KR0143493B1 - Combustion supporting composition for the analysis of carbon & sulphur in molten metal - Google Patents
Combustion supporting composition for the analysis of carbon & sulphur in molten metalInfo
- Publication number
- KR0143493B1 KR0143493B1 KR1019940038973A KR19940038973A KR0143493B1 KR 0143493 B1 KR0143493 B1 KR 0143493B1 KR 1019940038973 A KR1019940038973 A KR 1019940038973A KR 19940038973 A KR19940038973 A KR 19940038973A KR 0143493 B1 KR0143493 B1 KR 0143493B1
- Authority
- KR
- South Korea
- Prior art keywords
- carbon
- analysis
- sample
- weight
- pure
- Prior art date
Links
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000000203 mixture Substances 0.000 title claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 24
- 229910052799 carbon Inorganic materials 0.000 title abstract description 23
- 238000002485 combustion reaction Methods 0.000 title abstract description 22
- 229910052751 metal Inorganic materials 0.000 title description 2
- 239000002184 metal Substances 0.000 title description 2
- 239000005864 Sulphur Substances 0.000 title 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 79
- 229910052742 iron Inorganic materials 0.000 claims abstract description 39
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 30
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000010937 tungsten Substances 0.000 claims abstract description 29
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 24
- 239000011593 sulfur Substances 0.000 claims abstract description 24
- 229910000975 Carbon steel Inorganic materials 0.000 claims 1
- 239000010962 carbon steel Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000000446 fuel Substances 0.000 abstract description 3
- 239000000701 coagulant Substances 0.000 abstract 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- 230000006698 induction Effects 0.000 description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 6
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000003063 flame retardant Substances 0.000 description 5
- 229960004424 carbon dioxide Drugs 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910001930 tungsten oxide Inorganic materials 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- -1 respectively Chemical compound 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
-
- 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
Abstract
연소적외선 흡광법에 의한 용선중의 탄소 및 유황 분석시 시료의 연소를 촉진하기 위한 조연제로서 시료 100중량부를 기준으로 순철 280-360중량부, 및 순수 텅스텐 600-800중량부로 조성된 조연제가 제공된다.As a coagulant for promoting combustion of the sample during carbon and sulfur analysis in molten iron by the combustion infrared absorption method, a coagulant composed of 280-360 parts by weight of pure iron and 600-800 parts by weight of pure tungsten is provided based on 100 parts by weight of the sample. do.
이같은 조연제를 사용함으로써 탄소 및 유황 분석시 최적의 연소상태를 유지시켜 시료를 완전 연소시킴으로써 분석 데이타의 정확도 및 재현성을 극대화하고 분석 잔유물을 극소화하여 기기의 운전상태를 최적화 시킬 수 있다.The use of these fuels helps to optimize the operating conditions of the instrument by maximizing the accuracy and reproducibility of the analytical data and minimizing the analytical residues by maintaining the optimum combustion conditions for carbon and sulfur analysis.
Description
본 발명은 용선중에 함유되어 있는 탄소 및 유황분석용 조연제 조성물에 관한 것이며, 보다 상세하게는 가열 연소에 의한 적외선 흡광법으로 용선중에 함유되어 있는 탄소 및 유황성분을 분석함에 있어 시료의 연소 촉진제를 첨가되는 용선중의 탄소 및 유황 분석용 조연제 조성물에 관한 것이다.The present invention relates to a carbon and sulfur analyte composition for analyzing carbon and sulfur contained in molten iron, and more particularly, in order to analyze carbon and sulfur components contained in molten iron by infrared absorption by heat and combustion. The present invention relates to a carbon and sulfur analysis aid composition for molten iron added.
종래 탄소 및 유황을 분석하는 경우, 일반적으로 분석하고자 하는 시료를 일정한 규격(분말, 칩)으로 가공한 후 분석기 자체에 부착되어 있는 천청위에 도가니를 올려놓고 시료를 평량, 무게값을 입력한 다음, 순수 텅스텐(4.0g) 조연제를 첨가하여 고주파 유도 용해로에 정입한 다음 산소를 공급하면서 1300℃~1800℃로 가열 연소시키는 탄소 및 유황분석기를 이용한 적외선 흡광법이 이용되어 왔다.In the case of analyzing carbon and sulfur in the prior art, in general, after processing the sample to be analyzed to a certain standard (powder, chip), put the crucible on the ceiling attached to the analyzer itself, enter the basis weight and weight value, Infrared absorption using a carbon and sulfur analyzer has been used in which a pure tungsten (4.0 g) supporting agent is added to a high frequency induction furnace and heated and burned at 1300 ° C to 1800 ° C while supplying oxygen.
