CN114018847A - Device and method for measuring total sulfur content in solid sample - Google Patents
Device and method for measuring total sulfur content in solid sample Download PDFInfo
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- CN114018847A CN114018847A CN202111274391.2A CN202111274391A CN114018847A CN 114018847 A CN114018847 A CN 114018847A CN 202111274391 A CN202111274391 A CN 202111274391A CN 114018847 A CN114018847 A CN 114018847A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 75
- 239000011593 sulfur Substances 0.000 title claims abstract description 75
- 239000007787 solid Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 111
- 238000000197 pyrolysis Methods 0.000 claims abstract description 52
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 45
- 239000001301 oxygen Substances 0.000 claims abstract description 45
- 238000000746 purification Methods 0.000 claims abstract description 28
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002274 desiccant Substances 0.000 claims abstract description 23
- 238000005259 measurement Methods 0.000 claims abstract description 19
- 238000002485 combustion reaction Methods 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims abstract description 15
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 5
- 239000011707 mineral Substances 0.000 claims abstract description 5
- 239000003546 flue gas Substances 0.000 claims description 28
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 25
- 238000000354 decomposition reaction Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 239000000779 smoke Substances 0.000 claims description 15
- 239000000428 dust Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012494 Quartz wool Substances 0.000 claims description 6
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 claims description 4
- 238000004887 air purification Methods 0.000 claims description 4
- 230000003993 interaction Effects 0.000 claims description 4
- 239000002808 molecular sieve Substances 0.000 claims description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003814 drug Substances 0.000 abstract description 3
- 239000003245 coal Substances 0.000 description 19
- 239000004568 cement Substances 0.000 description 12
- 235000019738 Limestone Nutrition 0.000 description 10
- 239000006028 limestone Substances 0.000 description 10
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 238000010926 purge Methods 0.000 description 5
- 229920000742 Cotton Polymers 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000571 coke Substances 0.000 description 3
- 238000003869 coulometry Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to a device and a method for measuring total sulfur content in a solid sample, which comprises a controller, an oxygen supply device, a pyrolysis furnace, a gas purification device, an ultraviolet module, an electronic gas flow controller and an air pump, wherein the sulfur in the solid sample is converted into sulfur dioxide through high-temperature combustion, the sulfur dioxide content is detected by the ultraviolet module to reversely push the total sulfur content in the solid sample, and the ultraviolet module measures the SO2 content by adopting an ultraviolet differential absorption spectrum principle. The invention adopts an ultraviolet method for measurement, is slightly influenced by water vapor, only needs conventional anhydrous calcium chloride as a water vapor drying agent, has low use cost, and even can directly use a membrane dryer to replace the conventional medicine drying agent without replacing the drying agent; the ultraviolet module is a single-channel or double-channel range, so that the mineral measurement precision with low sulfur content is ensured.
Description
Technical Field
The invention mainly relates to a technology for measuring the total sulfur content in solid minerals such as coal, coke, iron ore, cement, limestone, steel and the like, in particular to a device and a method for measuring the total sulfur content in a solid sample.
Background
Sulfur is a harmful element. For coal, sulfur can cause great harm when the sulfur is used for combustion, gasification or coking. Sulfur in coal is converted into sulfur dioxide in the combustion process, so that the boiler is seriously corroded, and the atmosphere is seriously polluted; the coal gas is the most important link in coal chemical industry, and sulfur is converted into hydrogen sulfide in the coal gasification process, so that a catalyst is poisoned; for cement production, the over standard of sulfur content in cement directly causes unqualified cement quality; the cement production raw material limestone contains a small amount of sulfur, which can affect the burning of clinker, and cause the strength reduction of the clinker; the sulfur content in steel is more than 0.07%, hot brittleness is generated to reduce performance, and the quality of steel is directly influenced. Therefore, in order to make reasonable use of resources and control product quality, the total sulfur content in the solid sample must be detected.
