CN106323730A - Special quartz cracking tube for off-line gas analysis - Google Patents
Special quartz cracking tube for off-line gas analysis Download PDFInfo
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- CN106323730A CN106323730A CN201510416543.6A CN201510416543A CN106323730A CN 106323730 A CN106323730 A CN 106323730A CN 201510416543 A CN201510416543 A CN 201510416543A CN 106323730 A CN106323730 A CN 106323730A
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Abstract
The invention relates to a special quartz cracking tube for off-line gas analysis. The special quartz cracking tube is characterized in that (1) the cracking tube is prepared by firing high-purity quartz and can resist high temperature over 1,250 DEG C; (2) only one oxygen inlet is designed for the cracking tube, and the oxygen serves as a carrier gas as well as a combustion-supporting gas; (3) a sample inlet is designed at an entrance of the tube body, and a to-be-measured gas is introduced into the quartz cracking tube through the sample inlet for combustion; and (4) coaxial sample-in tube and double-layer combustion tube in sealed connection are designed for the cracking tube, an exit of the sample-in tube is opposite to the exit direction of the inner-layer combustion tube, and the inner-layer combustion tube is opposite to the exit direction of the outer-layer combustion tube. The quartz cracking tube provided by the invention is mainly used for analyzing and measuring the harmful elements such as total sulfur, total nitrogen and total chlorine in the gas samples of petrochemical industry such as natural gas, coal gas, liquefied gas, ethylene and propane, and can be used for remarkably increasing the current maximum sample size of 10ml in gas analysis by 4 times to 50ml so as to enhance the signals in measurement.
Description
Technical field
The present invention relates to a kind of special crystalline silica cracking tube of off-line gas analysis, be mainly used in natural gas, coal gas, liquefied gas, ethylene,
The harmful elements such as total sulfur in the petrochemical industry class gaseous samples such as propane, total nitrogen and total chlorine measure containing quantitative analysis, belong to petrochemical industry
Analysis technical field.
Background technology
The petrochemical industry class gaseous samples such as natural gas, coal gas, liquefied gas, ethylene, propane production, store, transport and make
During with, the existence of the trace element such as sulfur therein, chlorine, nitrogen is to cause production equipment corrosion, catalyst poisoning, commercialization
The principal element that the discharge of product poor stability, waste gas exceeds standard etc..Therefore, to units such as sulfur, chlorine, nitrogen in various gaseous state petroleum chemicals
The detection of cellulose content has become analysis project most important in current oil chemical industry, modal.And to various gaseous samples
During detection, off-line analysis remains current Main Means.
Nowadays, when carrying out the off-line analysis of the trace element such as total sulfur, total nitrogen, total chlorine in various gaseous state petroleum chemicals, mainly adopt
With ultraviolet fluorescence method, chemoluminescence method and small-hole drilling, these methods all must introduce the sample into and be heated to 800～1100 DEG C
Make sample generation oxidizing fire in crystalline silica cracking tube, be converted into detectable sulfur, chlorine, nitrogen etc., then detect.Occurring
During combustion reaction, the structure design of crystalline silica cracking tube directly affects maximum sample size and the detection essence of instrument that instrument is allowed
Degree and sensitivity.Currently marketed off-line gas analysis crystalline silica cracking tube generally also exists sample at cracking intraductal retention time
The problem that short, sample size is little, general sample size is all at 1～5 milliliter, and maximum sample size is also only 10 milliliters, and sample size is slightly larger then
Easily cause incomplete combustion and form carbon distribution, thus cause light path pollution, sample room pollution, detector to pollute and electrolyzer
Pollute, deal with and bother very much, even cause instrument to run when carbon distribution is serious, directly scrap.Due to the impact of carbon distribution,
Directly limit cannot promoting of sample size, thus the precision of method when limiting the trace element detections such as total sulfur, total nitrogen, total chlorine
The further lifting of degree, accuracy, Monitoring lower-cut and detection limit.Therefore, a big sample size off-line gas analysis is designed special
Crystalline silica cracking tube, the always striving direction of petrochemical industry analyst.
Summary of the invention
It is an object of the invention to overcome weak point of the prior art, it is provided that a kind of brand new design, can be fully solved
Carbon distribution problem, significantly improve gaseous sample sample size, fundamentally promote harmful element detection time method precision, accuracy,
Monitoring lower-cut and the special crystalline silica cracking tube of off-line gas analysis of detection limit.
The present invention adopts the following technical scheme that
A kind of special crystalline silica cracking tube of off-line gas analysis, including body, combustor, is positioned at the injection port of body front end, oxygen
Entrance, fixing post, sample feeding pipe and be positioned at the mixed gas outlet pipe of body rear end.Described cracking tube is designed with and is sealedly connected on
The most coaxial sample feeding pipe and double-deck cracking tube, sample feeding pipe outlet is contrary with internal layer cracking tube Way out, internal layer cracking tube and
Outer layer cracking tube Way out is contrary.Described cracking tube only designs an oxygen intake, and oxygen is not only as carrier gas but also make combustion-supporting gas；
Body front end is also devised with fixing post, for crystalline silica cracking tube is fixed on high-temperature cracking furnace.
