CN114235734A - Method for determining high-sulfur content in pyrite - Google Patents
Method for determining high-sulfur content in pyrite Download PDFInfo
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- CN114235734A CN114235734A CN202111244403.7A CN202111244403A CN114235734A CN 114235734 A CN114235734 A CN 114235734A CN 202111244403 A CN202111244403 A CN 202111244403A CN 114235734 A CN114235734 A CN 114235734A
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- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052683 pyrite Inorganic materials 0.000 title claims abstract description 84
- 239000011028 pyrite Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 62
- 239000011593 sulfur Substances 0.000 title claims abstract description 48
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 48
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 64
- 239000002245 particle Substances 0.000 claims abstract description 54
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 47
- 239000010937 tungsten Substances 0.000 claims abstract description 47
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052718 tin Inorganic materials 0.000 claims abstract description 41
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 38
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- 238000002485 combustion reaction Methods 0.000 claims abstract description 12
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 15
- 230000004907 flux Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 34
- 238000005259 measurement Methods 0.000 abstract description 21
- 229910052742 iron Inorganic materials 0.000 abstract description 17
- 238000004458 analytical method Methods 0.000 abstract description 9
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 13
- 238000005303 weighing Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000004164 analytical calibration Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 description 1
- WXGWJJXYTWIFST-UHFFFAOYSA-L [O-]S([O-])(=O)=O.OS(O)(=O)=O.S.[Ba+2] Chemical compound [O-]S([O-])(=O)=O.OS(O)(=O)=O.S.[Ba+2] WXGWJJXYTWIFST-UHFFFAOYSA-L 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- NNIPDXPTJYIMKW-UHFFFAOYSA-N iron tin Chemical compound [Fe].[Sn] NNIPDXPTJYIMKW-UHFFFAOYSA-N 0.000 description 1
- JHOPGIQVBWUSNH-UHFFFAOYSA-N iron tungsten Chemical compound [Fe].[Fe].[W] JHOPGIQVBWUSNH-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000007 visual effect Effects 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
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- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for measuring high-sulfur content in pyrite, which uses a combustion infrared absorption method for measurement, takes ferric oxide, tin and tungsten as fluxing agents, and takes barium sulfate as a calibration sample to calibrate a working curve; the mass ratio of the ferric oxide to the pyrite is (6-18): 1; the mass ratio of the tin to the pyrite is (6-12): 1; the mass ratio of the tungsten to the pyrite is (24-50): 1. the invention uses ferric oxide to replace metallic iron (pure iron filings), and the ferric oxide is fully oxidized to generate sulfur dioxide gas, and the sulfur is released more completely. The ferric oxide can stabilize the whole combustion process, and has no splashing phenomenon generated when the metallic iron is combusted. In the implementation process of the invention, the analysis results of the measuring method adopting pure iron chips-tin particles-tungsten particles and pure iron chips-tungsten particles as fluxing agents are compared with the analysis results of the measuring method of the invention, and the results of the examples and the comparative examples show that the measuring method of the invention has reliable measured values and good precision.
Description
Technical Field
The invention belongs to the technical field of inorganic material detection, and particularly relates to a method for determining high sulfur content in pyrite.
Background
Pyrite is an important chemical raw material, and is mainly used for producing sulfuric acid, sulfur and chemical fertilizers, and the desulfurization by-products can also be used for smelting valuable metals in the sulfur. The sulfur content is an important index for evaluating the grade of the pyrite, so that the rapid and accurate determination of the sulfur content in the pyrite has important significance.
The sulfur content in the pyrite is high, and is usually between 15 and 50 percent. In the prior art, a gravimetric method, a combustion-neutralization titration method and a combustion-infrared absorption method are mostly adopted to determine the sulfur content in the pyrite. The gravimetric method belongs to an absolute measurement method, the measured value is accurate and reliable, but the method has longer measurement period and low working efficiency; the combustion-neutralization titration method needs visual judgment of the reaction end point, so that human errors are easy to generate, and the measurement precision is not ideal; compared with the former two determination methods, the combustion-infrared absorption method has the advantages of simple operation and high analysis speed, but the reliable high-sulfur standard sample is needed to carry out sulfur quantity value tracing (instrument working curve calibration), but because the pyrite standard sample is easy to deteriorate and has a short effective period, a gravimetric method is needed to periodically check the reliability of a sulfur standard value, and manpower and material resources are wasted.
