CN110095445A - A kind of Ultraluminescence analysis of total sulfur instrument combustion tube - Google Patents
A kind of Ultraluminescence analysis of total sulfur instrument combustion tube Download PDFInfo
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- CN110095445A CN110095445A CN201910403393.3A CN201910403393A CN110095445A CN 110095445 A CN110095445 A CN 110095445A CN 201910403393 A CN201910403393 A CN 201910403393A CN 110095445 A CN110095445 A CN 110095445A
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- silica wool
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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
- G01N21/01—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
Abstract
The invention discloses a kind of Ultraluminescence analysis of total sulfur instrument combustion tube, inside be sequentially filled from bottom to top: (1) be highly the silica wool of 1-20mm；It (2) is highly 30-80mm, internal diameter is greater than 3mm, and outer diameter is less than the quartz liner of burning bore, or height is the quartz sand of 30-80mm；It (3) is highly the silica wool of 5-20mm；It (4) is highly the tungsten oxide of 80-150mm；It (5) is highly the silica wool of 5-20mm；It (6) is highly 30-80mm, internal diameter is greater than 3mm, and outer diameter is less than the quartz liner of burning bore；It (7) is highly the silica wool of 1-20mm.Combustion tube of the invention eliminates influence of the traditional combustion pipe when carrying out Long carbon chain and short carbon chain sample alternately testing for test result, is of very high actual application value.
Description
Technical field
The present invention relates to a kind of Ultraluminescence analysis of total sulfur instrument combustion tubes, belong to petroleum chemicals total sulfur detection field.
Background technique
Sulfur content is an important Testing index and oil product and its conversion discharge gas in product oil and products thereof
The index that must be strictly controlled in body, sulfur content on-line monitoring all have weight to petroleum refining process and raising oil quality is improved
Want meaning.During high sulfur bauxite, a large amount of sulfur-containing waste waters, exhaust gas are inevitably resulted from, refinery is to improve environment,
The discharge amount and concentration of emission of pollutant must be further reduced.It is right with the growing attention to environmental protection of people
More stringent requirements are proposed for sulfur content in petrochemicals, the measurement lower limit ability to its corresponding method of detection it is also proposed that
Higher requirement.
Ultraluminescence analysis of total sulfur instrument is mainly used for refinery and related petroleum chemicals manufacturing enterprise, is generally mounted to laboratory
Or moving testing vehicle, for examining the detection system of sulfur content in acquisition sample.
Ultraluminescence analysis of total sulfur instrument Main Analysis sample includes: reconciliation vapour, diesel oil；Naphtha；Kerosene；Gas oil；It
Right gas and oil liquefied gas etc..
The standard that analyzer measurement meets:
1. American society of test material standards: ASTM D5453 " Determination of Total Sulphur in
Light Hydrocarbons, Motor Fuels and Oils by Ultraviolet Fluorescence " use ultraviolet
Fluorescence method determines the total sulfur content in lighter hydrocarbons, power diesel oil and various oils.
2. petrochemical industry standard --- arbitration analysis method: 0689 light hydrocarbon of SH/T and engine fuel and other oil products
Total sulfur content measuring method (ultraviolet fluorescence method) Designated the UV as the Arbitrate Method for
Sulfur Measurement。
3. national standard: 17,040 1 2008 petroleum of GB/T and oil product sulphur content determination.
Ultraluminescence total sulfur test method is usually using pure argon and purity oxygen as carrier gas and combustion-supporting gas, this type at present
The analyzer reaction tube of type is usually not filled with catalyst or fills a small amount of silica wool, and the present invention is not directed to using this reaction tube
The Ultraluminescence analysis of total sulfur instrument of form.
