CN109540830A - A kind of method of carbon content in measurement ferro-niobium - Google Patents
A kind of method of carbon content in measurement ferro-niobium Download PDFInfo
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- CN109540830A CN109540830A CN201811592676.9A CN201811592676A CN109540830A CN 109540830 A CN109540830 A CN 109540830A CN 201811592676 A CN201811592676 A CN 201811592676A CN 109540830 A CN109540830 A CN 109540830A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 91
- 229910000592 Ferroniobium Inorganic materials 0.000 title claims abstract description 66
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000005259 measurement Methods 0.000 title claims abstract description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 62
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 34
- 239000010959 steel Substances 0.000 claims abstract description 34
- 229910052742 iron Inorganic materials 0.000 claims abstract description 31
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 31
- 239000010937 tungsten Substances 0.000 claims abstract description 31
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000012937 correction Methods 0.000 claims abstract description 23
- 238000004458 analytical method Methods 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 10
- 229910001882 dioxygen Inorganic materials 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- BSPSZRDIBCCYNN-UHFFFAOYSA-N phosphanylidynetin Chemical compound [Sn]#P BSPSZRDIBCCYNN-UHFFFAOYSA-N 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 238000003908 quality control method Methods 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 24
- 238000003556 assay Methods 0.000 description 18
- 238000005303 weighing Methods 0.000 description 18
- 239000001569 carbon dioxide Substances 0.000 description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 7
- 229910001220 stainless steel Inorganic materials 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000005864 Sulphur Substances 0.000 description 6
- 229910001315 Tool steel Inorganic materials 0.000 description 6
- 230000033228 biological regulation Effects 0.000 description 6
- 238000001354 calcination Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 229910052571 earthenware Inorganic materials 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 230000010076 replication Effects 0.000 description 6
- 238000007619 statistical method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of methods of carbon content in measurement ferro-niobium, and the method is using high frequency infrared ray carbon sulphur analyser as measuring instrument, and using pure iron, high purity tin and high purity tungsten as fluxing agent, sample leads to the CO generated after oxygen burning2Gas can absorb certain specific wavelength infrared light strongly, and the Strength Changes by measuring the infrared light before and after entering infrared detection pond obtain the C content in sample to be tested.This method has selected best fluxing agent, correction is standardized using steel Plays sample, it solves the problems, such as quickly to measure carbon content in ferro-niobium, with simple and convenient analysis steps, chemistry disruption is few, analytical cycle is short, the features such as result precision is high, reliable technical guarantee is provided for smelting, application and the quality control of ferro-niobium, has effectively cooperated the progress of scientific research and special production work.
Description
Technical field
The invention belongs to technical field of ferrous metallurgical analysis, and in particular to a method of carbon content in measurement ferro-niobium.
Background technique
The niobium in the world about 85%~90% is produced in the form of ferro-niobium for steel, is particularly applied to alloy steel smelting, alloy
Element additive and stainless steel welding electrode coating etc..
Niobium is added in steel not only can be improved the intensity of steel, can also improve the toughness of steel, high temperature oxidation resistance and anti-corrosion
Property.Therefore, quickly and accurately carbon content in ferro-niobium is measured extremely important.China is for carbon content in ferro-niobium at present
Measurement standard only has " GB 3654.4-1983 ferro-niobium chemical analysis method: burning gravimetric detemination carbon amounts ".
But GB 3654.4-1983 examination criteria is chemical analysis method, for high-frequency induction burning-infrared absorption side
Carbon content there is no examination criteria in method measurement ferro-niobium.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of methods of carbon content in measurement ferro-niobium.The invention is according to detection
Need of work bases oneself upon the existing instrument and equipment in laboratory, establishes carbon content in high-frequency induction burning-infrared absorption determining ferro-niobium
Detection method meets the needs of scientific research, production.
