CN110095445B - Ultraviolet fluorescence total sulfur analyzer combustion tube - Google Patents
Ultraviolet fluorescence total sulfur analyzer combustion tube Download PDFInfo
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- CN110095445B CN110095445B CN201910403393.3A CN201910403393A CN110095445B CN 110095445 B CN110095445 B CN 110095445B CN 201910403393 A CN201910403393 A CN 201910403393A CN 110095445 B CN110095445 B CN 110095445B
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- G—PHYSICS
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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Abstract
The invention discloses a combustion tube of an ultraviolet fluorescence total sulfur analyzer, which is filled with the following components in sequence from bottom to top: (1) quartz wool with the height of 1-20 mm; (2) quartz liner tube with height of 30-80mm, inner diameter greater than 3mm, and outer diameter smaller than inner diameter of combustion tube, or quartz sand with height of 30-80 mm; (3) quartz wool with the height of 5-20 mm; (4) tungsten oxide with a height of 80-150 mm; (5) quartz wool with the height of 5-20 mm; (6) the height is 30-80mm, the inner diameter is larger than 3mm, and the outer diameter is smaller than the quartz liner tube of the inner diameter of the combustion tube; (7) quartz wool with a height of 1-20 mm. The combustion tube eliminates the influence of the traditional combustion tube on the test result when the long carbon chain and short carbon chain samples are alternately tested, and has high practical application value.
Description
Technical Field
The invention relates to an ultraviolet fluorescence total sulfur analyzer combustion tube, and belongs to the field of petrochemical product total sulfur detection.
Background
The sulfur content is an important detection index in the finished oil and the products thereof, and is also an index which must be strictly controlled in the petroleum products and the conversion exhaust gas thereof, and the online monitoring of the sulfur content has important significance for improving the petroleum processing process and the quality of the oil products. In the process of processing high-sulfur crude oil, a large amount of sulfur-containing waste water and waste gas are inevitably generated, and the emission amount and emission concentration of pollutants must be further reduced for improving the environment of a refinery. With the increasing attention on environmental protection, higher requirements are put forward on the content of sulfur elements in petrochemical products, and higher requirements are put forward on the lower limit measurement capability of corresponding detection methods.
The ultraviolet fluorescence total sulfur analyzer is mainly used for refineries and related petrochemical product production enterprises, is generally installed in laboratories or flow detection vehicles, and is a detection system for detecting the content of sulfur elements in collected samples.
The ultraviolet fluorescence total sulfur analyzer mainly analyzes samples and comprises the following components: blending gasoline and diesel; naphtha; kerosene; gas oil; natural gas and liquefied petroleum gas, etc.
The analyzer measures the compliance criteria:
american society for testing and materials standard: ASTM D5453 "Determination of Total Sulphur in Light Hydrocarbons, Motor Fuels and Oils by ultraviroet Fluorescence" uses UV Fluorescence to determine the Total Sulphur content in Light Hydrocarbons, power diesel and various Oils.
Second, the standard of petrochemical industry-arbitration analysis Method, SH/T0689 light hydrocarbon and total Sulfur content determination Method (ultraviolet fluorescence Method) of engine fuel and other oil products designed the UV as the Arbitrate Method for Sulfur Measurement.
State standard: GB/T17040-2008 oil and oil product sulfur content determination.
The existing ultraviolet fluorescence total sulfur testing method generally uses pure argon and pure oxygen as carrier gas and combustion-supporting gas, a reaction tube of the analyzer is not filled with a catalyst or a small amount of quartz wool, and the invention is not directed to an ultraviolet fluorescence total sulfur analyzer adopting the reaction tube form.
In the other method, clean air is used as carrier gas and combustion-supporting gas, but a reaction tube is filled with a catalyst which is usually granular tungsten oxide, quartz wool is filled at the upper end of the catalyst, namely the injection position of a sample injection needle, so as to help the sample to be fully gasified, and the sample injection needle injects the sample into the quartz wool. The present invention is directed to this form of ultraviolet fluorescence total sulfur analyzer.
The ultraviolet fluorescence total sulfur analyzer generally adopts an electric heating furnace to heat and keep the reaction tube at a certain temperature, and the characteristics of the electric heating furnace determine that the high-temperature area of the heating furnace is positioned at the central position of the heating furnace, the farther away from the central position, the lower the temperature of the heating furnace, and the filled quartz cotton is just positioned at the lower temperature area. When the sample is injected, the needle is in the quartz wool area, and the temperature is relatively low.