상기 공정중에서 고주파 유도 용해로를 이용한 가열 연소 공정은 고주파 유도 용해로내의 연소부에 설치되어 있는 유도코일에 고주파 전류가 공급되면 유도코일 죄, 우측에 강한 자장이 형성됨과 동시에 중심부에 자력이 형성된다.In the heating combustion process using the high frequency induction melting furnace during the above process, when a high frequency current is supplied to the induction coil installed in the combustion unit in the high frequency induction melting furnace, a strong magnetic field is formed on the right side of the coil and a magnetic force is formed at the center.
이때 유도코일 중심부에 장입된 도가니 내에서는 조연제로 첨가된 순수텅스텐은 자력에 의해 연소되며, 급격한 산화열이 발생되기 때문에 시료가 연소된다.At this time, in the crucible charged in the center of the induction coil, pure tungsten added as a supporting agent is burned by magnetic force, and a sample is burned because of rapid heat of oxidation.
상기의 공정에서 시료(용선)에 함유된 탄소 및 유황은 시료가 연소되면서 공급되는 산소와 반응하여 하기반응식(1)에 따라 Fe2O3SiO2, P2O5, MnO등 분석잔유물과 함께 이산탄소 및 일산화탄소, 이산화황 및 삼산화황 가스가 발생된다.In the above process, carbon and sulfur contained in the sample (molten iron) react with oxygen supplied as the sample is burned, and together with the analytical residues such as Fe 2 O 3 SiO 2 , P 2 O 5 , MnO according to the following Reaction Formula (1) Carbon dioxide and carbon monoxide, sulfur dioxide and sulfur trioxide gases are generated.
상기 반응식(1)에서 발생되는 분석 잔유물은 고체상태와 미세한 분말상태로 발생되며 이중 고체 상태인 것은 도가니 내벽 및 연소관 내벽에 부착되고 미세한 분말상태인 것은 가스 통로에 설치되어 있는 메탈필터에서 여과되며, 분석가스로 발생되는 이산화탄소 및 일산화탄소, 이산화황 및 삼산화황은 강 산화제가 충진된 백금촉매를 통과하면서 일산화탄소는 이산화탄소로, 삼산화황은 이산화황으로 각각 산화되어 적외선 흡광법에 의하여 이산화탄소가 탄소로, 이산화황이 유황으로 각각 변환되어져 정량화된다.The analytical residue generated in the reaction formula (1) is generated in a solid state and a fine powder state, the solid state of which is attached to the inner wall of the crucible and the combustion tube, and the fine powder state is filtered by a metal filter installed in the gas passage, Carbon dioxide, carbon monoxide, sulfur dioxide and sulfur trioxide generated from the analytical gas are oxidized through a platinum catalyst filled with a strong oxidant, and carbon monoxide is oxidized to carbon dioxide, sulfur trioxide to sulfur dioxide, respectively, and carbon dioxide is carbon and sulfur dioxide is sulfur by infrared absorption. Is converted and quantified.
이와같이 종래의 분석공정중 가장 중요한 공정은 고주파 유도용해로에 의한 가열연소 공정으로서 조연제의 조성은 도가니에 걸리는 전류량의 변화를 가져오며 이에 따라 연소 온도가 변화되고 이에 따라 연소 상태가 변화된다.As such, the most important process of the conventional analysis process is a heating combustion process by a high frequency induction furnace, and the composition of the supporting agent brings about a change in the amount of current applied to the crucible, and thus the combustion temperature is changed and thus the combustion state is changed.
그러나 종래 용선중의 조연제로 사용되는 순수텅스텐은 열전도성이 낮아 자력에 의해 큰 저항이 형성되며, 상기 텅스텐을 과량 첨가함으로 해서 도가니 바닥면에 있는 시료가 잘 응용되지 않으며 특히 시료의 과다평량과 텅스텐의 과다첨가로 시료 및 텅스텐이 비산하여 연소관을 손상시키는 문제 및 시료의 비산으로 분석의 정확도 및 재현성이 저하되는 문제점이 있었다.However, pure tungsten, which is used as a softener in conventional molten iron, has a low thermal conductivity, and thus a large resistance is formed by magnetic force, and the sample on the bottom surface of the crucible is not applied well by adding an excess of tungsten. Due to the excessive addition of the sample and tungsten scattered damage to the combustion tube and the scattering of the sample has a problem of lowering the accuracy and reproducibility of the analysis.