Disclosure of Invention
The invention aims to provide a method for measuring the high sulfur content in pyrite, which is simple and convenient to operate, high in detection efficiency, suitable for analysis of mass samples and high in practicability.
The invention provides a method for measuring high-sulfur content in pyrite, which uses a combustion infrared absorption method for measurement, takes ferric oxide, tin and tungsten as fluxing agents, and takes barium sulfate as a calibration sample to calibrate a working curve;
the mass ratio of the ferric oxide to the pyrite is (6-18): 1; the mass ratio of the tin to the pyrite is (6-12): 1; the mass ratio of the tungsten to the pyrite is (24-50): 1.
preferably, the barium sulfate is high-purity barium sulfate, and the purity of the high-purity barium sulfate is not less than 99.95%.
Preferably, a flux of the same mass and composition as the pyrite is measured is added when the working curve is calibrated using barium sulfate.
Preferably, the measured results of barium sulfate are used to plot a calibration operating curve against theoretical values.
Preferably, the mass ratio of the ferric oxide to the pyrite is (10-16): 1; the mass ratio of the tin to the pyrite is (8-10): 1; the mass ratio of the tungsten to the pyrite is (30-44): 1.
preferably, the mass ratio of the ferric oxide to the pyrite is 16: 1; the mass ratio of the tin to the pyrite is 8: 1; the mass ratio of the tungsten to the pyrite is 44: 1.
preferably, the particle size of the ferric oxide is less than 0.106 mm.
Preferably, the particle size of the tin is 0.38-0.83 mm.
Preferably, the particle size of the tungsten is 0.38-0.83 mm.
Preferably, the pyrite to be detected is placed in a carbon-sulfur ceramic crucible, ferric oxide is added to be mixed with the pyrite to be detected, and then tin and tungsten are added for detection.
The invention provides a method for measuring high-sulfur content in pyrite, which uses a combustion infrared absorption method for measurement, takes ferric oxide, tin and tungsten as fluxing agents, and takes barium sulfate as a calibration sample to calibrate a working curve; the mass ratio of the ferric oxide to the pyrite is (6-18): 1; the mass ratio of the tin to the pyrite is (6-12): 1; the mass ratio of the tungsten to the pyrite is (24-50): 1. the invention uses ferric oxide to replace metallic iron (pure iron filings), and the action mechanism is that ferric oxide powder can react with sulfur in pyrite, and is fully oxidized to generate sulfur dioxide gas, and the sulfur is released more completely. Another advantage is that the ferric oxide can stabilize the whole combustion process without splashing phenomenon generated when the metallic iron is combusted. In the specific implementation process of the invention, the analysis results of the measuring method adopting pure iron chips-tin particles-tungsten particles and pure iron chips-tungsten particles as fluxing agents are compared with the analysis results of the measuring method of the invention, and the results of the examples and the comparative examples show that the measuring method of the invention has reliable measured values and good precision.
Detailed Description
The invention provides a method for measuring high-sulfur content in pyrite, which uses a combustion infrared absorption method for measurement, takes ferric oxide, tin and tungsten as fluxing agents, and takes barium sulfate as a calibration sample to calibrate a working curve;
the mass ratio of the ferric oxide to the pyrite is (6-18): 1; the mass ratio of the tin to the pyrite is (6-12): 1; the mass ratio of the tungsten to the pyrite is (24-50): 1.
according to the principle of high-frequency furnace heating, a proper fluxing agent is required to be added into a sample to be measured so as to completely release sulfur in the sample. Compared with the method for measuring the sulfur content in the pyrite under the flux condition provided by the prior art, such as pure iron filings-tungsten particles and pure iron filings-tin particles-tungsten particles, the method has the problems that the stability of a measurement result is not good enough, and the sulfur in barium sulfate used for calibration is not completely released, so that the accuracy of the result is poor. The inventor of the present invention believes that, in order to overcome the problems existing in the foregoing and enable the analysis technology of the high frequency infrared absorption method to be used for simultaneously determining the sulfur content in the pyrite, the key problem is to select and obtain a proper fluxing agent so as to enable sulfur in different samples to be simultaneously and fully oxidized into sulfur dioxide gas and to be released completely as far as possible for the detection of an infrared absorber, so as to reduce the measurement error as far as possible.