By adopting the filling mode, different types of samples are tested, and the fact that the samples with short carbon chains are analyzed after the samples with longer carbon chains are analyzed is found that the measured value of the samples with short carbon chains gradually rises and tends to be stable, and conversely, when the samples with short carbon chains (gasoline) are analyzed again, the measured value of the samples with longer carbon chains (diesel oil) gradually falls and tends to be stable. We analyzed this phenomenon because the catalyst tungsten oxide is in the central area of the furnace, the sample is unlikely to remain in the catalyst area, and the sample has been completely combusted through the catalyst to generate gas, and the sample is less likely to remain in the quartz wool at the outlet of the reaction tube, and most likely to remain in the quartz wool at the inlet of the reaction tube.
The diesel oil sample (sample with longer carbon chain) generates higher heat when burning than the gasoline sample (sample with shorter carbon chain), when the gasoline sample is analyzed again, a small amount of gasoline sample remains in the quartz cotton at the inlet, and the diesel oil sample generates higher heat when burning, which inevitably makes the quartz cotton area at the inlet have higher temperature, thereby gradually burning out the remaining gasoline sample, and from the analysis result, the result of the diesel oil sample is gradually reduced. And when the diesel oil sample is analyzed and the gasoline sample is analyzed, the gasoline sample is gradually adsorbed at the quartz cotton at the inlet and gradually reaches saturation, and the measurement result of the gasoline sample gradually rises and tends to be stable from the analysis result. There is no solution to this problem in the prior art.
Disclosure of Invention
In order to solve the problems in the prior art, the filling of the quartz tube is changed, in the first step, quartz cotton at the inlet end of the catalyst is completely removed, but the height of the catalyst is not increased, so that the needle head of the sample injection needle has a certain distance from the catalyst, a sample is analyzed, and the inlet of the reaction tube gradually becomes black under the condition, so that an obvious carbon deposition phenomenon is generated, and the test result is not ideal. In the second step, we tried to increase the filling of the catalyst tungsten oxide on the basis of the first step until the injection needle just touches the upper surface of the catalyst, and no fundamental improvement is found. The above two phenomena illustrate that the method for completely removing the quartz wool is not feasible. Thirdly, the tungsten oxide is arranged at a certain distance from the needle head of the sample injection needle, a layer of quartz cotton with the thickness of 5-20mm is filled on the existing catalyst, and the sample injection needle head is ensured not to contact the layer of quartz cotton; and placing a quartz tube with the outer diameter smaller than the inner diameter of the reaction tube on the quartz cotton, wherein the length of the quartz tube is between 30mm and 80mm, the inner diameter is larger than 3mm, a layer of quartz cotton is filled on the quartz tube, and the thickness of the layer of quartz cotton ensures that the needle head of the sample injection needle can penetrate through the layer of quartz cotton by more than 5 mm. The experiment shows that the effect is good.
On the basis of the research, the invention provides a combustion tube of an ultraviolet fluorescence total sulfur analyzer, which is internally filled with the following components in sequence from bottom to top:
(1) quartz wool with the height of 1-20 mm;
(2) quartz liner tube with height of 30-80mm, inner diameter greater than 3mm, and outer diameter smaller than inner diameter of combustion tube, or quartz sand with height of 30-80 mm;
(3) quartz wool with the height of 5-20 mm;
(4) tungsten oxide with a height of 80-150 mm;
(5) quartz wool with the height of 5-20 mm;
(6) the height is 30-80mm, the inner diameter is larger than 3mm, and the outer diameter is smaller than the quartz liner tube of the inner diameter of the combustion tube;
(7) quartz wool with a height of 1-20 mm.
Preferably, the height of the quartz liner tube in (6) should ensure that the sample injection needle can penetrate through the quartz wool at the upper end of the quartz liner tube by more than 1mm, and the inner diameter of the quartz liner tube should be greater than 3mm, so as to ensure that the sample injection needle can penetrate through the quartz wool and be inserted into the quartz liner tube without being blocked by the upper end surface of the quartz liner tube to bend the sample injection needle.