In order to solve the above technical problems, the technical solution used in the present invention is: a kind of side for measuring carbon content in ferro-niobium
Method, the method is using high frequency infrared ray carbon sulphur analyser as measuring instrument, using pure iron, high purity tin and high purity tungsten as fluxing agent,
Sample leads to the CO generated after oxygen burning2Gas can absorb certain specific wavelength infrared light strongly, enter infrared detection pond by measurement
The Strength Changes of the infrared light of front and back obtain the C content in sample to be tested, the specific steps are as follows:
(1) high purity tin is weighed, high purity tin is placed in infrared C-S analyzer special copple, crucible bottom is uniformly layered on；It is described high-purity
Tin phosphorus content less than 0.0005%,
(2) ferro-niobium powdered sample is weighed, load weighted sample is placed in step (1) the infrared C-S analyzer special copple；
(3) pure iron, high purity tungsten are weighed, pure iron and high purity tungsten are covered in above ferro-niobium sample；The pure iron and high purity tungsten are carbon containing
Amount is respectively less than 0.0005%,
(4) the infrared C-S analyzer special copple equipped with sample is placed in Efco-Northrup furnace, opens high frequency infrared ray carbon sulphur analyser
Start measurement analysis, obtains the mass fraction of total carbon in ferro-niobium sample.
The sample weighting amount of ferro-niobium powdered sample and pure iron, high purity tin and the total fluxing agent of high purity tungsten in step (2) of the present invention
Mass ratio is 1:4~5.
In fluxing agent of the present invention, the mass ratio of high purity tin, pure iron and high purity tungsten is 2:1:5~7.
The high frequency infrared ray carbon sulphur analyser of step (4) of the present invention, Efco-Northrup furnace setup parameter are as follows: purge time
For 10~15s, delay time 20s, analysis time is 40~50s, and comparator level is 1~3%, is divided between cleaning 5 times.
In the high frequency infrared ray carbon sulphur analyser measurement analytic process of step (4) of the present invention, high purity oxygen gas flow is 3.0
±0.2L/min。
In the high frequency infrared ray carbon sulphur analyser measurement analytic process of step (4) of the present invention, high purity oxygen gas purity is greater than
99.999%。
The high frequency infrared ray carbon sulphur analyser of step (4) of the present invention, instrument model are that U.S.'s power can CS600.
In the high frequency infrared ray carbon sulphur analyser measurement analytic process of step (4) of the present invention, before measuring ferro-niobium sample, adopt
Be standardized correction with steel standard sample, the blank test of fluxing agent carried out before measuring, then when measuring ferro-niobium sample into
The electronic compensation of line blank value.
The high frequency infrared ray carbon sulphur analyser of step (4) of the present invention, running parameter are as follows: purge time: 10s, delay
Time: 20s, analysis time: 40s, comparator are horizontal: 2%, it cleans and is spaced: 5 times.
The carbon content range that the method for the invention detects ferro-niobium sample is C >=0.03%.
The beneficial effects of adopting the technical scheme are that the 1, present invention has simple and convenient analysis steps, chemistry dry
Disturb less, analytical cycle it is short, the features such as result precision is high.2, this method has selected best fluxing agent, using steel Plays sample
It is standardized correction, solves the problems, such as quickly to measure carbon content in ferro-niobium, is mentioned for smelting, application and the quality control of ferro-niobium
For reliable technical guarantee, the progress of scientific research and special production work is effectively cooperated.
Specific embodiment
The present invention will be further described in detail below with reference to specific embodiments.