For coal, according to the national standard GB/T214-2007 method for measuring total sulfur in coal, the total sulfur in coal can be determined by three methods, namely an Eschka method (gravimetric method), a coulometry method and an infrared method. The determination precision of the Eschka method is high, but the operation is complex and long, and the coulometry and the infrared method are generally adopted in industry. Although the coulomb method has short test time and simple operation, the electrolyte needs to be frequently replaced, the waste sample is used for finding the balance of the electrolytic cell to solve the overshoot problem, the failure rate is high, and the daily maintenance workload is large. The infrared sulfur detector is simple to operate and high in speed, but infrared is sensitive to water vapor, the water vapor is not thoroughly dried, and the determination precision is influenced, so that high-quality anhydrous magnesium perchlorate must be used as a flue gas drying agent, pure oxygen needs to be used, and the use cost of the infrared sulfur detector is very high.
For limestone and steel samples, the sulfur content is extremely low and is generally lower than 0.2%, a conventional coulomb sulfur meter and an infrared sulfur meter cannot measure the sulfur content, and the problems of large error and poor stability exist in the high-frequency infrared method commonly used in the steel industry.
Disclosure of Invention
The invention aims to provide a device and a method for measuring total sulfur content in a solid sample, aiming at solving the problems of the existing solid sample sulfur content measuring technology. The invention provides an ultraviolet sulfur detector, which converts sulfur in a sample into sulfur dioxide by adopting high-temperature combustion, and then detects the content of the sulfur dioxide by using an ultraviolet module to reversely deduce the total sulfur content in a solid sample.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a device for measuring the total sulfur content in a solid sample comprises a controller, an oxygen supply device, a pyrolysis furnace, a gas purification device, an ultraviolet module, an electronic gas flow controller and an air pump, wherein the oxygen supply device is connected with an air inlet of the pyrolysis furnace and is used for providing oxygen required by combustion decomposition of the sample; the high-temperature decomposing furnace provides required constant temperature for combustion and decomposition of the sample; the gas purification device is connected with a gas outlet of the pyrolysis furnace, and is used for filtering and drying flue gas generated by pyrolysis of a sample, and conveying the purified gas to the ultraviolet module for detection; the ultraviolet module is connected with the gas outlet of the gas purification device and used for detecting SO in the purified gas2The content of (A); and the gas outlet of the electronic gas flow controller is connected with the gas pump, and gas is pumped out by the gas pump.
Furthermore, the controller is a program control terminal, controls all components to operate and is used as a human-computer interaction platform.
Furthermore, the pyrolysis furnace comprises a sample feeding device, a furnace body, a heating device and a reducing pipe, wherein the sample feeding device is used for feeding a sample into the high-temperature area for decomposition, and the heating device and the reducing pipe are positioned inside the furnace body.
Preferably, the oxygen supply device is an oxygen generator, and the oxygen is separated from air by a molecular sieve to obtain high-purity and dry oxygen, or an oxygen bottle is used as the oxygen supply device to supply oxygen.
Further, the gas purification device comprises a filter and a dryer; quartz wool for filtering dust is filled in the filter; the dryer is a drying pipe or a membrane type gas dryer with the interior filled with a drying agent, or a drying system formed by connecting the membrane type gas dryer and the drying pipe with the interior filled with the drying agent.
Wherein, the desiccant is anhydrous calcium chloride or anhydrous magnesium perchlorate or other reagents capable of removing moisture.
As a preferred scheme, the ultraviolet module has a single-channel or double-channel range: the sample with high sulfur content is selected to be measured by a high-range channel SO as to ensure the SO to be measured2The instantaneous concentration value does not exceed the upper limit of measurement, and the sample with low sulfur content is measured by selecting a low-range channel so as to ensure the measurement accuracy of the mineral with low sulfur content.
The invention also discloses a method for measuring the total sulfur content in the solid sample, which adopts the device to measure, converts the sulfur in the solid sample into sulfur dioxide through high-temperature combustion, detects the sulfur dioxide content by using an ultraviolet module to reversely push the total sulfur content in the solid sample, and measures SO by using the ultraviolet module according to the ultraviolet differential absorption spectrum principle2And (4) content.