If the inner diameter of the quartz liner tube is large and cannot support the quartz wool at the upper end of the quartz liner tube, preferably, the quartz liner tube in (6) further comprises a quartz ring piece which is arranged at the top of the quartz liner tube and has a thickness of 3-10mm and is used for supporting the quartz wool at the upper end of the quartz liner tube, so that the problem that the quartz wool at the upper end of the quartz liner tube cannot be supported due to the large inner diameter of the quartz liner tube or the quartz wool enters the quartz liner tube, so that the sample injection needle cannot penetrate through the quartz wool is solved.
Preferably, the interior of the combustion tube is filled from bottom to top in sequence:
(1) quartz wool with the height of 15 mm;
(2) a quartz liner tube with the height of 65mm, the inner diameter of 8mm and the outer diameter of 22mm, or quartz sand with the height of 65 mm;
(3) quartz wool with the height of 20 mm;
(4) tungsten oxide having a height of 140 mm;
(5) quartz wool with the height of 15 mm;
(6) the height is 65mm, the inner diameter is 8mm, and the outer diameter is smaller than the quartz liner tube of the inner diameter of the combustion tube;
(7) quartz wool 5mm in height.
According to the filling mode of the invention, the sample injection needle can penetrate through the quartz wool to inject the sample into the liner tube, the liner tube provides enough gasification space for the sample, oxygen in tungsten oxide and oxygen in air provide an oxygen-rich environment for sample combustion, and sulfur in the sample is converted into sulfur dioxide after being sufficiently oxidized.
Compared with the prior art, the invention has the beneficial effects that:
1. when the sample injection needle is used for injecting a sample, the sample injection needle directly injects the sample into the liner tube without contacting with the quartz cotton, so that the residue of the sample in the quartz cotton is greatly reduced, and the interference of the firstly-measured sample on the secondly-measured sample is eliminated.
2. The hollow quartz liner tube is used for replacing quartz cotton, so that the gasification space of the sample is enlarged, the sample is gasified more sufficiently, and the reaction for converting sulfur element into sulfur dioxide is more sufficient.
3. The use amount of the quartz wool is reduced, and the risk of bringing impurities can be reduced.
4. The combustion tube eliminates the influence of the traditional combustion tube on the test result when the long carbon chain and short carbon chain samples are alternately tested, and has high practical application value.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1
In this embodiment, a burner tube with a length of 340mm and an inner diameter of 24mm is taken as an example, and the filling is performed from bottom to top in the following order:
(1)15mm quartz wool;
(2) a quartz liner tube with the length of 65mm, the inner diameter of 8mm and the outer diameter of 22 mm;
(3)20mm quartz wool;
(4)140mm of tungsten oxide;
(5)15mm quartz wool;
(6) a quartz liner tube with the length of 65mm, the inner diameter of 8mm and the outer diameter of 22 mm;
(7)5mm quartz wool.
Example 2
In this embodiment, a combustion tube with a length of 160mm and an inner diameter of 6mm is taken as an example, and the filling is performed from bottom to top in the following order:
(1)5mm quartz wool;
(2) a quartz liner tube with the length of 30mm, the inner diameter of 3.5mm and the outer diameter of 4 mm;
(3)5mm quartz wool;
(4)80mm of tungsten oxide;
(5)5mm quartz wool;
(6) a quartz liner tube with the length of 30mm, the inner diameter of 3.5mm and the outer diameter of 4 mm;
(7)1mm of quartz wool.
Example 3
In this embodiment, a burner tube with a length of 340mm and an inner diameter of 24mm is taken as an example, and the filling is performed from bottom to top in the following order:
(1)15mm quartz wool;
(2)65mm of quartz sand;
(3)20mm quartz wool;
(4)140mm of tungsten oxide;
(5)5mm quartz wool;
(6) a quartz liner tube with the length of 60mm, the inner diameter of 8mm and the outer diameter of 22 mm;
(7)5mm quartz wool.
Example 4
In this embodiment, a combustion tube with a length of 400mm and an inner diameter of 10mm is taken as an example, and the filling is performed from bottom to top in the following order:
(1)20mm quartz wool;
(2)80mm quartz sand;
(3)20mm quartz wool;
(4) tungsten oxide of 150 mm;
(5)20mm quartz wool;
(6) the quartz liner tube is 80mm long, 8mm in inner diameter and 9mm in outer diameter, and a 7mm thick quartz ring piece is placed at the top of the quartz liner tube;
(7)20mm quartz wool.