Embodiment 1
The present embodiment measures the method and process of carbon content in ferro-niobium, and that steps are as follows is described:
(1) reagent prepares:
Stainless steel standard sample YSBC11341-2005 (304L), carbon content 0.015%；
GBW (E) 010198 (05-70), carbon content 0.045%；
YSBC31904-2012, carbon content 0.171%；
High-speed tool steel GSBH40091-96, carbon content 0.909%；
Carbon sulphur detects dedicated standard specimen LECO501-677, carbon content 0.39% in steel；
The equal < 0.0005% of carbon content in pure iron, high purity tin and high purity tungsten；
Infrared C-S analyzer special copple is placed on spare in drier in 1000 DEG C of calcination 4h；
(2) standardization correction: standard substance of the step (1) in addition to carbon sulphur detects dedicated standard specimen YSBC31904-2012 in steel is put
Enter high frequency infrared ray carbon sulphur analyser, the carbon content of steel standard sample measured, each standard specimen three times assay value be no more than permit
Perhaps poor, finally multiple spot standardization correction is carried out by instrumentation regulation；Obtain standard curve；Carbon sulphur in steel is detected into dedicated standard specimen
YSBC31904-2012 is put into high frequency infrared ray carbon sulphur analyser and is analyzed, and assay value is in GB/T20123-2006 tolerance range
It is interior, sample analysis can be carried out, otherwise does standardization correction again；
(3) blank assay: required same amount of fluxing agent when be added in an empty infrared C-S analyzer special copple with analysis sample,
Sample weight is set as 1.0000g, is measured in step (2) resulting standardized curve, replication 6 times, each numerical value
≤ 0.0020, record it is the smallest read three times, note calculate average value, input instrument in, instrument carries out blank value when measuring sample
Electronic compensation；
(4) electronic balance weighing 0.18g high purity tin is used, high purity tin is placed in infrared C-S analyzer special copple, earthenware is uniformly layered on
Crucible bottom；
(5) electronic balance weighing 0.2000g ferro-niobium powdered sample A is used, it is dedicated that load weighted sample is placed in infrared C-S analyzer
In crucible；
(6) electronic balance weighing 0.09g pure iron is used, pure iron and high purity tungsten are covered on ferro-niobium powdered sample by 0.55g high purity tungsten
Face；
(7) infrared C-S analyzer special copple is placed in Efco-Northrup furnace together with sample, opening Efco-Northrup furnace makes sample
Melt-combustion；
(8) carbon dioxide that sample burning generates is loaded into carbon dioxide pond with high purity oxygen gas to absorb, by detector to absorption
After infrared light is detected, electric signal is converted optical signal into；
(9) instrument calculates peak area by setup parameter；It is calculated according to Lambert-Beer's law, obtains total carbon in ferro-niobium sample
Mass fraction.
Step (4)~(9) are repeated 6 times, 7 tests are obtained into measured value statistical analysis, respectively obtain statistical survey value
Average value and relative standard deviation (RSD), be shown in Table 1.
The measurement result of 1 embodiment 1 of table
Embodiment 2
The present embodiment measures the method and process of carbon content in ferro-niobium, and that steps are as follows is described:
(1) reagent prepares:
Stainless steel standard sample YSBC11341-2005 (304L), carbon content 0.015%；
GBW (E) 010198 (05-70), carbon content 0.045%；
YSBC31904-2012, carbon content 0.171%；
High-speed tool steel GSBH40091-96, carbon content 0.909%；
Carbon sulphur detects dedicated standard specimen LECO501-677, carbon content 0.39% in steel；
The equal < 0.0005% of carbon content in pure iron, high purity tin and high purity tungsten；
Infrared C-S analyzer special copple is placed on spare in drier in 1000 DEG C of calcination 4h；
(2) standardization correction: standard substance of the step (1) in addition to carbon sulphur detects dedicated standard specimen YSBC31904-2012 in steel is put
Enter high frequency infrared ray carbon sulphur analyser, the carbon content of steel standard sample measured, each standard specimen three times assay value be no more than permit
Perhaps poor, multiple spot standardization correction finally is carried out by instrumentation regulation, obtains standard curve；Carbon sulphur in steel is detected into dedicated standard specimen
YSBC31904-2012 is put into high frequency infrared ray carbon sulphur analyser and is analyzed, and assay value is in GB/T20123-2006 tolerance range
It is interior, sample analysis can be carried out, otherwise does standardization correction again；
(3) blank assay: required same amount of fluxing agent when be added in an empty infrared C-S analyzer special copple with analysis sample,
Sample weight is set as 1.0000g, is measured in step (2) resulting standardized curve, replication 6 times, each numerical value
≤ 0.0020, record it is the smallest read three times, note calculate average value, input instrument in, instrument will do it blank when measuring sample
The electronic compensation of value；
(4) electronic balance weighing 0.19g high purity tin is used, high purity tin is placed in infrared C-S analyzer special copple, earthenware is uniformly layered on
Crucible bottom；
(5) electronic balance weighing 0.2100g ferro-niobium powdered sample B is used, it is dedicated that load weighted sample is placed in infrared C-S analyzer
In crucible；
(6) electronic balance weighing 0.095g pure iron is used, pure iron and high purity tungsten are covered in ferro-niobium powdered sample by 0.58g high purity tungsten
Above；
(7) infrared C-S analyzer special copple is placed in Efco-Northrup furnace together with sample, opening Efco-Northrup furnace makes sample
Melt-combustion；
(8) carbon dioxide that sample burning generates is loaded into carbon dioxide pond with high purity oxygen gas to absorb, by detector to absorption
After infrared light is detected, electric signal is converted optical signal into；
(9) instrument calculates peak area by setup parameter；It is calculated according to Lambert-Beer's law, obtains total carbon in ferro-niobium sample
Mass fraction.