In the invention, the sulfur content in the pyrite is measured by a high-frequency induction furnace combustion infrared absorption method, and in the measuring process by the high-frequency induction furnace combustion infrared absorption method, the fluxing agents used are ferric oxide powder, tin particles and tungsten particles. Specifically, a pyrite or barium sulfate calibration sample is quantitatively weighed and placed in a carbon-sulfur ceramic crucible, ferric oxide powder is added to be mixed with the sample, and then tin particles and tungsten particles are added to carry out determination.
In the present invention, the particle size of the iron oxide trioxide is preferably less than 0.106 mm; the particle size of the tin particles is preferably 0.38-0.83 mm; the particle size of the tungsten particles is preferably 0.38-0.83 mm.
In the invention, the mass ratio of the ferric oxide powder to the pyrite sample to be detected is preferably (6-18):1, such as 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, preferably any of the above values is an upper or lower limit.
In the invention, the mass ratio of the tin particles to the pyrite sample to be detected is preferably (6-12):1, such as 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, preferably any of the above values is the upper or lower limit.
In the invention, the mass ratio of the tungsten particles to the pyrite sample to be detected is preferably (24-50): 1, such as 24:1, 25:1, 26:1, 27:1, 28:1, 29:1, 30:1, 31:1, 32:1, 33:1, 34:1, 35:1, 36:1, 37:1, 38:1, 39:1, 40:1, 41:1, 42:1, 43:1, 44:1, 45:1, 46:1, 47:1, 48:1, 49:1, 50:1, preferably any of the above values is an upper limit or a lower limit.
In the calibration measurement using the high-purity barium sulfate calibration sample, a flux of the same mass and composition as in the measurement of the pyrite sample was added.
In the invention, the high-purity barium sulfate calibration samples, namely calibration points with different sulfur contents (mass fractions), are realized by weighing barium sulfate with different masses and manually inputting the sample mass with fixed mass during measurement.
The invention preferably enables the determination of the sulphur content in pyrite using a CS844 high frequency furnace infrared carbon-sulphur instrument, supplied by LECO, usa.
The invention provides a method for measuring high-sulfur content in pyrite, which uses a combustion infrared absorption method for measurement, takes ferric oxide, tin and tungsten as fluxing agents, and takes barium sulfate as a calibration sample to calibrate a working curve; the mass ratio of the ferric oxide to the pyrite is (6-18): 1; the mass ratio of the tin to the pyrite is (6-12): 1; the mass ratio of the tungsten to the pyrite is (24-50): 1. the invention uses ferric oxide to replace metallic iron (pure iron filings), and the action mechanism is that ferric oxide powder can react with sulfur in pyrite, and is fully oxidized to generate sulfur dioxide gas, and the sulfur is released more completely. Another advantage is that the ferric oxide can stabilize the whole combustion process without splashing phenomenon generated when the metallic iron is combusted. In the specific implementation process of the invention, the analysis results of the measuring method adopting pure iron chips-tin particles-tungsten particles and pure iron chips-tungsten particles as fluxing agents are compared with the analysis results of the measuring method of the invention, and the results of the examples and the comparative examples show that the measuring method of the invention has reliable measured values and good precision.
In order to further illustrate the present invention, the following will describe in detail a method for determining high sulfur content in pyrite, which is provided by the present invention, with reference to the following examples, but it should not be construed as limiting the scope of the present invention.
Example 1
In the condition test, the invention takes the condition that the measured value of sulfur in the pyrite sample and the calibration sample (barium sulfate) is stable as the preferable range.
