CN201716291U - Analyzer for measuring gas - Google Patents
Analyzer for measuring gas Download PDFInfo
- Publication number
- CN201716291U CN201716291U CN2010202486632U CN201020248663U CN201716291U CN 201716291 U CN201716291 U CN 201716291U CN 2010202486632 U CN2010202486632 U CN 2010202486632U CN 201020248663 U CN201020248663 U CN 201020248663U CN 201716291 U CN201716291 U CN 201716291U
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- sample
- gasification section
- gas
- burning zone
- sample introduction
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- Expired - Lifetime
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Abstract
The utility model relates to an analyzer for measuring gas, which is used for analyzing the gas sample by Coulometry. The analyzer has a sample feeding pipe which enters from a head end of a quartz cracking pipe and penetrates through a gasification section and then enters into a combustion section after passing through the baffle disposed between the combustion section and the gasification section. The feeding gas sample in the utility model directly enters into the combustion section without passing through the gasification section of the quartz cracking pipe so as to increase the analysis speed and the accuracy, change the peak shape and avoid the gas sample from diffusing and caking in the gasification section and leaking from a pin hole of a feeding pad in the gasification section.
Description
Technical field
The utility model relates to a kind of analytical instrument of measuring gas, and the quartz in the coulometry analytical gas sample instrument of more specifically saying so splits pipe unit.
Background technology
The analysis of total sulfur major part is to measure with the coulometry instrument in petroleum chemical enterprise's gas at present, uses homemade syringe sampling.Homemade syringe needle easily stops up, wall easily leaks gas, residual sample is difficult to influences such as displacement is clean, reading is inaccurate in the syringe, makes in the gas analysis of total sulfur repeatability and accuracy very poor, and is all the more so when particularly sulfur content is very low.
With gas sampler by six-way valve with constant volume, stationary temperature and pressure and constant speed sample introduction, analysis result repeatability and accuracy are well a lot.Existing gaseous sample is identical by syringe sampling by gas sampler sample introduction and liquid, and the gasification section of the advanced crystalline silica cracking tube of sample is advanced burning zone then and oxygen reacts, and reaction product is all advanced titration cell.When analyzing the very low gaseous sample of sulfur content by gas sampler and syringe sampling, the sample that has causes the peak to broaden, trail, unstability of base line because of reasons such as diffusion or absorption in gasification section, appearance time prolongs, control rapid and accurate analysis requirement in can not satisfying.
Summary of the invention
The purpose of this utility model provides a kind of analytical instrument of measuring gas, when it can make gas sample introduction without the gasification section of crystalline silica cracking tube, directly enter burning zone, to improve analysis speed and accuracy, change peak shape, avoid gaseous sample at gasification section diffusion, knot charcoal with from the pin hole of gasification section sample introduction pad, leak.
Technical solution of the present utility model is Microcoulomb instrument and the registering instrument in the analytical instrument of existing analytical gas, titration cell, crystalline silica cracking tube and inner gasification section and burning zone, oxygen hose, improve on the basis of nitrogen tube, the utility model particularly has a sample introduction pipeline in the crystalline silica cracking tube, and the sample introduction straight line enters and pass gasification section from the crystalline silica cracking tube head end, and enters burning zone after continuing across dividing plate between burning zone and the gasification section.
The above sample introduction pipeline is connected with gas sampler.
Gas sampler described in the utility model is equipped with six-way valve quantity tube and needle valve respectively on a connecting pipe, or loads onto needle valve on a connecting pipe, threeway, six-way valve quantity tube and the pressure maintaining valve of band needle valve.
The utility model is to increase a sample introduction pipeline on the basis of traditional crystalline silica cracking tube, and this pipeline is connected with gas sampler, by the gas sampler sample introduction, makes gaseous sample directly enter the burning zone of crystalline silica cracking tube.Other structure and conventional quartz cracking tube are identical.Fluid sample is by the gasification section of syringe injection crystalline silica cracking tube during use, and the sample after the gasification is brought burning zone into by carrier gas.Gaseous sample is directly entered the burning zone of crystalline silica cracking tube by the sample introduction pipeline by gas sampler.Gaseous sample also can be injected the gasification section (identical with traditional method) of crystalline silica cracking tube by syringe.