Experimental example 1
The test is carried out by using a combustion tube in a traditional filling mode and an ultraviolet fluorescence total sulfur analyzer, the temperature of a heating furnace is 1075 ℃, clean compressed air is used as carrier gas and combustion-supporting gas, the pressure of the carrier gas is about 200Kpa, the flow rate is 420ml/min, and the experimental results are shown in table 1. It can be seen that when gasoline and diesel samples are alternately tested, the test results of the samples are far from ideal, and show a trend of increasing or decreasing in sequence.
TABLE 1 results of alternate gasoline and diesel samples
| Sample name | Sample volume | Integral area | Sample content |
| Diesel oil 1 | 20 microliter | 18789 | 8.03 |
| Diesel oil 1 | 20 microliter | 19558 | 8.36 |
| Diesel oil 1 | 20 microliter | 19409 | 8.3 |
| Diesel oil 1 | 20 microliter | 19563 | 8.36 |
| Gasoline 1 | 20 microliter | 2198 | 0.88 |
| Gasoline 1 | 20 microliter | 2905 | 1.19 |
| Gasoline 1 | 20 microliter | 3621 | 1.5 |
| Gasoline 1 | 20 microliter | 5117 | 2.14 |
| Diesel oil 2 | 20 microliter | 23552 | 10.1 |
| Diesel oil 2 | 20 microliter | 20193 | 8.63 |
| Diesel oil 2 | 20 microliter | 18481 | 7.9 |
| Diesel oil 2 | 20 microliter | 17951 | 7.67 |
| Gasoline 2 | 20 microliter | 2156 | 0.86 |
| Gasoline 2 | 20 microliter | 2977 | 1.22 |
| Gasoline 2 | 20 microliter | 3266 | 1.34 |
| Gasoline 2 | 20 microliter | 3821 | 1.58 |
| Diesel oil 3 | 20 microliter | 29311 | 12.9 |
| Diesel oil 3 | 20 microliter | 22616 | 9.68 |
| Diesel oil 3 | 20 microliter | 19915 | 8.51 |
| Diesel oil 3 | 20 microliter | 16940 | 7.23 |
| Gasoline 3 | 20 microliter | 1975 | 0.79 |
| Gasoline 3 | 20 microliter | 2373 | 0.96 |
| Gasoline 3 | 20 microliter | 2968 | 1.21 |
| Gasoline 3 | 20 microliter | 3369 | 1.39 |
Experimental example 2
The combustion tube of the embodiment 1 of the invention is used, an ultraviolet fluorescence total sulfur analyzer is used for testing, the temperature of a heating furnace is 1075 ℃, clean compressed air is used as carrier gas and combustion-supporting gas, the pressure of the carrier gas is about 200Kpa, and the flow rate is 420 ml/min. The results of the experiment are shown in Table 2. As can be seen from the data, the ideal calibration curve can be obtained from 1mg/L to 300mg/L, and the alternate testing of the gasoline and diesel oil samples from Table 3 can obtain very stable testing results. Therefore, the filling mode of the combustion tube eliminates the influence of samples when the combustion tube is subjected to the gasoline and diesel alternating test according to the traditional filling mode.
TABLE 2 test results of the Standard samples
TABLE 3 alternate gasoline and diesel samples test results
Experimental example 3
Another batch of gasoline and diesel oil samples were replaced with the combustion tube of the invention in example 2, and the test was performed with an ultraviolet fluorescence total sulfur analyzer, the heating furnace temperature was 1075 ℃, the clean compressed air was used as carrier gas and combustion-supporting gas, the carrier gas pressure was about 200Kpa, the flow rate was 420ml/min, and the experimental results are shown in table 4. From the data, it can be seen that the alternate testing of the gasoline and diesel samples can obtain very stable test results.