Described sample feeding pipe is straight tube, and a diameter of Ф 10～15mm, this sample feeding pipe extends to the rear end of internal layer cracking tube.Described
Internal layer cracking tube a length of 200～300mm, outer layer cracking tube a length of 400～450mm, internal layer cracking tube is a diameter of
Ф 18-25mm, outer layer cracking tube a diameter of Ф 25-30mm.
This cracking tube is fired by high purity quartz and is formed, and is resistant to the high temperature of more than 1250 DEG C.
The invention have the advantage that
1. devise and be sealed connected together and coaxial sample feeding pipe and double-deck cracking tube, after gaseous sample is introduced into sample feeding pipe, first
First the end at sample feeding pipe i.e. burns, and is then passed through internal layer cracking tube generation second-time burning, and the product after burning is again from internal layer
Cracking tube enters outer layer cracking tube, again occurs fully to burn completely, eventually passes mixed gas outlet pipe and enter detector.This
Sample, gas to be measured will occur the most fully to burn in crystalline silica cracking tube, does not have any carbon distribution and produces, thus significantly improves
The sample size of gaseous sample, it is ensured that the big sample size of gas and fast sample analysis.
2. abandoned traditional carrier gas inlet (argon) and helped double entry design of fuel gas inlet (oxygen), only one oxygen of design
Gas entrance, gaseous sample to be measured was both loaded into cracking tube as carrier gas, and made gaseous sample to be measured in cracking as combustion-supporting gas again by oxygen
Fully burn in pipe.Traditional carrier gas inlet design is to use argon as carrier gas, and this is primarily to prevent liquid sample
At high temperature during gasification, the rustless steel syringe needle of microsyringe is burnt out；And when carrying out gaseous sample analysis, then need not move through liquid
To the conversion of gaseous state, therefore without using argon as carrier gas, only the first half of sample feeding pipe need to be designed in the outside of pyrolysis furnace,
I.e. part between injection port and fixing post.Owing to this part is in the outside of pyrolysis furnace, temperature is relatively low, thus without appearance
The situation that syringe needle is burnt.The advantage of this design is i.e. to save the argon of costliness, decreases again a possible interference
Source；And due to oxygen all in cracking tube, burn even if raising sample size also can make sample obtain more substantially entirely,
Do not produce any carbon distribution, it is achieved thereby that the accurate stable of the micronutrient levels such as sulfur, chlorine, nitrogen is measured in gaseous sample.
3. devise fixing post, for crystalline silica cracking tube is fixed on high-temperature cracking furnace.Which solves during sample introduction due to
The mobile problem of cracking tube and the crystalline silica cracking tube that causes damages, and the problem of the analysis result poor repeatability caused.
4. use the special crystalline silica cracking tube of off-line gas analysis of present invention design, due to sample combustion reaction completely, do not produce and appoint
What carbon distribution, then the current maximum sample size 10 milliliters when can be analyzed by gaseous sample harmful element significantly improves 4 times, reaches 50
Milliliter, thus relatively strengthen signal when measuring, significantly improve the detection sensitivity of low content total sulfur, total nitrogen, total chlorine etc., inspection
Surveying lower limit can as little as 0.05mg/m3, detection limit can as little as 0.02mg/m3。
Accompanying drawing explanation
Fig. 1 is the special crystalline silica cracking tube of off-line gas analysis of the present invention.
Detailed description of the invention
Fig. 1 show the special crystalline silica cracking tube of off-line gas analysis of the present invention, oxygen intake 3 and the injection port 2 of combustion tube front end
Connection, oxygen purity is generally high purity oxygen gas, and regulation oxygen flow is 250～450ml/min, and injection port 2 silica gel plug enters
Row seals.After glass syringe extraction appropriate amount of sample, penetrate injection port 2 by silica gel plug, then utilize mechanical pusher
Or manually gaseous sample to be measured is pushed sample feeding pipe 5.Under the carrying of oxygen, sample burns at the latter end of sample feeding pipe 5
Reaction.
Gaseous mixture after burning is entered internal layer cracking tube 6 by sample feeding pipe 5, and second-time burning occurs.Sample feeding pipe 5 is designed as and internal layer
Cracking tube 6 is in opposite direction, so that the gaseous sample burnt the most completely at sample feeding pipe 5 latter end fully enters internal layer cracking tube
6, again burn.Internal layer cracking tube 6 is contrary with outer layer cracking tube 7 Way out, and gaseous mixture occurs at internal layer cracking tube 6
After second-time burning, then entered outer layer cracking tube 7 by internal layer cracking tube 6, again burn.Through the most fully repeating burning,
The most do not have any carbon distribution to produce, thus significantly improve the sample size of gaseous sample, it is ensured that entering greatly when gaseous sample is analyzed
Sample amount and fast sample analysis.