Step (4)~(9) are repeated 6 times, 7 tests are obtained into measured value statistical analysis, respectively obtain statistical survey value
Average value and relative standard deviation (RSD), be shown in Table 2.
The measurement result of 2 embodiment 2 of table
Embodiment 3
The present embodiment measures the method and process of carbon content in ferro-niobium, and that steps are as follows is described:
(1) reagent prepares:
Stainless steel standard sample YSBC11341-2005 (304L), carbon content 0.015%；
GBW (E) 010198 (05-70), carbon content 0.045%；
YSBC31904-2012, carbon content 0.171%；
High-speed tool steel GSBH40091-96, carbon content 0.909%；
Carbon sulphur detects dedicated standard specimen LECO501-677, carbon content 0.39% in steel；
The equal < 0.0005% of carbon content in pure iron, high purity tin and high purity tungsten；
Infrared C-S analyzer special copple is placed on spare in drier in 1000 DEG C of calcination 4h；
(2) standardization correction: standard substance of the step (1) in addition to carbon sulphur detects dedicated standard specimen YSBC31904-2012 in steel is put
Enter high frequency infrared ray carbon sulphur analyser, the carbon content of steel standard sample measured, each standard specimen three times assay value be no more than permit
Perhaps poor, finally multiple spot standardization correction is carried out by instrumentation regulation；Carbon sulphur in steel is detected into dedicated standard specimen YSBC31904-
2012, which are put into high frequency infrared ray carbon sulphur analyser, is analyzed, and assay value is within the scope of GB/T20123-2006 tolerance, Ji Kejin
Otherwise row sample analysis does standardization correction again；
(3) blank assay: required same amount of fluxing agent when be added in an empty infrared C-S analyzer special copple with analysis sample,
Sample weight is set as 1.0000g, is measured in step (2) resulting standardized curve, replication 6 times, each numerical value
≤ 0.0020, record it is the smallest read three times, note calculate average value, input instrument in, instrument will do it blank when measuring sample
The electronic compensation of value；
(4) electronic balance weighing 0.20g high purity tin is used, high purity tin is placed in infrared C-S analyzer special copple, earthenware is uniformly layered on
Crucible bottom；
(5) electronic balance weighing 0.2200g ferro-niobium powdered sample C is used, it is dedicated that load weighted sample is placed in infrared C-S analyzer
In crucible；
(6) electronic balance weighing 0.10g pure iron is used, pure iron and high purity tungsten are covered on ferro-niobium powdered sample by 0.60g high purity tungsten
Face；
(7) infrared C-S analyzer special copple is placed in Efco-Northrup furnace together with sample, opening Efco-Northrup furnace makes sample
Melt-combustion；
(8) carbon dioxide that sample burning generates is loaded into carbon dioxide pond with high purity oxygen gas to absorb, by detector to absorption
After infrared light is detected, electric signal is converted optical signal into；
(9) instrument calculates peak area by setup parameter；It is calculated according to Lambert-Beer's law, obtains total carbon in ferro-niobium sample
Mass fraction.
Step (4)~(9) are repeated 6 times, 7 tests are obtained into measured value statistical analysis, respectively obtain statistical survey value
Average value and relative standard deviation (RSD), be shown in Table 3.