Gaseous sample of the present utility model is connected with gas sampler, and sample enters in the quantity tube of six-way valve, enters burning zone with the sample introduction carrier gas of gas sampler, reacts with oxygen, and the sulphur component is converted into SO
2Deng material, reaction product all flows into titration cell with carrier gas.SO in titration cell
2With I
2Deng material generation redox reaction, the I of consumption
2By electrolysis I
-Replenish, can calculate sulfur content in the sample by Faraday's law according to the electric weight of electrolysis.Crystalline silica cracking tube is the sample dissociation device that is used in the analytical instrument of constituent contents such as micro-coulometric determination petroleum chemicals sulphur, chlorine.Must carry out oxicracking to sample when measuring, whether the crystalline silica cracking tubular construction is reasonable, the sensitivity when being related to sample dissociation and whether reaching instrument detecting fully.
The utility model has the advantages that measure that the gaseous sample analysis speed is fast, good reproducibility, accuracy height, baseline stability, peak shape be good; It is highly sensitive to analyze the very low gaseous sample of sulfur content.Gaseous sample does not advance gasification section, avoids sample at gasification section diffusion, knot charcoal, can reduce the frequent of anti-burning gasification section; Can avoid small amount of sample from the pin hole of gasification section sample introduction pad, to leak.Analyze the high-sulfur gaseous sample, split sampling is simple to operate, good reproducibility, accuracy height.
Description of drawings
Fig. 1 is an organigram of the present utility model;
Fig. 2 is the utility model and gas sampler organigram;
Fig. 3 is the utility model and shunting gas sampler organigram.
Embodiment
Embodiment 1
According to shown in Figure 1, the utility model is a kind of analytical instrument of measuring gas, gasification section 4 and burning zone 3 are arranged on the crystalline silica cracking device of described instrument, there are oxygen hose 5 straight cuttings to cross gasification section 4 and enter burning zone 3, have a nitrogen tube 6 to enter in the gasification section 4 and nitrogen is fed in the gasification section of crystalline silica cracking tube.Tail end at this crystalline silica cracking tube connects a titration cell 2, and titration cell 2 links to each other with micro-library positions instrument and registering instrument 1.The utility model particularly increases a sample introduction pipeline 7 on this basis, and sample introduction pipeline 7 is entered and pass gasification section 4 from the crystalline silica cracking tube head end, and the dividing plate that continues across between burning zone 3 and the gasification section 4 enters burning zone 3.
According to shown in Figure 2, on Fig. 2 with the diacritical point of Fig. 1 only at the gas sampler of sample introduction pipeline rear end, and this gas sampler has a six-way valve quantity tube 8, sample introduction carrier gas delivery pipe 9, needle valve 10, they are cascaded by pipeline.
It is fast that the utility model is measured the gaseous sample analysis speed, good reproducibility, and the accuracy height, baseline stability, peak shape is good; It is highly sensitive to analyze the very low gaseous sample of sulfur content.
Method of operating: press Fig. 2 and connect, the flow velocity of regulating the sample introduction carrier gas is 20~180mL/min, and nitrogen flow rate is 100~200mL/min, and oxygen gas flow rate is 100~160mL/min.Set the coulomb meter operating parameter, treat the instrument baseline stability after, inject a certain amount of sulphur liquid standard specimen with micro syringe, suitably regulate the flow velocity of nitrogen and oxygen, the conversion ratio that makes sulphur liquid standard specimen is 80~120%.Gaseous sample to be measured is connected with gas sampler, and by the gas sampler sample introduction, gaseous sample directly enters burning zone with the sample introduction carrier gas, after the reaction, and the automatic display analysis result of instrument.