이에 본 발명의 목적은 상기와 같은 종래의 탄소 및 유황성분 분석방법의 문제점을 해결한 보다 개선된 탄소 및 유황분석용 조연제를 제공하는 것이다.Accordingly, an object of the present invention is to provide an improved carbon and sulfur analyzing aid that solves the problems of the conventional method of analyzing carbon and sulfur as described above.
본 발명의 다른 목적은 연소적외선 흡광법으로 용선중의 탄소 및 유황분석시 최적의 연소상태를 유지시켜 시료를 완전 용융시킴으로써 분석데이타의 정화도 및 재현성을 극대화하고 분체상태의 분석잔유를 극소화시켜 기기의 오염을 최소화 할 수 있는 보다 개선된 조연제를 제공하는 것이다.It is another object of the present invention to maintain the optimum combustion state in the analysis of carbon and sulfur in molten iron by combustion infrared absorption method to completely melt the sample to maximize the purification and reproducibility of the analysis data and to minimize the analysis residue in the powder state It is to provide a more improved fuel retardant that can minimize the contamination.
본 발명에 의하면, 시료 100를 기준으로, 순철 280~360중량부와 순수텅스텐 600-800중량부로 조성된 용선중 탄소 및 유황분석용 조연제 조성물이 제공된다.According to the present invention, based on the sample 100, there is provided a carbon and sulfur analyzing aid composition for analysis of molten iron composed of 280 to 360 parts by weight of pure iron and 600-800 parts by weight of pure tungsten.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
적외선 흡광법을 이용한 탄소 및 유황분석시 사용되는 조연제로서 순철과 텅스텐을 함께 사용함으로써 최적의 연소상태를 유지시켜 시료를 완전용융시킴으로써 분석의 정확도 및 재현성을 개선시킬수 있는 것이다.By using a combination of pure iron and tungsten as the coarse agent used in carbon and sulfur analysis using infrared absorption method, it is possible to improve the accuracy and reproducibility of the analysis by maintaining the optimum combustion state and melting the sample completely.
상기 텅스텐(W)은 열전도성이 낮아 자력에 의해 큰 저항이 형성되며 이같은 텅스텐이 연소될때 고온의 산화열이 발생되며 이열에 의해 텅스텐 산화물, 순철 및 시료가 연쇄적으로 반응하여 연소됨으로써 최적의 연소상태를 유지하고자 하였다.The tungsten (W) has a low thermal conductivity, so a large resistance is formed by magnetic force, and when such tungsten is burned, high-temperature oxidation heat is generated, and by this heat, tungsten oxide, pure iron, and a sample are reacted in series to be burned for optimum combustion. The state was to be maintained.
상기 조연제 조성물중 순철 및 순수텅스텐은 시료 100중량부 기준으로, 순철 280-360중량부 및 순수텅스텐 600-800중량부로 조성된 것이 바람직화다. 순철 및 순수 턴스텐이 각각 80, 600중량부 이하인 경우에는 시료등이 완전히 산화되지 않으며, 각각 360, 800중량부 이상인 경우에는 연소반응 후 도가니내에 잔유물이 다량발생된다. 또한 상기 순철 및 텅스텐은 그 순도가 가각 99.999%이상의 것이다.Pure iron and pure tungsten is preferably composed of 280-360 parts by weight of pure iron and 600-800 parts by weight of pure tungsten based on 100 parts by weight of the sample. When the pure iron and pure turnsten are 80 or 600 parts by weight or less, the sample is not completely oxidized, and when 360 or 800 parts by weight or more, respectively, large amounts of residues are generated in the crucible after the combustion reaction. In addition, the pure iron and tungsten are each 99.999% or more of purity.