The measurement result of 3 embodiment 3 of table
Embodiment 4
The present embodiment measures the method and process of carbon content in ferro-niobium, and that steps are as follows is described:
(1) reagent prepares:
Stainless steel standard sample YSBC11341-2005 (304L), carbon content 0.015%；
GBW (E) 010198 (05-70), carbon content 0.045%；
YSBC31904-2012, carbon content 0.171%；
High-speed tool steel GSBH40091-96, carbon content 0.909%；
Carbon sulphur detects dedicated standard specimen LECO501-677, carbon content 0.39% in steel；
The equal < 0.0005% of carbon content in pure iron, high purity tin and high purity tungsten；
Infrared C-S analyzer special copple is placed on spare in drier in 1000 DEG C of calcination 4h；
(2) standardization correction: standard substance of the step (1) in addition to carbon sulphur detects dedicated standard specimen YSBC31904-2012 in steel is put
Enter high frequency infrared ray carbon sulphur analyser, the carbon content of steel standard sample measured, each standard specimen three times assay value be no more than permit
Perhaps poor, finally multiple spot standardization correction is carried out by instrumentation regulation；Carbon sulphur in steel is detected into dedicated standard specimen YSBC31904-
2012, which are put into high frequency infrared ray carbon sulphur analyser, is analyzed, and assay value is within the scope of GB/T20123-2006 tolerance, Ji Kejin
Otherwise row sample analysis does standardization correction again；
(3) blank assay: required same amount of fluxing agent when be added in an empty infrared C-S analyzer special copple with analysis sample,
Sample weight is set as 1.0000g, is measured in step (2) resulting standardized curve, replication 6 times, each numerical value
≤ 0.0020, record it is the smallest read three times, note calculate average value, input instrument in, instrument will do it blank when measuring sample
The electronic compensation of value；
(4) electronic balance weighing 0.21g high purity tin is used, high purity tin is placed in infrared C-S analyzer special copple, earthenware is uniformly layered on
Crucible bottom；
(5) electronic balance weighing 0.2340g ferro-niobium powdered sample D is used, it is dedicated that load weighted sample is placed in infrared C-S analyzer
In crucible；
(6) electronic balance weighing 0.105g pure iron is used, pure iron and high purity tungsten are covered in ferro-niobium powdered sample by 0.62g high purity tungsten
Above；
(7) infrared C-S analyzer special copple is placed in Efco-Northrup furnace together with sample, opening Efco-Northrup furnace makes sample
Melt-combustion；
(8) carbon dioxide that sample burning generates is loaded into carbon dioxide pond with high purity oxygen gas to absorb, by detector to absorption
After infrared light is detected, electric signal is converted optical signal into；
(9) instrument calculates peak area by setup parameter；It is calculated according to Lambert-Beer's law, obtains total carbon in ferro-niobium sample
Mass fraction.
Step (4)~(9) are repeated 6 times, 7 tests are obtained into measured value statistical analysis, respectively obtain statistical survey value
Average value and relative standard deviation (RSD), be shown in Table 4.
The measurement result of 4 embodiment 4 of table
Embodiment 5
The present embodiment measures the method and process of carbon content in ferro-niobium, and that steps are as follows is described:
(1) reagent prepares:
Stainless steel standard sample YSBC11341-2005 (304L), carbon content 0.015%；
GBW (E) 010198 (05-70), carbon content 0.045%；
YSBC31904-2012, carbon content 0.171%；
High-speed tool steel GSBH40091-96, carbon content 0.909%；
Carbon sulphur detects dedicated standard specimen LECO501-677, carbon content 0.39% in steel；
The equal < 0.0005% of carbon content in pure iron, high purity tin and high purity tungsten；
Infrared C-S analyzer special copple is placed on spare in drier in 1000 DEG C of calcination 4h；
(2) standardization correction: standard substance of the step (1) in addition to carbon sulphur detects dedicated standard specimen YSBC31904-2012 in steel is put
Enter high frequency infrared ray carbon sulphur analyser, the carbon content of steel standard sample measured, each standard specimen three times assay value be no more than permit
Perhaps poor, finally multiple spot standardization correction is carried out by instrumentation regulation；Carbon sulphur in steel is detected into dedicated standard specimen YSBC31904-
2012, which are put into high frequency infrared ray carbon sulphur analyser, is analyzed, and assay value is within the scope of GB/T20123-2006 tolerance, Ji Kejin
Otherwise row sample analysis does standardization correction again；
(3) blank assay: required same amount of fluxing agent when be added in an empty infrared C-S analyzer special copple with analysis sample,
Sample weight is set as 1.0000g, is measured in step (2) resulting standardized curve, replication 6 times, each numerical value
≤ 0.0020, record it is the smallest read three times, note calculate average value, input instrument in, instrument will do it blank when measuring sample
The electronic compensation of value；
(4) electronic balance weighing 0.22g high purity tin is used, high purity tin is placed in infrared C-S analyzer special copple, earthenware is uniformly layered on
Crucible bottom；
(5) electronic balance weighing 0.1760g ferro-niobium powdered sample E is used, it is dedicated that load weighted sample is placed in infrared C-S analyzer
In crucible；
(6) electronic balance weighing 0.11g pure iron is used, pure iron and high purity tungsten are covered on ferro-niobium powdered sample by 0.55g high purity tungsten
Face；
(7) infrared C-S analyzer special copple is placed in Efco-Northrup furnace together with sample, opening Efco-Northrup furnace makes sample
Melt-combustion；
(8) carbon dioxide that sample burning generates is loaded into carbon dioxide pond with high purity oxygen gas to absorb, by detector to absorption
After infrared light is detected, electric signal is converted optical signal into；
(9) instrument calculates peak area by setup parameter；It is calculated according to Lambert-Beer's law, obtains total carbon in ferro-niobium sample
Mass fraction.