(1) The amount of ferric oxide powder
Weighing a certain mass of pyrite (sample A) to be measured by using an electronic balance, and accurately measuring the mass of pyrite to be measured to be 0.1 mg; the calibration sample (high purity barium sulfate) was tested using the highest calibration point (50.00% by mass sulfur). Putting the weighed sample into a carbon-sulfur ceramic crucible, adding ferric oxide powder with different masses, and mixing with the sample; and fixedly adding tin particles and tungsten particles, wherein the mass ratio of the tin particles to the pyrite sample is 6:1 and 40:1 respectively. The flux used for the calibration sample was consistent with pyrite. The ceramic crucible is placed on a high-frequency infrared carbon-sulfur instrument to measure the content of carbon and sulfur, the operation is carried out according to the instruction of the instrument, and the measured values are shown in table 1. As can be seen from Table 1, the sulfur measurement results for both samples were stable at a mass ratio of ferric oxide to sample of (6-18): 1.
TABLE 1
(2) Mass ratio of tin particles to sample
Weighing a pyrite sample (sample A) to be measured by using an electronic balance, accurately measuring the pyrite sample (sample A) to 0.1mg, placing the sample in a carbon-sulfur ceramic crucible, fixedly adding ferric oxide powder, wherein the mass ratio of the ferric oxide powder to the sample is 16:1, then adding tin particles with different masses, and finally adding tungsten particles with fixed masses, wherein the mass ratio of the tungsten particles to the sample is 40: 1. The flux used for the calibration sample was consistent with pyrite. The carbon-sulfur ceramic crucible is placed on a high-frequency infrared carbon-sulfur instrument to measure the content of carbon and sulfur, the operation is carried out according to the instruction of the instrument, and the measured values are shown in table 2. As can be seen from Table 2, the sulfur measurement results in both samples were stable at a tin particle to sample mass ratio of (6-12): 1.
TABLE 2
(3) Mass ratio of tungsten particles to sample
Weighing a pyrite sample (sample A) to be detected by using an electronic balance, accurately measuring the pyrite sample (sample A) to 0.1mg, placing the pyrite sample in a carbon-sulfur ceramic crucible, fixedly adding ferric oxide powder, wherein the mass ratio of the ferric oxide powder to the sample is 16:1, adding tin particles with fixed mass, wherein the mass ratio of the tin particles to the sample is 8:1, and finally adding tungsten particles with different masses. The flux used for the calibration sample was consistent with pyrite. The carbon-sulfur ceramic crucible is placed on a high-frequency infrared carbon-sulfur instrument to measure the sulfur content, the operation is carried out according to the instrument instruction, and the measured values are shown in table 3. As can be seen from Table 3, when the mass ratio of tungsten particles to the sample is (24-50): in 1 hour, the sulfur measurement results of the two samples are stable.
TABLE 3
Comparative example 1
Weighing a pyrite sample A to be measured and a calibration sample (barium sulfate) by using an electronic balance, accurately measuring the sample A to be measured and the calibration sample (barium sulfate) to 0.1mg, placing the weighed sample A and the calibration sample (barium sulfate) into a carbon-sulfur ceramic crucible, and adding ferric oxide powder, tin particles and tungsten particles, wherein the mass ratio of the ferric oxide powder, the tin particles and the tungsten particles to the sample is 16:1, 8:1 and 44:1 respectively. According to the method of the invention, high-purity barium sulfate is adopted for instrument calibration, the two samples are weighed simultaneously, the conditions of the fluxing agent in the prior art, namely scrap iron-tungsten particles or scrap iron-tin particles-tungsten particles, are adopted for determination, and the results are compared, which is shown in Table 4. As can be seen from the results in Table 4, the results of the measurement of the method of the present invention are higher than those of the other two methods, and the standard deviation of the results of the method of the present invention is significantly better than those of the other two methods.
TABLE 4
Example 2
Weighing barium sulfate calibration samples with different masses by using an electronic balance according to a calibration working curve, accurately measuring the barium sulfate calibration samples to 0.1mg, placing the barium sulfate calibration samples in a ceramic crucible, manually inputting the sample mass with fixed mass in analysis software, adding ferric oxide, tin particles and tungsten particles according to the invention, wherein the mass ratio of the ferric oxide, the tin particles and the tungsten particles to the input sample is respectively 16:1, 8:1 and 44:1, placing the carbon-sulfur ceramic crucible on an instrument to measure the sulfur content, and operating according to the instruction of the instrument to measure the sulfur content.