본 발명의 조연제를 이용하여 용선중의 탄소 및 유황을 분석하는 경우, 먼저 시료를 일정한 규격(분말, 칩)으로 가공한 다음 분석기 자체에 부착된 천칭위에 도가니를 올려 놓고 시료 100중량부(예를들어 0.25g)를 기준으로 순철 280-360 중량부(0.7-0.9g)를 평량하여 도가니에 장입한다.When analyzing carbon and sulfur in molten iron using the present invention, the sample is first processed into a standard (powder, chip), and then a crucible is placed on a balance attached to the analyzer itself. For example, based on 0.25 g), 280-360 parts by weight (0.7-0.9 g) of pure iron is weighed into a crucible.
그후 분석기에 부착된 천칭을 이용하여 분석하고자 하는 시료의 무게를 평량하여 도가니에 장입하고, 컴퓨터에 입력시키고나서 시료 100중량부를 기준으로 순수 텅스텐 600-800중량부(1.5g-2.0g)를 평량하여 도가니에 장입한다. 그후 조연제와 시료가 장입된 도가니를 고주파 유도 용해로에 장진시켜 다음 잔류를 공급하여 분석한후, 분석이 완료된 폐 도가니를 제거함으로서 분석은 종료된다.Then, using the balance attached to the analyzer, the weight of the sample to be analyzed is weighed into a crucible, input into a computer, and then 600-800 parts by weight of pure tungsten (1.5g-2.0g) based on 100 parts by weight of the sample. To the crucible. After that, the crucible loaded with the flame retardant and the sample is loaded into a high frequency induction furnace and analyzed by supplying the next residue, and then the analysis is completed by removing the waste crucible after the analysis is completed.
상기한 바와같이 순철, 시료 및 순수 텅스텐의 순으로 도가니에 넣고 고주파 유도 용해로의 유도코일 중앙에 도가니를 장입후 고주파 전류를 공급하면 고주파 코일 좌, 우측에 강한 자장이 형성됨과 동시에 중심부에 자력이 형성되고, 상기 순철, 시료 및 순수 텅스텐은 용융되어 상기 조성으로 혼합된다. 상기 조연제로 사용되는 순철 및 순수텅스텐을 상기 조성으로 혼합하여 첨가할 수도 있으나, 순철의 경우 강한 전류를 걸어주게 되면 비산됨으로 상기한 순서에 따라 도가니에 장입하는 것이 바람직하다.Put the crucible in the order of pure iron, sample and pure tungsten as described above, insert the crucible in the center of the induction coil of the high frequency induction furnace, and supply high frequency current to form a strong magnetic field on the left and right sides of the high frequency coil and at the same time, the magnetic force is formed in the center. The pure iron, sample and pure tungsten are melted and mixed into the composition. Pure iron and pure tungsten used as the supporting agent may be mixed and added to the composition, but in the case of pure iron, it is preferable to charge the crucible according to the above procedure because it is scattered when a strong current is applied.
상기 순철, 시료 및 텅스텐 순서로 장입된 도가니에 고주파 전류를 걸어주면 조연제는 도가니내에서 용융되어 균일한 조성물로 존재하게되며, 후술하는 바와같이 반응하여 시료(용선)중 탄소 및 유황성분이 분석된다.When a high frequency current is applied to the crucible loaded in the order of pure iron, the sample and tungsten, the flame retardant is melted in the crucible to exist as a uniform composition, and as described below, the carbon and sulfur components in the sample (molten iron) are analyzed. do.
전류를 공급함과 동시에 열전도성이 낮은 텅스텐은 자력에 의한 큰 저항이 형성되어 제일 먼저 도가니 내에서 하기 식(2)와 같이 반응하여 연소된다.At the same time as supplying current, tungsten with low thermal conductivity forms a large resistance due to magnetic force, and first reacts and burns in a crucible as shown in the following formula (2).
상기 식(2)에서 나타난 바와같이 텅스텐 산화물(W2O3)은 분체 상태의 분석 잔유물로서 시료 분석시 필연적으로 발생되는 잔유물이다.As shown in Equation (2), tungsten oxide (W 2 O 3 ) is an analytical residue in a powder state and is inevitably generated during sample analysis.
하기 식(3)에서 생성되는 분석잔유물(W, Fe, Mn, SiOn)은 도가니내의 온도가 1300℃-1800℃로 유지될때 생성됨으로 상기 고온의 산화열이 필수적인 것이다.Analysis residues (W, Fe, Mn, SiOn) produced in the following formula (3) is generated when the temperature in the crucible is maintained at 1300 ℃-1800 ℃ is the heat of high temperature oxidation is essential.