Step (4)~(9) are repeated 6 times, 7 tests are obtained into measured value statistical analysis, respectively obtain statistical survey value
Average value and relative standard deviation (RSD), be shown in Table 5.
The measurement result of 5 embodiment 5 of table
Embodiment 6
The present embodiment measures the method and process of carbon content in ferro-niobium, and that steps are as follows is described:
(1) reagent prepares:
Stainless steel standard sample YSBC11341-2005 (304L), carbon content 0.015%；
GBW (E) 010198 (05-70), carbon content 0.045%；
YSBC31904-2012, carbon content 0.171%；
High-speed tool steel GSBH40091-96, carbon content 0.909%；
Carbon sulphur detects dedicated standard specimen LECO501-677, carbon content 0.39% in steel；
The equal < 0.0005% of carbon content in pure iron, high purity tin and high purity tungsten；
Infrared C-S analyzer special copple is placed on spare in drier in 1000 DEG C of calcination 4h；
(2) standardization correction: standard substance of the step (1) in addition to carbon sulphur detects dedicated standard specimen YSBC31904-2012 in steel is put
Enter high frequency infrared ray carbon sulphur analyser, the carbon content of steel standard sample measured, each standard specimen three times assay value be no more than permit
Perhaps poor, finally multiple spot standardization correction is carried out by instrumentation regulation；Carbon sulphur in steel is detected into dedicated standard specimen YSBC31904-
2012, which are put into high frequency infrared ray carbon sulphur analyser, is analyzed, and assay value is within the scope of GB/T20123-2006 tolerance, Ji Kejin
Otherwise row sample analysis does standardization correction again；
(3) blank assay: required same amount of fluxing agent when be added in an empty infrared C-S analyzer special copple with analysis sample,
Sample weight is set as 1.0000g, is measured in step (2) resulting standardized curve, replication 6 times, each numerical value
≤ 0.0020, record it is the smallest read three times, note calculate average value, input instrument in, instrument will do it blank when measuring sample
The electronic compensation of value；
(4) electronic balance weighing 0.22g high purity tin is used, high purity tin is placed in infrared C-S analyzer special copple, earthenware is uniformly layered on
Crucible bottom；
(5) electronic balance weighing 0.2500g ferro-niobium powdered sample F is used, it is dedicated that load weighted sample is placed in infrared C-S analyzer
In crucible；
(6) electronic balance weighing 0.11g pure iron is used, pure iron and high purity tungsten are covered on ferro-niobium powdered sample by 0.77g high purity tungsten
Face；
(7) infrared C-S analyzer special copple is placed in Efco-Northrup furnace together with sample, opening Efco-Northrup furnace makes sample
Melt-combustion；
(8) carbon dioxide that sample burning generates is loaded into carbon dioxide pond with high purity oxygen gas to absorb, by detector to absorption
After infrared light is detected, electric signal is converted optical signal into；
(9) instrument calculates peak area by setup parameter；It is calculated according to Lambert-Beer's law, obtains total carbon in ferro-niobium sample
Mass fraction.
Step (4)~(9) are repeated 6 times, 7 tests are obtained into measured value statistical analysis, respectively obtain statistical survey value
Average value and relative standard deviation (RSD), be shown in Table 6.
The measurement result of 6 embodiment 6 of table
Mark-on reclaims test: quantitative weighs ferro-niobium sample and steel standard specimen, different amounts of calcium carbonate benchmark is added, according to the side
Method is under the setting of identical instrument condition, using calcium carbonate benchmark, steel standard specimen correction work curve (using Supplements), measurement
Carbon content in its sample, the results are shown in Table 7.