Which comprises the following steps:
1) when determining the total sulfur content in the solid sample, firstly, automatically opening an oxygen supply device, an electronic gas flow controller and an air pump by a controller, purging the whole gas circuit, and controlling the pyrolysis furnace to be heated to a set temperature;
2) after the pyrolysis furnace reaches the set temperature, putting a solid sample to be detected, and controlling a sample feeding device by a controller to feed the solid sample to be detected into the pyrolysis furnace for pyrolysis;
3) smoke generated by pyrolysis of a solid sample to be detected is pumped out by an air pump, the smoke firstly enters through an air inlet of an air purification device, dust is filtered by a filter filled with quartz cotton, and the smoke is dried by the air purification device;
4) the flue gas filtered and dried by the gas purification device is sent to an ultraviolet module for detection, and the ultraviolet module selects a measurement channel according to the components and the concentration of the flue gas to be detected;
5) the smoke measured by the ultraviolet module enters the electronic gas flow controller, the stability of the gas flow of the whole gas circuit is controlled, and the smoke is pumped out by the gas pump.
Wherein, the heating set temperature of the pyrolysis furnace is controlled according to the type of the solid sample; changing the selection type of the gas purification device according to the type of the solid sample; according to the kind of solid sample and the SO produced2And the concentration selects a measuring channel of the ultraviolet module.
The ultraviolet module in the invention adopts the ultraviolet differential absorption spectrum principle to measure SO2Content, ultraviolet band SO2The absorption section is a high-frequency component, and background gas and dust are scattered and absorbed to be a low-frequency component, so that the interference of dust, water vapor and background gas in the combustion flue gas to the spectrum of the gas to be detected is small. Because ultraviolet is little influenced by water vapor, only the conventional anhydrous calcium chloride is needed to be used as the water vapor drying agent, the use cost is low, a membrane type dryer can be used for replacing the conventional medicine drying agent, the drying agent does not need to be replaced, the trouble of frequently replacing the drying agent by workers is eliminated, and the use cost is also saved. The method has the advantages of no need of electrolyte, no need of high-quality drying agent, no need of pure oxygen, wide measurement range, and capability of thoroughly solving the problems of long time for determination by the Eschka method, large workload for maintenance by the coulometry method and high cost by the infrared method, and can be used for determination of the total sulfur content of solid samples such as coal, coke, limestone, steel and the like.
The invention provides an ultraviolet sulfur detector for a solid sample, which structurally comprises a controller, an oxygen supply device, a pyrolysis furnace, a gas purification device, an ultraviolet module, an electronic gas flow controller and an air pump. The controller is a program control terminal, controls all components to operate and is used as a human-computer interaction platform; the oxygen supply device is connected with the air inlet of the pyrolysis furnace and provides oxygen required by combustion and decomposition of the sample; the high-temperature decomposition furnace provides required constant temperature for combustion and decomposition of a sample, and comprises a sample feeding device, a furnace body, a heating device, a reducing pipe and the like, wherein the sample feeding device is used for feeding the sample into a high-temperature region for decomposition, and the heating device and the reducing pipe are positioned in the furnace body; the gas purification device is connected with the gas outlet of the pyrolysis furnaceFiltering and drying flue gas generated by pyrolysis of a sample, and conveying the purified gas to an ultraviolet module for detection; the gas outlet of the ultraviolet module gas purification device is connected and used for detecting SO in the purified gas2The content of (A); the air inlet of the electronic air flow controller is connected with the air outlet of the ultraviolet module and used for controlling the stability of the air flow of the air path, and the air outlet of the electronic air flow controller is connected with the air pump and is pumped out by the air pump.
Compared with the prior art, the invention has the beneficial effects that:
(1) the oxygen supply device is an oxygen generator, and the molecular sieve is used for separating air to obtain high-purity and dry oxygen to replace an oxygen bottle to supply the oxygen, so that the oxygen consumption cost is saved, and the trouble of frequently replacing the oxygen bottle is avoided.
(2) The gas purification device of the present invention includes a filter and a dryer. Quartz wool is filled in the filter to filter dust; the dryer can be a dryer tube filled with a drying agent for drying, or directly dried by a membrane gas dryer, or dried by the membrane gas dryer and then dried by the dryer tube. The invention adopts an ultraviolet method for measurement, is slightly influenced by water vapor, only needs the conventional anhydrous calcium chloride as a water vapor drying agent, and has low use cost; or the membrane dryer is used for replacing the conventional medicine desiccant, the desiccant does not need to be replaced, the trouble of frequently replacing the desiccant by workers is eliminated, and the use cost is further saved.