상기 식(2)의 반응이 진행되면서 발생하는 산화열로 인하여 도가니내에서 텅스텐산화물 순철 및 시료가 하기식(3)과 같이 반응하여 연소된다.Due to the heat of oxidation generated as the reaction of Equation (2) proceeds, the tungsten oxide pure iron and the sample in the crucible react and combust as shown in the following Equation (3).
상기 식(3)에서 나타난 바와같이 상기 식(2)에서 생성된 분말상태의 텅스텐 산화물은 상기 식(3)의 순철, 텅스텐 및 시료와 연쇄적으로 가열반응하여 텅스텐 및 철을 주성분으로 하는 고체 상태의 분석 잔유물로 도가니 내벽에 부착되기 때문에 분체상태이 분석 잔유물을 극소화 할 수 있을 뿐만 아니라, 연소상태의 최적 유지가 가능하여 분석의 정확도 및 재현성을 극대화 할 수 있는 것이다. 또한 조연제로서 순철을 사용함으로써 시료의 용점 또한 저하된다.As shown in Equation (3), the powdered tungsten oxide produced in Equation (2) is thermally reacted with pure iron, tungsten and the sample of Equation (3) in a solid state containing tungsten and iron as main components. Because it is attached to the inner wall of the crucible as an analysis residue of, it is possible not only to minimize the analysis residue, but also to maintain the optimum combustion state, thereby maximizing the accuracy and reproducibility of the analysis. Moreover, the melting point of the sample is also lowered by using pure iron as a supporting agent.
이하, 본 발명의 실시예에 대하여 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, the Example of this invention is described.
[실시예 1]Example 1
본 발명에 의한 조연제 첨가제애 대한 성분 및 조성량을 변화시켜 시료의 용융상태, 연소란 파손상태, 분석시간 및 분석의 정확성등에 대하여 조사하였으며, 그 결과를 하기표 1에 나타내었다.The molten state of the sample, the burned state, the breakage state, the analysis time and the accuracy of the analysis were investigated by changing the composition and the amount of the additive for the flame retardant additive according to the present invention, and the results are shown in Table 1 below.
상기 표(1)에 의하면 시료무게 0.25g을 기준으로 하여 순철(Fe)과 순수텅스텐(W)의 양을 변화시켜 실시한 결과 순철 0.1g 및 순수 텅스텐 0.5g을 투입하였을 경우 유도코일에 걸리는 전류는 180-200mA로서 연소상태가 극히 불량하며 조연제가 비산되어 연소관을 손상시킬 뿐만 아니라 시료중의 탄소 및 유황성분이 충분히 연소되지 않아 분석의 정화도 및 재현성이 극히 저하되었으며, 순수 텅스텐 1.0g, 순철 0.3g을 투입한 결과도 같은 결과를 나타내었다.According to the above table (1), the amount of pure iron (Fe) and pure tungsten (W) was changed based on the sample weight of 0.25 g. As a result, when 0.1 g of pure iron and 0.5 g of pure tungsten were added, the current applied to the induction coil was As the combustion state is 180-200mA, the combustion condition is extremely poor, and the flame retardant is scattered, which not only damages the combustion tube but also the carbon and sulfur components in the sample are not sufficiently burned, and the purity and reproducibility of the analysis are extremely reduced. Pure tungsten 1.0g, pure iron 0.3 The result of adding g also showed the same result.