Sample layer cracking tube 7 outside, after again fully burning, under the carrying of oxygen, enters via mixed gas outlet pipe 8
Detector detects.
The present invention is total sulfur, total nitrogen and total in the petrochemical industry gaseous sample such as natural gas, coal gas, liquefied gas, ethylene, propane
The analysis of the impurity contents such as chlorine measures, and is a kind of special cracking tube of off-line gas analysis, is transformed injection port part, it is possible to
In various petrochemical industry gaseous samples, the on-line analysis of the impurity content such as total sulfur, total nitrogen and total chlorine measures.Have sample size big,
Signal absolute value is high, signal to noise ratio high, testing result accuracy is high, precision is good, Monitoring lower-cut and the low advantage of detection limit.
Claims (6)
1. the special crystalline silica cracking tube of off-line gas analysis, including body, combustor, is positioned at the injection port of body front end, oxygen
Gas entrance, fixing post, sample feeding pipe and be positioned at the mixed gas outlet pipe of body rear end, it is characterised in that described cracking tube designs
Having and be sealed connected together and coaxial sample feeding pipe and double-deck cracking tube, sample feeding pipe outlet is contrary with internal layer cracking tube Way out,
Internal layer cracking tube is contrary with outer layer cracking tube Way out, and is resistant to the high temperature of more than 1250 DEG C；Described cracking tube only designs one
Oxygen intake, oxygen is not only as carrier gas but also make combustion-supporting gas；Body front end is also devised with fixing post, for being fixed by crystalline silica cracking tube
On high-temperature cracking furnace.
Cracking tube the most according to claim 1, it is characterised in that this cracking tube is fired by high purity quartz and formed.
Cracking tube the most according to claim 1, it is characterised in that the 1/2～3/4 of its internal layer cracking tube a length of outer layer cracking tube,
The 2/3～4/5 of internal layer cracking tube a diameter of outer layer cracking tube.
Cracking tube the most according to claim 1, it is characterised in that its sample feeding pipe is straight tube, a diameter of 10～15mm.
Cracking tube the most according to claim 1, it is characterised in that its sample feeding pipe extends to the rear end of internal layer cracking tube.
Cracking tube the most according to claim 1, it is characterised in that needed for this cracking tube, carrier gas is oxygen, and required combustion-supporting gas is also
For oxygen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510416543.6A CN106323730A (en) | 2015-07-07 | 2015-07-07 | Special quartz cracking tube for off-line gas analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510416543.6A CN106323730A (en) | 2015-07-07 | 2015-07-07 | Special quartz cracking tube for off-line gas analysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106323730A true CN106323730A (en) | 2017-01-11 |
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ID=57725448
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510416543.6A Pending CN106323730A (en) | 2015-07-07 | 2015-07-07 | Special quartz cracking tube for off-line gas analysis |
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| CN (1) | CN106323730A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109580327A (en) * | 2018-12-17 | 2019-04-05 | 北矿检测技术有限公司 | Pyrohydrolysis combustion tube |
| CN112098587A (en) * | 2019-06-18 | 2020-12-18 | 耶拿分析仪器股份公司 | Reaction tube for elemental analysis |
| CN112964751A (en) * | 2021-02-05 | 2021-06-15 | 上海元析仪器有限公司 | Double-layer combustion tube for total organic carbon analyzer |
| CN112964826A (en) * | 2021-03-17 | 2021-06-15 | 中国大唐集团科学技术研究院有限公司华中电力试验研究院 | Trapping device and method for measuring chloride ions in oil through high-temperature combustion hydrolysis-potentiometric titration |
-
2015
- 2015-07-07 CN CN201510416543.6A patent/CN106323730A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109580327A (en) * | 2018-12-17 | 2019-04-05 | 北矿检测技术有限公司 | Pyrohydrolysis combustion tube |
| CN112098587A (en) * | 2019-06-18 | 2020-12-18 | 耶拿分析仪器股份公司 | Reaction tube for elemental analysis |
| US11435329B2 (en) | 2019-06-18 | 2022-09-06 | Analytik Jena Ag | Reaction tube for elemental analysis |
| CN112964751A (en) * | 2021-02-05 | 2021-06-15 | 上海元析仪器有限公司 | Double-layer combustion tube for total organic carbon analyzer |
| CN112964826A (en) * | 2021-03-17 | 2021-06-15 | 中国大唐集团科学技术研究院有限公司华中电力试验研究院 | Trapping device and method for measuring chloride ions in oil through high-temperature combustion hydrolysis-potentiometric titration |
| CN112964826B (en) * | 2021-03-17 | 2023-10-17 | 中国大唐集团科学技术研究院有限公司华中电力试验研究院 | Device and method for capturing chloride ions in high-temperature combustion hydrolysis-potentiometric titration measurement oil |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170111 |
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| WD01 | Invention patent application deemed withdrawn after publication |