(3) The ultraviolet module in the invention is in single-channel or double-channel range. Selecting high-range channel measurement for samples with high sulfur content such as coal, coke, cement and the like to ensure SO to be measured2The instantaneous concentration value does not exceed the upper limit of measurement, so that the accuracy of measurement of the high-sulfur sample is ensured; and a low-range channel is selected for measuring solid samples such as limestone, steel and the like with low sulfur content, so that the measurement accuracy of the samples with low sulfur content is ensured.
Drawings
FIG. 1: the detection device of the invention is schematically structured.
In the figure: 1-a controller; 2-an oxygen supply apparatus; 3-a pyrolysis furnace; 4-a gas purification device; 5-an ultraviolet module; 6-electronic gas flow controller; 7-air pump.
Detailed Description
The foregoing aspects of the present invention are described in further detail below by way of examples, but it should not be construed that the scope of the subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above aspects of the present invention are within the scope of the present invention.
As shown in figure 1, the invention provides an ultraviolet sulfur detector, which structurally comprises a controller 1, an oxygen supply device 2, a pyrolysis furnace 3, a gas purification device 4, an ultraviolet module 5, an electronic gas flow controller 6 and a gas pump 7. The controller 1 is a program control terminal, controls all components to operate and is used as a human-computer interaction platform; the oxygen supply device 2 is connected with an air inlet of the high-temperature decomposition furnace 3 and provides oxygen required for combustion and decomposition of the sample; the high-temperature decomposition furnace 3 provides required constant temperature for combustion and decomposition of a sample, and comprises a sample feeding device, a furnace body, a heating device, a reducing pipe and the like, wherein the sample feeding device is used for feeding the sample into a high-temperature region for decomposition, and the heating device and the reducing pipe are positioned in the furnace body; the gas purification device 4 is connected with a gas outlet of the pyrolysis furnace 3, and is used for filtering and drying flue gas generated by pyrolysis of a sample, and conveying the purified gas to the ultraviolet module 5 for detection; the ultraviolet module 5 is connected with the gas outlet of the gas purification device 4 and is used for detecting SO in the purified gas2The content of (A); and the air inlet of the electronic gas flow controller 6 is connected with the air outlet of the ultraviolet module 5 and is used for controlling the stability of the gas flow of the gas circuit, and the air outlet of the electronic gas flow controller 6 is connected with the air pump 7 and is pumped out by the air pump 7.
The high-temperature decomposition furnace 3 comprises a sample feeding device, a furnace body, a heating device and a reducing pipe, wherein the sample feeding device is used for feeding a sample into a high-temperature area for decomposition, and the heating device and the reducing pipe are positioned inside the furnace body.
The oxygen supply device 2 is an oxygen generator that separates air by a molecular sieve to obtain high-purity and dry oxygen, or an oxygen cylinder is used as the oxygen supply device 2 to supply oxygen.
The gas purification device 4 includes a filter and a dryer; quartz wool for filtering dust is filled in the filter; the dryer is a drying pipe filled with a drying agent inside or a membrane type gas dryer, or is a drying system formed by connecting the membrane type gas dryer and the drying pipe filled with the drying agent inside.
Wherein, the desiccant is anhydrous calcium chloride or anhydrous magnesium perchlorate or other reagents capable of removing moisture.
The ultraviolet module is a single-channel or double-channel range: the sample with high sulfur content is selected to be measured by a high-range channel SO as to ensure the SO to be measured2The instantaneous concentration value does not exceed the upper limit of measurement, and the sample with low sulfur content is measured by selecting a low-range channel so as to ensure the measurement accuracy of the mineral with low sulfur content.
The invention provides a method for measuring total sulfur content in a solid sample, which adopts the device for measurement, converts sulfur in the solid sample into sulfur dioxide through high-temperature combustion, detects the sulfur dioxide content by using an ultraviolet module to reversely push the total sulfur content in the solid sample, and measures SO by using the ultraviolet module according to the ultraviolet differential absorption spectrum principle2And (4) content.