Embodiment 3
According to shown in Figure 3, the difference of Fig. 3 and Fig. 1, Fig. 2 is the shunting gas sampler of sample introduction pipe rear end, and it is by needle valve 11, sample introduction carrier gas delivery pipe 9, the needle valve 12 of three-way pipe 13 and shunting outlet, six-way valve quantity tube 8, voltage stabilizer 14 constitutes, and they are cascaded by pipeline.Pressing Fig. 3 when analyzing high-sulfur gaseous sample split sampling (having declared patent) connects, the flow velocity that adjusting enters the sample introduction carrier gas of coulomb meter is 80 mL/min, the flow velocity of regulating the shunting outlet of three-way pipe is 320 mL/min, nitrogen flow rate is 100~180mL/min, and oxygen gas flow rate is 100~160mL/min, and split ratio is 5: 1, make the gaseous sample after the shunting directly advance burning zone, input enters the actual sample size of coulomb meter, after the reaction, and the automatic display analysis result of instrument.The flow velocity of sample introduction carrier gas is determined by experiment according to the size of sulfur content, can not be too low, can not be too high, otherwise can go out anomaly peak, and cause that analysis result is inaccurate, poor repeatability.(total sulfur is less than 5 mg/m to analyze the very low gaseous sample of sulfur content
3), the suitable flow velocity of sample introduction carrier gas is 20~80 mL/min, the flow velocity of oxygen can not be too low (should greater than 120mL/min), otherwise very big anomaly peak can appear in the sample rough burning; (total sulfur is greater than 5 mg/m to analyze the bigger gaseous sample of sulfur content
3), the suitable flow velocity of sample introduction carrier gas is 60~180 mL/min.
Use a kind of analysis data of measuring the analytical instrument of gas of the utility model:
The mensuration of standard specimen repeatability and accuracy;
Use the analytical instrument of mensuration gas of the present utility model by gas sampler sample directly to be sent into burning zone, measuring total sulfur content is 15.16 mg/m
3H
2S gas (nitrogen is spirit), measurement result such as table 1:
(unit is mg/m to the measurement result of table 1 standard specimen repeatability and accuracy as a result
3)
Can find out that from table 1 it is all fine that standard specimen directly advances the repeatability and the accuracy of burning zone measurement result.This is that the sulphur component is adsorbed seldom owing to delivering path in the sample introduction process has shortened.Sample does not advance gasification section, avoids sample to leak from the sample introduction pad of gasification section or residual in gasification section, thereby it is more accurate to measure the result of standard specimen.
The utility model sample advances the comparison of burning zone and air inlet piecewise analysis result, analysis time, peak shape;
(flow rate of carrier gas that advances gasification section and directly advance burning zone all is 150 mL/ minutes) under the same conditions, use the utility model by the gas sampler sample introduction, sample directly advances burning zone, sample and advances gasification section and measure sulfuretted hydrogen and record analysis time in the nitrogen simultaneously, observe the peak type simultaneously, result such as table 2:
Table 2 sample directly advance analysis result that burning zone, sample advance gasification section, analysis time and and the peak type (unit is mg/m as a result
3).
From table 2, can find out and directly enter burning zone and sample by sample to enter the gasification section result almost equal, it is better that sample advances burning zone repeatability, and sample directly to enter burning zone faster than air inlet piecewise analysis speed, baseline is steady, the peak symmetry is high, sharp, narrow peak shape.This is to be avoided diffusion, absorption (or be detained) and a spot of leakage of sample in gasification section because sample directly advances burning zone, avoid of a small amount of absorption of the sample introduction plug of gasification section to the sulphur component, thereby peak shape is relatively good, it is fast to go out the peak, it is fast 36% that analysis speed advances gasification section than sample, and it is big by 0.2% that the result advances gasification section than sample.Therefore, gaseous sample is by the gas sampler sample introduction, and directly advancing the burning zone ratio, to advance gasification section quicker, more accurate.
The utility model sample advances the result of burning zone and the airtight syringe sampling mensuration of import low sulfur gas sample;
The instrumentation condition: nitrogen flow rate is 137 mL/ minutes, and oxygen gas flow rate is 139 mL/ minutes, and the sample introduction flow rate of carrier gas is 50 mL/ minutes, and sample is a SP101 material carbon four, and the liquid standard specimen total sulfur content of demodulating apparatus conversion ratio is 0
.5 mg/L.