Use pure air as carrier gas and combustion-supporting gas there are also a kind of, but its reaction tube domestic demand catalyst filling, catalyst
Granular tungsten oxide is generallyd use, and is stuffed entirely with silica wool in the upper end of catalyst, that is, sample introduction needle injection position and is used to help
Sample sufficiently gasifies, and sample introduction needle injects a sample into silica wool.The present invention be directed to the Ultraluminescence of this form is total
Sulphur content analyzer.
Ultraluminescence analysis of total sulfur instrument generallys use electric furnace and heats and keeps reaction tube in certain temperature, and electric heating
The characteristic of furnace determines that heating furnace high-temperature region is located at heating furnace center, and remoter away from center, temperature is lower, filling
Silica wool be just in the lower region of temperature.When sample introduction, syringe needle is in silica wool region, and temperature herein is relatively
It is low.
Using such filling mode, different types of sample is tested, it has been found that just having analyzed, carbochain is longer
Sample after analyze the short sample of carbochain again, the measured value of the short sample of carbochain can gradually rise and tend towards stability, on the contrary when point
It has analysed the short sample of carbochain (gasoline) and has analyzed the longer sample of carbochain (diesel oil) again, measured value can be gradually decreased and be tended towards stability.
We are analyzed for this phenomenon, because catalyst tungsten oxide is in heating furnace central area, sample is almost impossible
Catalyst area can be remained in, and sample passes through catalyst completely burned generation gas, sample carryover is exported in reaction tube
A possibility that locating silica wool very little, maximum may be to remain in the silica wool of reaction tube entrance.
The heat that diesel samples (the longer sample of carbochain) generate when burning than gasoline sample (the shorter sample of carbochain) is more
Height has remained a small amount of gasoline sample in the silica wool of entrance when analyzing gasoline sample and analyzing diesel samples again, and diesel oil
Higher heat is generated when sample combustion, this will make the silica wool regional temperature of entrance higher, thus by remaining gasoline
Sample, which gradually burns, to be come out, and is exactly that the results of diesel samples gradually decreases from analysis result.And works as and analyzed diesel samples
When analyzing gasoline sample again, gasoline sample can be gradually adsorbed at the silica wool of entrance again, and progressively reach saturation, from point
It is seen in analysis result, the measurement result of gasoline sample can gradually rise and tend towards stability.The problem is not deposited temporarily in the prior art
In any solution.
Summary of the invention
In order to solve the problems in the prior art, we change the filling of quartz ampoule, the first step, we are completely
The silica wool at catalyst inlet end is eliminated, but the height of catalyst does not increase, such sample introduction needle syringe needle has apart from catalyst
A certain distance analyzes sample, discovery in this case reaction tube inlet can gradually blackening, generate apparent carbon distribution
Phenomenon, test result are also undesirable.Second step, we attempt to increase the filling of catalyst tungsten oxide on the basis of the first step,
Until sample introduction needle still finds no basic change i.e. into contact with catalyst upper surface.Both the above phenomenon explanation completely removes
The method of silica wool is unworkable.Third step, we still make tungsten oxide and sample introduction needle syringe needle has certain distance, first present catalyst
The silica wool of one layer of 5-20mm of upper filling, and ensure that sample introduction syringe needle is not exposed to this layer of silica wool；It is put on silica wool outside one
Diameter is less than the quartz ampoule of tube inner diameter, this root quartz length of tube is between 30mm-80mm, and internal diameter should be greater than 3mm, it is ensured that sample introduction
Needle can enter this quartz ampoule, one layer of silica wool be refilled above quartz ampoule, the thickness of this layer of silica wool is it is ensured that sample introduction needle syringe needle
This layer of silica wool 5mm or more can be pierced through.Experiment discovery effect is fine.