The specific embodiment is as follows:
example 1: when the device is used for measuring the total sulfur content of coal, the controller 1 automatically opens the oxygen supply device 2, the electronic gas flow controller 6 and the air pump 7 to purge the whole gas circuit and control the pyrolysis furnace 3 to heat to the set temperature 1150 ℃. After the pyrolysis furnace 3 reaches the set temperature, the coal sample is put in, and the controller 1 controls the sample feeding device to feed the coal sample into the pyrolysis furnace 3 for pyrolysis. Flue gas generated by coal sample pyrolysis is pumped out by an air pump 7, the flue gas firstly enters through an air inlet of a gas purification device 4, dust is filtered by a filter filled with quartz wool, the flue gas is dried by a membrane dryer and an internally filled anhydrous calcium chloride drying tube, the flue gas filtered and dried by the gas purification device 4 is sent into an ultraviolet module 5 for detection, the content of sulfur in coal is high, and the ultraviolet module 5 detects the sulfur in the flue gas according to SO in the flue gas2The concentration is automatically measured by selecting a wide-range channel, the smoke measured by the ultraviolet module 5 enters the electronic gas flow controller 6, the stability of the gas flow of the whole gas circuit is controlled, and finally the smoke is pumped out by the gas pump 7.
Example 2: for the measurement of the total sulfur content of limestone, it is necessary to increase the decomposition temperature since the sulfur in limestone is generally present in the form of sulfate. The controller 1 automatically turns on the oxygen supply device 2, the electronic gas flow controller 6 and the air pump 7 to purge the whole gas path, and controls the pyrolysis furnace 3 to be heated to the set temperature of 1200 ℃. After the pyrolysis furnace 3 reaches the set temperature, the iron ore sample is put in, and the controller 1 controls the sample feeding device to feed the limestone sample into the pyrolysis furnace 3 for pyrolysis. The flue gas that limestone sample pyrolysis produced is taken out by air pump 7, and the flue gas is at first got into through gas purification device 4 air inlet, is filtered the dust by the cotton filter of inside packing quartz, and dry through the membrane type desicator again, the flue gas after gas purification device 4 filters, the drying is sent into ultraviolet module 5 and is detected, and the sulphur content is lower in the limestone sample, and ultraviolet module 5 is according to SO in the flue gas2The concentration is automatically measured by selecting a low-range channel, the smoke measured by the ultraviolet module 5 enters the electronic gas flow controller 6, the stability of the gas flow of the whole gas circuit is controlled, and the smoke is finally pumped out by the gas pump 7.
Example 3: for SO in cement3In the content measurement, since sulfur is generally present in the form of sulfate in cement, it is necessary to increase the decomposition temperature. The controller 1 automatically turns on the oxygen supply device 2, the electronic gas flow controller 6 and the air pump 7 to purge the whole gas path, and controls the pyrolysis furnace 3 to be heated to the set temperature of 1200 ℃. After the pyrolysis furnace 3 reaches the set temperature, a cement sample is put in, and the controller 1 controls the sample feeding device to feed the cement sample into the pyrolysis furnace 3 for pyrolysis. The flue gas that the pyrolysis of cement appearance produced is taken out by air pump 7, and the flue gas is at first got into through 4 air inlets of gas purification device, filters the dust by the cotton filter of inside packing quartz, and dry through the membrane type desicator again, the flue gas after 4 filtration of gas purification device, drying is sent into ultraviolet module 5 and is detected, and sulfur content is higher in the cement appearance, and ultraviolet module 5 is according to SO in the flue gas2The concentration is automatically selected to be measured by a high-range channel, the smoke measured by the ultraviolet module 5 enters the electronic gas flow controller 6 to control the stability of the gas flow of the whole gas circuit, and finally the smoke passes through the gas pumpAnd 7, extracting.
