0019 at ﹪; S:0.0053 at ﹪) middle carbon, sulfur content.In table 2.
Table 2 flux addition
By experiment above add 0.3g tin grain+1.5g tungsten powder, 0.2g tin grain+1.5g tungsten powder, 0.8g fine copper flux sample can Thorough combustion, oxidation, the recovery is high, and release profiles is unimodal, and de-tail, in 40 ~ 60s, carbon sulphur can discharge completely; Although using fine copper to make flux sample can be fully oxidized, when burning, reaction is violent, and residue splashes acutely, quartz combustion tube well damage, is therefore defined as 0.2g tin grain+1.5g tungsten powder adding of flux.
four, determine to analyze lower limit
Take a certain amount of flux in crucible, be placed in infrared C-S analyzer analysis, after analysis, exsiccator is put in crucible taking-up and cool, then carry out the mensuration of blank value.Identical instrument parameter is set and carries out mensuration 11 times, according to the detection limit formula C of IUPAC definition
l=3
s b /
k(S
bfor the standard deviation of blank, k is corresponding Slope of Calibration Curve) calculate, Carbon analysis lower limit of the present invention: 0.0003%, the Determination Limit of sulphur: 0.0003%.
five, the pre-service of sample
After using planer sample to be processed into bits shape, sample can stain some oil, the cleaning dirty accuracy that can reduce analytical sample of greasy dirt.Made by sample differently to clean, flux and crucible by after the process of embodiment 4 method, then take a certain amount of sample in crucible, and identical instrument parameter arranges carbon, sulfur content in lower working sample.In table 3.
Table 3 uses different cleaning way
Drawn by above data: with more than ether washed samples 5min in ultrasonic cleaner, the greasy dirt that specimen surface glues all processes totally.
Embodiment 5
Accuracy is tested
For investigating accuracy of analysis, selecting Ultra-low carbon, sulphur standard specimen 8 respectively, adopting two point calibration curve, eachly to average for 3 times (extreme difference of 3 measurement results is less than national standard) by replicate determination under above-mentioned optimal conditions, the results are shown in Table 4.
Table 4 result precision %
| Standard specimen title | Carbon standard value | Sulphur standard value | Carbon measures mean value | Sulphur measures mean value |
| 300 | 0.0019 | 0.0053 | 0.00182 | 0.00547 |
| 821 | 0.0012 | 0.0052 | 0.00127 | 0.00485 |
| GBW01146-20033 | 0.0025 | 0.0019 | 0.0024 | 0.00181 |
| GSB03-1598-2003 | 0.00067 | 0.0016 | 0.000695 | 0.00148 |
| YSBC20117C-2009 | 0.00034 | 0.00044 | 0.00039 | 0.00043 |
| 501-673 | 0.00040 | 0.0011 | 0.00048 | 0.00116 |
| GBW01148 | 0.0093 | 0.0014 | 0.00909 | 0.00135 |
| YSBC11088-98 | 0.0016 | 0.0063 | 0.00156 | 0.00682 |
From above situation: the analysis recovery of standard specimen is all 95% ~ 105%, and accuracy is high, the requirement that meets standard GB/T/T20126-2006.
Embodiment 6
Precision Experiment
For investigating the precision of analysis result, selecting Ultra-low carbon, sulphur standard specimen 4 respectively, measuring 11 times altogether by different time under above-mentioned optimal conditions.In table 5
The precision % of table 5 method
| Standard specimen title | Carbon mean value | Sulphur mean value | Carbon relative standard deviation | Sulphur relative standard deviation |
| GBW01146-20033 | 0.00246 | 0.00193 | 2.80 | 3.28 |
| YSBC20117C-2009 | 0.00036 | 0.00045 | 7.65 | 6.67 |
| GBW01148 | 0.0093 | 0.00138 | 2.86 | 2.78 |
| JSS652-14 | 0.0357 | 0.00136 | 1.36 | 2.64 |
As known from Table 5, the relative standard deviation RSD of each group result is all less than 10%.
Claims (3)
1. measure Ultra-low carbon and a sulfur content method in straight carbon steel-low alloy steel, it is characterized in that: concrete steps are as follows:
1) sample planer is processed into bits shape;
2) shape sample will be considered to be worth doing clean with ether in ultrasonic cleaner, and after ether volatilization, load rapidly in drying, clean vial and cover tightly;
3) take flux in crucible, be placed in infrared C-S analyzer analysis, after analysis, exsiccator is put in crucible taking-up and cool;
4) standardization corrects: according to specimen types and content selection analysis passage, and analyzes with selected standard specimen, when three times assay value is no more than tolerance, is undertaken a bit or multiple spot standardization correction by instrumentation code;
The standard specimen that alternative one is of the same type with tested sample or benchmark are analyzed, and assay value, within the scope of tolerance, can carry out sample analysis, otherwise, again do standardization and correct;
5) take in sample and above-mentioned steps crucible, be put in by crucible on the crucible tray of high frequency infrared ray carbon sulphur analyser, by start key, the burner of instrument closes automatically, and sample is through coreless induction furnace heating in oxygen stream, and carbon and sulphur content do not generate CO
2, CO and SO
2, be that carrier gas is through filtering dirt and after dehumidifying, entering SO with oxygen
2cell for infrared absorption, measures sulphur, measures SO
2after gas, after desulfurization, enter CO, CO
2cell for infrared absorption, measures carbon content.
2. Ultra-low carbon and sulfur content method in mensuration straight carbon steel-low alloy steel according to claim 1, is characterized in that: described flux is the mixing of tin grain and tungsten powder.
3. Ultra-low carbon and sulfur content method in mensuration straight carbon steel-low alloy steel according to claim 1, is characterized in that: determined straight carbon steel-Carbon in Low Alloy Steel and sulphur scope are respectively C:0.0003 ~ 0.050at%; S:0.0003 ~ 0.010at%.
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| CN106568735A (en) * | 2016-10-25 | 2017-04-19 | 福建紫金矿冶测试技术有限公司 | High-frequency infrared carbon and sulfur analyzer standard sample selection and working curve production method |
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| CN106766913A (en) * | 2016-12-30 | 2017-05-31 | 南京麒麟科学仪器集团有限公司 | Novel high-frequency stove and infrared carbon sulfur analyzer |
| CN106932356A (en) * | 2015-12-31 | 2017-07-07 | 中核北方核燃料元件有限公司 | The assay method of carbon and sulphur contents in thorium tetrafluoride |
| CN107153045A (en) * | 2017-06-30 | 2017-09-12 | 马鞍山钢铁股份有限公司 | A kind of method that infrared absorption determines carbon content in covering agent in Ultra-low carbon |
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| 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 |
| CN109540830A (en) * | 2018-12-25 | 2019-03-29 | 河钢股份有限公司 | A kind of method of carbon content in measurement ferro-niobium |
| CN111122493A (en) * | 2020-01-06 | 2020-05-08 | 包头钢铁（集团）有限责任公司 | Method for measuring carbon and sulfur in dust mud by infrared absorption method-renewable resource different-standard correction |
| 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 |
| CN112345482A (en) * | 2020-10-23 | 2021-02-09 | 宁波江丰电子材料股份有限公司 | Analysis method for carbon content in aluminum material |
| CN116359166A (en) * | 2023-05-31 | 2023-06-30 | 北京一控系统技术有限公司 | Method for detecting sulfur-carbon content in steel |
| CN116359166B (en) * | 2023-05-31 | 2023-08-11 | 北京一控系统技术有限公司 | Method for detecting sulfur-carbon content in steel |
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