On the basis of the studies above, the present invention provides a kind of Ultraluminescence analysis of total sulfur instrument combustion tube, inside from
It is sequentially filled upwards down:
It (1) is highly the silica wool of 1-20mm；
It (2) is highly 30-80mm, internal diameter is greater than 3mm, and outer diameter is less than the quartz liner of burning bore, or height is 30-
The quartz sand of 80mm；
It (3) is highly the silica wool of 5-20mm；
It (4) is highly the tungsten oxide of 80-150mm；
It (5) is highly the silica wool of 5-20mm；
It (6) is highly 30-80mm, internal diameter is greater than 3mm, and outer diameter is less than the quartz liner of burning bore；
It (7) is highly the silica wool of 1-20mm.
Preferably, the height of quartz liner described in (6) be it is ensured that sample introduction needle can penetrate the upper end silica wool 1mm or more,
The internal diameter of the quartz liner should be greater than 3mm, it is ensured that sample introduction needle can pass through silica wool insertion quartz liner without by quartz liner
Upper surface stops to be bent sample introduction needle.
The silica wool of the upper end cannot be supported if quartz liner internal diameter is big, it is preferred that (6) in quartz liner described in
Further include one be placed at the top of the quartz liner and thickness 3-10mm quartzy circular ring plate, for supporting the upper end silica wool,
To solve the silica wool of the upper end or silica wool cannot to be supported to enter the quartz liner because the internal diameter of quartz liner is too big
In, thus the problem of making sample introduction needle cannot pass through silica wool.
Preferably, it is sequentially filled from bottom to top inside the combustion tube:
It (1) is highly the silica wool of 15mm；
It (2) is highly long 65mm, internal diameter 8mm, outer diameter is the quartz liner of 22mm, or height is the quartz sand of 65mm；
It (3) is highly the silica wool of 20mm；
It (4) is highly the tungsten oxide of 140mm；
It (5) is highly the silica wool of 15mm；
It (6) is highly 65mm, internal diameter 8mm, quartz liner of the outer diameter less than burning bore；
It (7) is highly the silica wool of 5mm.
Filling mode according to the invention, sample introduction needle can pass through silica wool, and by sample injection to bushing pipe, bushing pipe is sample
Product provide enough gasification spaces, and the oxygen in oxygen and air in tungsten oxide provides an oxygen-enriched environment, sample for sample combustion
Element sulphur in product is converted to sulfur dioxide after being substantially oxidized.
Compared to the prior art, the beneficial effects of the present invention are:
1. when sample introduction needle sample introduction, sample introduction needle by sample injection to bushing pipe, does not contact directly with silica wool, sample is substantially reduced
Residual of the product in silica wool eliminates interference of the first sample to rear sample.
2. replacing silica wool with hollow quartz liner, increase the gasification space of sample, keeps sample gasification more abundant, thus
The reaction for making element sulphur be converted into sulfur dioxide is more abundant.
3. reducing the usage amount of silica wool, the risk for bringing impurity into can be reduced.
4. combustion tube of the invention eliminates traditional combustion pipe and is carrying out Long carbon chain and when short carbon chain sample alternately testing pair
In the influence of test result, it is of very high actual application value.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and
It is apparent.But examples are merely exemplary for these, and it is not intended to limit the scope of the present invention in any way.Those skilled in the art
Member it should be understood that without departing from the spirit and scope of the invention can details to technical solution of the present invention and form into
Row modifications or substitutions, but these modifications and replacement are fallen within the protection scope of the present invention.
Embodiment 1
The present embodiment by taking length is 340mm, internal diameter is the combustion tube of 24mm as an example, from bottom to top successively by it is following illustrate into
Row filling:
(1) silica wool of 15mm；
(2) long 65mm, internal diameter 8mm, the quartz liner of outer diameter 22mm；
(3) silica wool of 20mm；
(4) tungsten oxide of 140mm；
(5) silica wool of 15mm；
(6) long 65mm, internal diameter 8mm, the quartz liner of outer diameter 22mm；
(7) silica wool of 5mm.