Example 4: when the total sulfur content in coal is measured under the conditions that a catalyst is not used and an ultraviolet module is a single channel, the controller 1 automatically opens the oxygen supply device 2, the electronic gas flow controller 6 and the air pump 7 to purge the whole gas circuit and controls the pyrolysis furnace 3 to be heated to the set temperature of 1300 ℃. After the pyrolysis furnace 3 reaches the set temperature, the coal sample is put in, and the controller 1 controls the sample feeding device to feed the coal sample into the pyrolysis furnace 3 for pyrolysis. The flue gas that coal sample pyrolysis produced is taken out by air pump 7, the flue gas at first gets into through 4 air inlets of gaseous purifier, filter the dust by the cotton filter of inside packing quartz, it is dry with the anhydrous calcium chloride drying tube of inside packing to pass through the membrane type desicator again, filter through gaseous purifier 4, flue gas after the drying is sent into ultraviolet module 5 and is detected, flue gas after ultraviolet module 5 measures gets into electronic gas flow controller 6, control whole gas circuit gas flow's stability, take out via air pump 7 at last.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. The device for measuring the total sulfur content in the solid sample is characterized in that: the device comprises a controller (1), an oxygen supply device (2), a pyrolysis furnace (3), a gas purification device (4), an ultraviolet module (5), an electronic gas flow controller (6) and an air pump (7), wherein the oxygen supply device (2) is connected with an air inlet of the pyrolysis furnace (3) to provide oxygen required for combustion and decomposition of a sample, and the pyrolysis furnace (3) provides required constant temperature for combustion and decomposition of the sample; the gas purification device (4) is connected with a gas outlet of the pyrolysis furnace (3) and is used for filtering and drying flue gas generated by pyrolysis of a sample and conveying the purified gas to the ultraviolet module (5) for detection; the ultraviolet module (5) is connected with the gas outlet of the gas purification device (4)For detecting SO in the purified gas2The content of (A); the air inlet of the electronic gas flow controller (6) is connected with the air outlet of the ultraviolet module (5) and used for controlling the stability of the gas flow of the gas circuit, the air outlet of the electronic gas flow controller (6) is connected with the air pump (7), and gas is pumped out through the air pump (7).
2. The apparatus for determining the total sulfur content in a solid sample according to claim 1, wherein: the controller (1) is a program control terminal, controls all components to operate and is used as a human-computer interaction platform.
3. The apparatus for determining the total sulfur content in a solid sample according to claim 1, wherein: the high-temperature decomposition furnace (3) comprises a sample feeding device, a furnace body, a heating device and a reducing pipe, wherein the sample feeding device is used for feeding a sample into the high-temperature area for decomposition, and the heating device and the reducing pipe are positioned inside the furnace body.
4. The apparatus for determining the total sulfur content in a solid sample according to claim 1, wherein: the oxygen supply device (2) is an oxygen generator, and high-purity and dry oxygen is obtained by separating air by a molecular sieve, or an oxygen bottle is adopted as the oxygen supply device (2) to supply oxygen.
5. The apparatus for determining the total sulfur content in a solid sample according to claim 1, wherein: the gas purification device (4) comprises a filter and a dryer; quartz wool for filtering dust is filled in the filter; the dryer is a drying pipe or a membrane type gas dryer with the interior filled with a drying agent, or a drying system formed by connecting the membrane type gas dryer and the drying pipe with the interior filled with the drying agent.
6. The apparatus for measuring the total sulfur content in a solid sample according to claim 5, wherein: the drying agent is anhydrous calcium chloride or anhydrous magnesium perchlorate.
7. The apparatus for determining the total sulfur content in a solid sample according to claim 1, wherein: the ultraviolet module is a single-channel or double-channel range: the sample with high sulfur content is selected to be measured by a high-range channel SO as to ensure the SO to be measured2The instantaneous concentration value does not exceed the upper limit of measurement, and the sample with low sulfur content is measured by selecting a low-range channel so as to ensure the measurement accuracy of the mineral with low sulfur content.
8. A method for measuring the total sulfur content in a solid sample is characterized in that: the device of any one of claims 1 to 7 is used for measuring the total sulfur content in the solid sample by converting the sulfur in the solid sample into sulfur dioxide through high-temperature combustion and detecting the sulfur dioxide content by using an ultraviolet module, wherein the ultraviolet module measures SO by adopting an ultraviolet differential absorption spectrum principle2And (4) content.