7 mark-on reclaims test result (%) of table
As shown in Table 7, sample carries out the measurement of recovery of standard addition, and the rate of recovery is 95~103%, it was demonstrated that this method can sufficiently expire
Carbon analysis requirement in sufficient ferro-niobium.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although referring to above-described embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that: still the present invention can be modified or be waited
With replacement, without departing from the spirit or scope of the invention, or any substitutions, should all cover in power of the invention
In sharp claimed range.
Claims (10)
1. it is a kind of measurement ferro-niobium in carbon content method, which is characterized in that the method using high frequency infrared ray carbon sulphur analyser as
Measuring instrument, using pure iron, high purity tin and high purity tungsten as fluxing agent, sample leads to the CO generated after oxygen burning2Gas can be inhaled strongly
Certain specific wavelength infrared light is received, the Strength Changes by measuring the infrared light before and after entering infrared detection pond obtain in sample to be tested
C content, the specific steps are as follows:
(1) high purity tin is weighed, high purity tin is placed in infrared C-S analyzer special copple, crucible bottom is uniformly layered on；It is described high-purity
Tin phosphorus content less than 0.0005%,
(2) ferro-niobium powdered sample is weighed, load weighted sample is placed in step (1) the infrared C-S analyzer special copple；
(3) pure iron, high purity tungsten are weighed, pure iron and high purity tungsten are covered in above ferro-niobium sample；The pure iron and high purity tungsten are carbon containing
Amount is respectively less than 0.0005%,
(4) the infrared C-S analyzer special copple equipped with sample is placed in Efco-Northrup furnace, opens high frequency infrared ray carbon sulphur analyser
Start measurement analysis, obtains the mass fraction of total carbon in ferro-niobium sample.
2. the method for carbon content in a kind of measurement ferro-niobium according to claim 1, which is characterized in that in the step (2)
The sample weighting amount and pure iron, high purity tin and the total fluxing agent mass ratio of high purity tungsten of ferro-niobium powdered sample are 1:4~5.
3. the method for carbon content in a kind of measurement ferro-niobium according to claim 1, which is characterized in that in the fluxing agent,
The mass ratio of high purity tin, pure iron and high purity tungsten is 2:1:5~7.
4. the method for carbon content in a kind of measurement ferro-niobium according to claim 1 to 3, which is characterized in that described
The high frequency infrared ray carbon sulphur analyser of step (4), Efco-Northrup furnace setup parameter are as follows: purge time is 10~15s, delay time
20s, analysis time are 40~50s, and comparator level is 1~3%, are divided between cleaning 5 times.
5. the method for carbon content in a kind of measurement ferro-niobium according to claim 1 to 3, which is characterized in that described
In the high frequency infrared ray carbon sulphur analyser measurement analytic process of step (4), high purity oxygen gas flow is 3.0 ± 0.2L/min.
6. the method for carbon content in a kind of measurement ferro-niobium according to claim 1 to 3, which is characterized in that described
In the high frequency infrared ray carbon sulphur analyser measurement analytic process of step (4), high purity oxygen gas purity is greater than 99.999%.
7. the method for carbon content in a kind of measurement ferro-niobium according to claim 1 to 3, which is characterized in that described
The high frequency infrared ray carbon sulphur analyser of step (4), instrument model are that U.S.'s power can CS600.
8. the method for carbon content in a kind of measurement ferro-niobium according to claim 1 to 3, which is characterized in that described
In the high frequency infrared ray carbon sulphur analyser measurement analytic process of step (4), before measuring ferro-niobium sample, marked using steel standard sample
Standardization correction carries out the blank test of fluxing agent, the electronic compensation of blank value is then carried out when measuring ferro-niobium sample before measuring.
9. the method for carbon content in a kind of measurement ferro-niobium according to claim 1 to 3, which is characterized in that described
The high frequency infrared ray carbon sulphur analyser of step (4), running parameter are as follows: purge time: 10s, delay time: 20s, analysis time:
40s, comparator are horizontal: 2%, it cleans and is spaced: 5 times.
10. the method for carbon content in a kind of measurement ferro-niobium according to claim 1 to 3, which is characterized in that institute
The carbon content range for stating method detection ferro-niobium sample is C >=0.03%.
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