또한 순수 텅세튼 3.0g-4.0g, 순철 1.2g-1.5g을 투입한 경우 순수 텅스텐과 순철이 다량 첨가되어 고주파 유도 용해로의 공급전류의 과부하 발생으로 유도 코일에 걸리는 전류가 460mA-480mA이상으로 변화되면서 분석되어지고, 분말상태의 분석 잔유물이 다량 발생될뿐만 아니라 도가니내의 온도저하로 시료내의 탄소 및 유황성분이 충분히 연소되지 않는 결점이 있음을 확인할 수 있었다. 그러나 순수 텅스텐 1.5-2.0g과 순철 0.7-0.9g을 투입하여 실시한 결과, 유도코일에 걸리는 전류는 420mA-450mA로 도가니 내의 저정온도 1300℃-1800℃가 유지되어 상기(3)의 분석 잔유물인 텅스텐과 철을 주성분으로 하는 고체 상태의 분석 잔유물이 발생하였을 뿐만 아니라 시료가 완전 연소되어 분석의 정확도 및 재현성을 극대화 할 수 있음을 확인할 수 있었다.In addition, when pure tungsten 3.0g-4.0g and pure iron 1.2g-1.5g are added, a large amount of pure tungsten and pure iron are added, and the current applied to the induction coil changes to more than 460mA-480mA due to the overload of the supply current of the high frequency induction furnace. As it was analyzed, the powdery analytical residues were not only generated in a large amount, but it was confirmed that the carbon and sulfur components in the sample were not sufficiently burned due to the temperature drop in the crucible. However, as a result of adding 1.5-2.0 g of pure tungsten and 0.7-0.9 g of pure iron, the current applied to the induction coil was 420 mA-450 mA, and the low temperature in the crucible was maintained at 1300 ° C-1800 ° C. It was confirmed that solid analytical residues based on tungsten and iron were generated as well as the samples were completely burned to maximize the accuracy and reproducibility of the analysis.
따라서, 용선중의 탄소 및 유황 분석시에 사용되는 조연제는 시료무게(0,.25g)기준으로 순수 텅스텐을 600중량부%-800중량%(1.5g-2.0g)와 순철 280중량%-360중량%(0.7g-0.9g)로 구성되는 것이 바람직하다.Therefore, the fuel retardant used for analyzing carbon and sulfur in molten iron is 600 parts by weight-800% by weight (1.5g-2.0g) and 280% by weight pure pure, based on the sample weight (0, .25g). It is preferably composed of 360% by weight (0.7g-0.9g).
[실시예 2]Example 2
본 발명의 조연제 및 종래의 조연제를 사용하여 탄소 및 유황성분 분석하였으며 그 결과를 하기표 2에 나타내었다.Carbon and sulfur components were analyzed by using the present invention and the conventional staring agent, and the results are shown in Table 2 below.
상기 표2에 의하면, 동일조성으로된 강재 시료로 1-10회 반복하여 분석한 결과 탄소농도는 본 발명의 경우 평균 3.3393%, 분석표준편차는 0.00427, 분석최대편차는 0.013이며, 비교예의 경우 평균은 3.3482%, 분석 표준편차는 0.01394%, 부넉 최대편차는 0.050로 나타났으며, 유황농도는 본 발명의 경우 평균 0.0104%, 분석 표준편차 0.00045, 분석 최대편차 0.0013이며 비교예의 경우 평균 0.0109%, 분석 표준편차 0.00134, 분석 최대편차 0.0038로 본발명의 경우가 비교예에 비하여 분석의 정확도 및 재현성이 매우 우수함을 확인할 수 있었으며, 또한 연소상태의 최적유지로 본체 형태의 분석잔유물 발생을 극소화 시킬 수 있음 또한 확인할 수 있었다.According to Table 2, the results of repeated analysis of steel samples of the same composition as a result of the carbon concentration is 3.3393%, the standard deviation is 0.00427, the analysis maximum deviation is 0.013 in the case of the present invention, the average in the comparative example Is 3.3482%, the standard deviation of analysis is 0.01394%, the maximum deviation is 0.050, the sulfur concentration is 0.0104% in the case of the present invention, the standard deviation of the standard deviation 0.00045, the analysis maximum deviation is 0.0013, the average 0.0109% in the comparative example, analysis The standard deviation of 0.00134 and the maximum analysis of deviation of 0.0038 showed that the present invention is more accurate and reproducible than the comparative example. Also, it is possible to minimize the occurrence of analyte residues in the form of the body by maintaining the optimum combustion state. I could confirm it.
상기에서 상술한 바와같이 본 발명은 용선 중에 함유되어 있는 탄소 및 유황분석시 사용되는 최상의 조연제 조성물을 개발함으로서 분석의 정확도 및 재현성을 확보함과 동시에 분체 형태의 분석 잔유물 발생을 극소화하여 기기운전 상태를 최적화 시킬 수 있는 효과가 있는 것이다.As described above, the present invention develops the best flame retardant composition to be used for carbon and sulfur analysis contained in molten iron, thereby ensuring the accuracy and reproducibility of the analysis and minimizing the generation of analytical residue in the form of powder. The effect is to optimize the.
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