Table 3 sample advances the measurement result of burning zone and the airtight syringe sampling of import, and (unit is mg/m as a result
3)
As can be seen from Table 3, sample advances burning zone and sample and advances the gasification section measurement result and coincide, by the gas sampler sample introduction, sample advances gasification section than the airtight syringe sampling analysis speed fast 20% of import, it is fast to illustrate that the utility model is analyzed low sulfur gas sample analysis speed, and the result is (the method permissible variation is 15%) accurately and reliably.
Use the utility model, by shunting gas sampler (patent applied for) sample introduction, the quantity tube volume is 2mL, split ratio is 5:1, and actual sample size is 0.4mL, analyzes the D1158 sample, advance 0.5mL with 2.5mL An Jielun gastight syringe simultaneously, analyse and compare result such as table 4:
(unit is mg/m as a result in the comparison of table 4 split sampling and airtight injector measurement result
3)
Can find out from table 4, use the utility model can split sampling, split sampling repeated fine, and connect and operate all very simple, analysis result and An Jielun gastight syringe coincide (the method permissible variation is 10%), can satisfy fully to produce and analyze requirement.
Claims (3)
1. analytical instrument of measuring gas, it comprises Microcoulomb instrument and registering instrument, titration cell, crystalline silica cracking tube and inner gasification section and burning zone, oxygen hose, nitrogen tube, it is characterized in that having in the crystalline silica cracking tube sample introduction pipeline, the sample introduction pipeline enters and passes gasification section from the crystalline silica cracking tube head end, and enters burning zone after continuing across dividing plate between burning zone and the gasification section.
2. a kind of analytical instrument of measuring gas according to claim 1 is characterized in that the sample introduction pipeline in the crystalline silica cracking tube is connected with gas sampler.
3. a kind of analytical instrument of measuring gas according to claim 2, it is characterized in that gas sampler is on a connecting pipe six-way valve quantity tube and needle valve to be housed respectively, or on a connecting pipe, load onto needle valve, threeway, six-way valve quantity tube and the pressure maintaining valve of band needle valve.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2010202486632U CN201716291U (en) | 2010-07-06 | 2010-07-06 | Analyzer for measuring gas |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2010202486632U CN201716291U (en) | 2010-07-06 | 2010-07-06 | Analyzer for measuring gas |
Publications (1)
Publication Number | Publication Date |
---|---|
CN201716291U true CN201716291U (en) | 2011-01-19 |
Family
ID=43462296
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2010202486632U Expired - Lifetime CN201716291U (en) | 2010-07-06 | 2010-07-06 | Analyzer for measuring gas |
Country Status (1)
Country | Link |
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CN (1) | CN201716291U (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103399074A (en) * | 2013-07-29 | 2013-11-20 | 中国石油化工股份有限公司 | Quartz tube device for determining trace total sulfur and trace total chlorine |
CN106153699A (en) * | 2016-07-28 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of method improving analysis of total sulfur accuracy |
-
2010
- 2010-07-06 CN CN2010202486632U patent/CN201716291U/en not_active Expired - Lifetime
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103399074A (en) * | 2013-07-29 | 2013-11-20 | 中国石油化工股份有限公司 | Quartz tube device for determining trace total sulfur and trace total chlorine |
CN103399074B (en) * | 2013-07-29 | 2015-05-13 | 中国石油化工股份有限公司 | Quartz tube device for determining trace total sulfur and trace total chlorine |
CN106153699A (en) * | 2016-07-28 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of method improving analysis of total sulfur accuracy |
CN106153699B (en) * | 2016-07-28 | 2019-03-15 | 中国石油化工股份有限公司 | A method of improving analysis of total sulfur accuracy |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CX01 | Expiry of patent term | ||
CX01 | Expiry of patent term |
Granted publication date: 20110119 |