Embodiment 2
The present embodiment by taking length is 160mm, internal diameter is the combustion tube of 6mm as an example, from bottom to top successively by it is following illustrate into
Row filling:
(1) silica wool of 5mm；
(2) long 30mm, internal diameter 3.5mm, the quartz liner of outer diameter 4mm；
(3) silica wool of 5mm；
(4) tungsten oxide of 80mm；
(5) silica wool of 5mm；
(6) long 30mm, internal diameter 3.5mm, the quartz liner of outer diameter 4mm；
(7) silica wool of 1mm.
Embodiment 3
The present embodiment by taking length is 340mm, internal diameter is the combustion tube of 24mm as an example, from bottom to top successively by it is following illustrate into
Row filling:
(1) silica wool of 15mm；
(2) quartz sand of 65mm；
(3) silica wool of 20mm；
(4) tungsten oxide of 140mm；
(5) silica wool of 5mm；
(6) long 60mm, internal diameter 8mm, the quartz liner of outer diameter 22mm；
(7) silica wool of 5mm.
Embodiment 4
The present embodiment by taking length is 400mm, internal diameter is the combustion tube of 10mm as an example, from bottom to top successively by it is following illustrate into
Row filling:
(1) silica wool of 20mm；
(2) quartz sand of 80mm；
(3) silica wool of 20mm；
(4) tungsten oxide of 150mm；
(5) silica wool of 20mm；
(6) the quartzy circular ring plate of thickness 7mm is placed at long 80mm, internal diameter 8mm, the quartz liner of outer diameter 9mm, top；
(7) silica wool of 20mm.
Experimental example 1
Using the combustion tube of conventional filling procedures, tested using Ultraluminescence analysis of total sulfur instrument, furnace temp is
1075 DEG C, clean compressed air is carrier gas and combustion-supporting gas, and nebulizer gas pressure is 200Kpa or so, flow velocity 420ml/min, experiment knot
Fruit is referring to table 1.As can be seen that sample tests are very unsatisfactory, show and successively increase when petrol and diesel oil sample alternately testing
Or reduced trend.
1 gasoline of table and diesel samples alternately testing result
| Sample ID | Sample volume | Integral area | Sample size |
| Diesel oil 1 | 20 microlitres | 18789 | 8.03 |
| Diesel oil 1 | 20 microlitres | 19558 | 8.36 |
| Diesel oil 1 | 20 microlitres | 19409 | 8.3 |
| Diesel oil 1 | 20 microlitres | 19563 | 8.36 |
| Gasoline 1 | 20 microlitres | 2198 | 0.88 |
| Gasoline 1 | 20 microlitres | 2905 | 1.19 |
| Gasoline 1 | 20 microlitres | 3621 | 1.5 |
| Gasoline 1 | 20 microlitres | 5117 | 2.14 |
| Diesel oil 2 | 20 microlitres | 23552 | 10.1 |
| Diesel oil 2 | 20 microlitres | 20193 | 8.63 |
| Diesel oil 2 | 20 microlitres | 18481 | 7.9 |
| Diesel oil 2 | 20 microlitres | 17951 | 7.67 |
| Gasoline 2 | 20 microlitres | 2156 | 0.86 |
| Gasoline 2 | 20 microlitres | 2977 | 1.22 |
| Gasoline 2 | 20 microlitres | 3266 | 1.34 |
| Gasoline 2 | 20 microlitres | 3821 | 1.58 |
| Diesel oil 3 | 20 microlitres | 29311 | 12.9 |
| Diesel oil 3 | 20 microlitres | 22616 | 9.68 |
| Diesel oil 3 | 20 microlitres | 19915 | 8.51 |
| Diesel oil 3 | 20 microlitres | 16940 | 7.23 |
| Gasoline 3 | 20 microlitres | 1975 | 0.79 |
| Gasoline 3 | 20 microlitres | 2373 | 0.96 |
| Gasoline 3 | 20 microlitres | 2968 | 1.21 |
| Gasoline 3 | 20 microlitres | 3369 | 1.39 |
Experimental example 2
Using the combustion tube of the embodiment of the present invention 1, tested using Ultraluminescence analysis of total sulfur instrument, furnace temp is
1075 DEG C, clean compressed air is carrier gas and combustion-supporting gas, and nebulizer gas pressure is 200Kpa or so, flow velocity 420ml/min.Experiment knot
Fruit is referring to table 2.It can be seen that from data, can get ideal calibration curve from 1mg/L to 300mg/L, handed over from 3 petrol and diesel oil sample of table
Very steadily test result can be obtained for test.As it can be seen that the filling mode of combustion tube of the present invention is eliminated by conventional filling procedures
Combustion tube carry out petrol and diesel oil alternately testing when sample room influence.