9. The method for determining the total sulfur content in a solid sample according to claim 8, wherein: which comprises the following steps:
1) when determining the total sulfur content in the solid sample, firstly, the controller (1) automatically opens the oxygen supply device (2), the electronic gas flow controller (6) and the air pump (7), sweeps the whole gas circuit, and controls the pyrolysis furnace (3) to be heated to a set temperature;
2) after the pyrolysis furnace (3) reaches a set temperature, a solid sample to be detected is placed in the pyrolysis furnace, and the controller (1) controls the sample feeding device to feed the solid sample to be detected into the pyrolysis furnace (3) for pyrolysis;
3) smoke generated by pyrolysis of a solid sample to be detected is pumped out by an air pump (7), the smoke firstly enters through an air inlet of an air purification device (4), dust is filtered by a filter filled with quartz wool, and the smoke is dried by the air purification device;
4) the flue gas filtered and dried by the gas purification device (4) is sent to an ultraviolet module (5) for detection, and the ultraviolet module (5) selects a measurement channel according to the components and the concentration of the flue gas to be detected;
5) the smoke measured by the ultraviolet module (5) enters the electronic gas flow controller (6), controls the stability of the gas flow of the whole gas circuit, and is finally pumped out by the gas pump (7).
10. The method for determining the total sulfur content in a solid sample according to claim 9, wherein: wherein the heating set temperature of the pyrolysis furnace (3) is controlled according to the type of the solid sample; changing the selection type of the gas purification device according to the type of the solid sample; according to the kind of solid sample and the SO produced2A measuring channel of the concentration selection ultraviolet module (5).
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| CN202111274391.2A CN114018847A (en) | 2021-10-29 | 2021-10-29 | Device and method for measuring total sulfur content in solid sample |
| PCT/CN2022/121996 WO2023071678A1 (en) | 2021-10-29 | 2022-09-28 | Apparatus and method for determining total sulfur content in solid sample |
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| CN202111274391.2A CN114018847A (en) | 2021-10-29 | 2021-10-29 | Device and method for measuring total sulfur content in solid sample |
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| WO (1) | WO2023071678A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023071678A1 (en) * | 2021-10-29 | 2023-05-04 | 徐州泰瑞仪器设备有限公司 | Apparatus and method for determining total sulfur content in solid sample |
| CN116183812A (en) * | 2022-12-05 | 2023-05-30 | 上海金艺检测技术有限公司 | Full-automatic determination method for ferrous oxide content in steel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2009300203A (en) * | 2008-06-12 | 2009-12-24 | Mitsubishi Chemical Analytech Co Ltd | Sulfur analyzing method and sulfur analyzer |
| JP2010048582A (en) * | 2008-08-19 | 2010-03-04 | Mitsubishi Chemical Analytech Co Ltd | Sulfur analyzing method and sulfur analyzing apparatus |
| CN101806727B (en) * | 2010-03-02 | 2012-06-27 | 东南大学 | Method and device for measuring sulfur content in coal by ultraviolet absorption spectroscopy |
| CN107478624A (en) * | 2017-07-31 | 2017-12-15 | 武汉工程大学 | A kind of method of quartz ampoule carbon deposit in reduction UV suLfur anaLyzer |
| CN208313835U (en) * | 2018-07-11 | 2019-01-01 | 北京诺德泰科仪器仪表有限公司 | Air catalytic formula ultraviolet fluorescence method total sulfur content measurement device |
| CN114018847A (en) * | 2021-10-29 | 2022-02-08 | 徐州泰瑞仪器设备有限公司 | Device and method for measuring total sulfur content in solid sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023071678A1 (en) * | 2021-10-29 | 2023-05-04 | 徐州泰瑞仪器设备有限公司 | Apparatus and method for determining total sulfur content in solid sample |
| CN116183812A (en) * | 2022-12-05 | 2023-05-30 | 上海金艺检测技术有限公司 | Full-automatic determination method for ferrous oxide content in steel |
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