TABLE 4 alternate gasoline and diesel samples test results
Claims (4)
1. The utility model provides a total sulphur analysis appearance burner of ultraviolet fluorescence which characterized in that, the inside from bottom to top of burner fills in proper order:
(1) quartz wool with the height of 1-20 mm;
(2) quartz liner tube with height of 30-80mm, inner diameter greater than 3mm, and outer diameter smaller than inner diameter of combustion tube, or quartz sand with height of 30-80 mm;
(3) quartz wool with the height of 5-20 mm;
(4) tungsten oxide with a height of 80-150 mm;
(5) quartz wool with the height of 5-20 mm;
(6) the height is 30-80mm, the inner diameter is larger than 3mm, and the outer diameter is smaller than the quartz liner tube of the inner diameter of the combustion tube;
(7) quartz wool with a height of 1-20 mm.
2. The burner tube of claim 1, wherein the quartz liner tube in (6) has a height ensuring that the injection needle can penetrate the quartz wool at the upper end thereof by more than 1mm, and an inner diameter greater than 3mm ensuring that the injection needle can be inserted into the quartz liner tube through the quartz wool without being blocked by the upper end surface of the quartz liner tube to bend the injection needle.
3. The burner of claim 1, wherein in (6) said quartz liner tube further comprises a quartz plate with a thickness of 3-10mm placed on top of said quartz liner tube for supporting the quartz wool on the upper end thereof.
4. The burner tube of claim 1, wherein the inside of the burner tube is filled in sequence from bottom to top:
(1) quartz wool with the height of 15 mm;
(2) a quartz liner tube with the height of 65mm, the inner diameter of more than 3mm and the outer diameter of less than the inner diameter of the combustion tube, or quartz sand with the height of 65 mm;
(3) quartz wool with the height of 20 mm;
(4) tungsten oxide having a height of 140 mm;
(5) quartz wool with the height of 15 mm;
(6) the height is 65mm, the inner diameter is more than 3mm, and the outer diameter is less than the quartz liner tube of the inner diameter of the combustion tube;
(7) quartz wool 5mm in height.
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Citations (8)
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| JPS51138496A (en) * | 1975-05-26 | 1976-11-30 | Japan Spectroscopic Co | Device for measuring carbon of entire organic substance |
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| JP3831671B2 (en) * | 2002-02-19 | 2006-10-11 | 株式会社堀場製作所 | Method and apparatus for injecting liquid sample into horizontal combustion tube |
| CN101241077A (en) * | 2008-03-14 | 2008-08-13 | 朱明俊 | Pulse type ultraluminescence method sulphur -measuring dedicated quartz tube |
| CN104678047A (en) * | 2015-03-18 | 2015-06-03 | 中国科学院上海应用物理研究所 | Organic tritium oxidation combustion tube and organic tritium oxidation combustion method |
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| CA2726889C (en) * | 2011-01-06 | 2018-11-13 | General Electric Company | Catalyst and method of manufacture |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51138496A (en) * | 1975-05-26 | 1976-11-30 | Japan Spectroscopic Co | Device for measuring carbon of entire organic substance |
| FR2599846A1 (en) * | 1986-06-05 | 1987-12-11 | Elf France | SULFUR ANALYSIS SYSTEM IN LIQUID HYDROCARBONS |
| JP3831671B2 (en) * | 2002-02-19 | 2006-10-11 | 株式会社堀場製作所 | Method and apparatus for injecting liquid sample into horizontal combustion tube |
| CN101241077A (en) * | 2008-03-14 | 2008-08-13 | 朱明俊 | Pulse type ultraluminescence method sulphur -measuring dedicated quartz tube |
| CA2726889C (en) * | 2011-01-06 | 2018-11-13 | General Electric Company | Catalyst and method of manufacture |
| JP5877540B2 (en) * | 2012-03-28 | 2016-03-08 | 京都電子工業株式会社 | Mercury concentration measuring device and pretreatment device |
| JP2015184065A (en) * | 2014-03-20 | 2015-10-22 | 国立研究開発法人産業技術総合研究所 | Method for analysing single-wall carbon nanotube in biological specimen, and analyzer used for method |
| CN104678047A (en) * | 2015-03-18 | 2015-06-03 | 中国科学院上海应用物理研究所 | Organic tritium oxidation combustion tube and organic tritium oxidation combustion method |
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| CHN模式下EA1110元素分析仪反应管填充及制样方法的改进;吴冰 等;《苏州大学学报（自然科学版）》;20100731;第87-90页 * |
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