2 standard sample test result of table
3 gasoline of table and diesel samples alternately testing result
Experimental example 3
Using the combustion tube of the embodiment of the present invention 2, another batch of gasoline and diesel samples are replaced, the total sulphur content of Ultraluminescence is used
Analyzer is tested, and furnace temp is 1075 DEG C, and clean compressed air is carrier gas and combustion-supporting gas, and nebulizer gas pressure is 200Kpa left
The right side, flow velocity 420ml/min, experimental result is referring to table 4.It is very stable to can be seen that petrol and diesel oil sample alternately testing can obtain from data
Ground test result.
4 gasoline of table and diesel samples alternately testing result
Claims (4)
1. a kind of Ultraluminescence analysis of total sulfur instrument combustion tube, which is characterized in that be sequentially filled from bottom to top inside the combustion tube:
It (1) is highly the silica wool of 1-20mm；
It (2) is highly 30-80mm, internal diameter is greater than 3mm, and outer diameter is less than the quartz liner of burning bore, or height is 30-80mm
Quartz sand；
It (3) is highly the silica wool of 5-20mm；
It (4) is highly the tungsten oxide of 80-150mm；
It (5) is highly the silica wool of 5-20mm；
It (6) is highly 30-80mm, internal diameter is greater than 3mm, and outer diameter is less than the quartz liner of burning bore；
It (7) is highly the silica wool of 1-20mm.
2. combustion tube according to claim 1, which is characterized in that (6) height of quartz liner described in is it is ensured that sample introduction
Needle can penetrate the upper end silica wool 1mm or more, and the internal diameter of the quartz liner should be greater than 3mm, it is ensured that sample introduction needle can pass through quartz
Cotton, which is inserted into quartz liner, is bent sample introduction needle without being stopped by quartz liner upper surface.
3. combustion tube according to claim 1, which is characterized in that (6) further include one being placed in institute in quartz liner described in
State at the top of quartz liner and thickness 3-10mm quartz plate, for supporting the upper end silica wool.
4. combustion tube according to claim 1, which is characterized in that be sequentially filled from bottom to top inside the combustion tube:
(1) silica wool of 15mm；
(2) long 65mm, internal diameter are greater than 3mm, and outer diameter is less than the quartz liner of burning bore or the quartz sand of 65mm；
(3) silica wool of 20mm；
(4) tungsten oxide of 140mm；
(5) silica wool of 15mm；
(6) long 65mm, internal diameter are greater than 3mm, and outer diameter is less than the quartz liner of burning bore；
(7) silica wool of 5mm.
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| CN201910403393.3A CN110095445B (en) | 2019-05-15 | 2019-05-15 | Ultraviolet fluorescence total sulfur analyzer combustion tube |
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| CN201910403393.3A CN110095445B (en) | 2019-05-15 | 2019-05-15 | Ultraviolet fluorescence total sulfur analyzer combustion tube |
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| CN110095445B CN110095445B (en) | 2021-11-23 |
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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 |
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| 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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2019
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|---|---|---|---|---|
| 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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| 吴冰 等: "CHN模式下EA1110元素分析仪反应管填充及制样方法的改进", 《苏州大学学报（自然科学版）》 * |
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