TABLE 5
| Numbering | Theoretical value of sulfur (wt%) | Measured value (wt%) of inventive example | Average value (wt%) |
| 1 | 15.00 | 15.00，14.98 | 14.99 |
| 2 | 20.00 | 19.98，19.96 | 19.97 |
| 3 | 30.00 | 30.01，29.95 | 29.98 |
| 4 | 40.00 | 39.99，40.03 | 40.01 |
| 5 | 50.00 | 50.01，49.95 | 49.98 |
Example 3
Weighing a pyrite standard sample to be measured by an electronic balance, accurately measuring the sample to 0.1mg, placing the sample in a carbon-sulfur ceramic crucible, adding ferric oxide, tin particles and tungsten particles, wherein the mass ratio of the ferric oxide to the sample to the tungsten particles to the sample is 16:1, 8:1 and 44:1 respectively, placing the carbon-sulfur ceramic crucible on an instrument to measure the sulfur content, and measuring according to the operation of an instrument instruction. The results of the sulfur measurement of the standard sample were obtained using a calibration curve prepared by plotting the measurement results of the high purity barium sulfate sulfur in example 2 and the theoretical values, and compared with the standard values of sulfur of the standard sample, and the results are shown in table 6. As can be seen from Table 6, the results of sulfur measurement in the pyrite standard sample according to the present invention are consistent with the standard values.
TABLE 6
Example 4
Weighing a pyrite sample to be measured by an electronic balance, accurately measuring the pyrite sample to be measured to 0.1mg, placing the pyrite sample in a carbon-sulfur ceramic crucible, and adding ferric oxide, tin particles and tungsten particles, wherein the mass ratio of the ferric oxide to the sample to the tungsten particles to the sample is 16:1, 8:1 and 44:1 respectively. According to the method of the invention, high-purity barium sulfate is used for instrument calibration, and the pyrite sample is subjected to 8 parallel measurements and compared with the results of the barium sulfate gravimetric method, and the results are shown in Table 7. As can be seen from the results in Table 7, the method of the present invention provides good precision of the measurement results, which are consistent with the results of the gravimetric method.
TABLE 7
In conclusion, the method solves the problem of measuring the high sulfur content in the pyrite by the high-frequency furnace combustion infrared absorption method, is applied to actual production, improves the efficiency of related detection, reduces the production cost and has a good effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for measuring high sulfur content in pyrite is characterized in that a combustion infrared absorption method is used for measuring, ferric oxide, tin and tungsten are used as fluxing agents, and barium sulfate is used as a calibration sample to calibrate a working curve;
the mass ratio of the ferric oxide to the pyrite is (6-18): 1; the mass ratio of the tin to the pyrite is (6-12): 1; the mass ratio of the tungsten to the pyrite is (24-50): 1.
2. the method of claim 1, wherein the barium sulfate is high purity barium sulfate, and the purity of the high purity barium sulfate is not less than 99.95%.
3. The method of claim 2, wherein a flux of the same mass and composition as the pyrite is measured is added when the working curve is calibrated using barium sulfate.
4. The method of claim 3, wherein the calibration operating curve is plotted using the measured results and theoretical values of barium sulfate.
5. The method according to claim 1, wherein the mass ratio of the ferric oxide to the pyrite is (10-16): 1; the mass ratio of the tin to the pyrite is (8-10): 1; the mass ratio of the tungsten to the pyrite is (30-44): 1.
6. the method according to claim 5, wherein the mass ratio of the ferric oxide to the pyrite is 16: 1; the mass ratio of the tin to the pyrite is 8: 1; the mass ratio of the tungsten to the pyrite is 44: 1.
7. the method of claim 6, wherein the ferric oxide has a particle size of less than 0.106 mm.
8. The method according to claim 7, wherein the tin has a particle size of 0.38 to 0.83 mm.
9. The method according to claim 8, wherein the tungsten has a particle size of 0.38 to 0.83 mm.
10. The method according to any one of claims 1 to 9, characterized in that the pyrite to be detected is placed in a carbon-sulfur ceramic crucible, ferric oxide is added to mix with the pyrite to be detected, and tin and tungsten are added for determination.
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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