CN101793863A - Split gas sample injection device - Google Patents
Split gas sample injection device Download PDFInfo
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- CN101793863A CN101793863A CN 201010126486 CN201010126486A CN101793863A CN 101793863 A CN101793863 A CN 101793863A CN 201010126486 CN201010126486 CN 201010126486 CN 201010126486 A CN201010126486 A CN 201010126486A CN 101793863 A CN101793863 A CN 101793863A
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Abstract
The invention relates to a split gas sample injection device which is used for analysis of total sulfur in gas of a petrochemical enterprise, a pressure stabilizing valve is arranged on a sample injection carrier gas pipe, two communicated three-ways are arranged on a conveying pipe, the first three-way is provided with a device for regulating the split ratio, the second three-way is provided with a carrier gas flow rate regulating and pressure stabilizing device for regulating the conversion rate of an instrument, and an outlet of the second three-way is communicated with a gas analyzer. The split gas sample injection device can analyze a variety of gas samples with different sulfur contents by taking a gas sample injection device, a liquid standard sample and the instrument as parameters, thereby expanding the analysis range of the sulfur content in the gas, simplifying the operation, improving the analysis speed, saving the time for debugging the instrument, saving the cost for purchasing the liquid standard sample and the instrument and reducing the production cost.
Description
Technical field
The present invention relates to the split sampling device of impurity content in the gas or composition analysis, be mainly used in impurity content analysis such as total sulfur in the gas.
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.Because homemade syringe needle easily stops up, the easily gas leakage behind pinprick repeatedly of the sample introduction pad of flame tube, chip enters easily that flame tube, syringe wall easily leak gas, reading be subjected to human factor to influence in big, the syringe residual sample to be difficult to displacement clean, make in the gas analysis of total sulfur repeatability and accuracy very poor, all the more so when particularly sulfur content is very low.As use gas sampler, with constant volume, stationary temperature and pressure and constant speed sample introduction, analysis result repeatability and accuracy can be got well much by six-way valve.But the volume of the quantity tube of six-way valve immobilizes, to sulfur content in the gas from several mg/m
3To several thousand mg/m
3Sample, obviously improper with a kind of sample size.Most of at present concentration and Instrument operation parameter that changes the liquid standard specimen with the size of sulfur content in the sample that adopt readjusts conversion ratio, wastes time and energy control rapid and accurate analysis requirement in can not satisfying like this.At present, gas sampler has ready-made product both at home and abroad, and sample size has 1mL, 2mL, 4mL, 10mL etc., but can not shunt, and sample size can not be regulated at any time, can only change the quantity tube that varies in size, operation inconvenience.Can occur not detecting or outrange for the very low or very high sample of sulfur content, a kind of sample size is difficult to adapt to sulfur content from several mg/m
3To several thousand mg/m
3The analysis of gaseous sample, need many people at present, many instruments, height sulphur content drives row analysis into, waste great amount of manpower and material resources.
Summary of the invention
The purpose of this invention is to provide a kind of shunting gas sample injection device, it is to change the gas sampling amount by shunting, and the sample size of gas sampler can be regulated arbitrarily within the specific limits, so that the very big all gases samples of impurity content variation range such as analysis sulphur.
Technical solution of the present invention is, on the basis of existing petrochemical industry gas analysis of total sulfur gas sampler, improve, promptly at the sample introduction carrier gas pipe that is provided with needle valve and six-way valve that is communicated with it and quantity tube, carrier gas and sample enter on the basis of delivery pipe of coulomb meter and improve.The present invention is that sample introduction carrier gas pipe is provided with a pressure maintaining valve, described delivery pipe is provided with two threeways that communicate, first threeway is provided with the device of regulating split ratio, second threeway is provided with the adjusting and the stable-pressure device of the flow rate of carrier gas of demodulating apparatus conversion ratio, and the outlet of second threeway is connected with gas analyzer.
The device of the adjusting split ratio of the above first threeway setting is that needle valve of connection in the shunting outlet of described first threeway is connected in its outlet and another needle valve with the import connection of second threeway.
The adjusting and the stable-pressure device of the flow rate of carrier gas of the demodulating apparatus conversion ratio of second threeway setting of the present invention be, is communicated with a needle valve at the carrier gas inlet place of the demodulating apparatus conversion ratio of described second threeway, and described needle valve is connected with a pressure maintaining valve.
The above gas analyzer is a coulomb meter.
The present invention connects a three-way shunt behind the six-way valve sample export of gas sampler, advance in the gas circuit of coulomb meter and the shunting outlet respectively connects a needle valve at sample, control the pressure of whole gas circuit with pressure maintaining valve, regulate the flow of this two-way gas by needle valve, change split ratio, thereby can regulate the sample size that enters in the coulomb meter arbitrarily within the specific limits, for the high-sulfur sample, it is big that split ratio is adjustable, the low content sample can be closed shunting, do not need to change liquid standard specimen and Instrument operation parameter like this, an instrument can be analyzed the gaseous sample of different sulfur contents, and work efficiency can improve greatly.For the bigger sample of sulfur content fluctuation ratio, the more convenient practicality of split sampling can not exceed the apparatus measures scope when content is very high, when content is very low, closes shunting, NF phenomenon can not occur.The flow of two-way gas can accurately be measured by the An Jielun gas meter, and actual sample size can accurately calculate.When very little, the shunting gas sampler is not subjected to the influence of artificial reading than the quantitative standard of syringe for sample size, thereby the repeatability of measurement result and accuracy want high a lot, and easy to operate, is difficult for stopping up.
Principle of work: under the identical condition of pressure and temperature, the volume that advances gas in the coulomb meter and the ratio of the volume of shunting exit gas equal the throughput ratio of this two-way gas.Flow by accurate mensuration two-way gas just can be calculated split ratio, thereby can calculate the actual sample size of gaseous sample.Because pressure maintaining valve has been installed, the gaseous tension of stainless steel threeway inlet is constant, two way outlets of threeway are respectively installed a needle valve, and by regulating this 2 needle valves, scalable enters the flow (V1 of gas in the coulomb meter, ml/min) with the flow (V2 that shunts exit gas, ml/min), thereby can calculate split ratio (n), split ratio (n) is big more, gas sample introduction amount (x, milliliter) is more little; (n) is more little for split ratio, and gas sample introduction amount (x, milliliter) is big more.
n＝(V2+V1)/V1
If the volume of six-way valve quantity tube is the V milliliter, gas sample introduction amount (x, milliliter): x=V/n shunting gas sample injection device of the present invention split sampling is analyzed data
Three, split sampling is measured the analysis result of gas and sample
(1) shunting gas sample injection device split sampling is measured the analysis result of high-sulfur gas and sample
1, shunting gas sample injection device split sampling is measured the analysis result of high-sulfur gas
With the COS gas of shunting gas sample injection device (the sample introduction flow rate of carrier gas that enters coulomb meter is 100ml/ minute, and the shunting exit velocity is 400ml/ minute, and split ratio is 5: 1) mensuration Foshan section, nitrogen is spirit, and total sulfur content is 3585.0mg/m
3, quantity tube is 1mL, and sample size is 0.2mL, and the liquid standard specimen of school instrument is 100mg/L, measurement result such as table 1:
The analysis result of 5: 1 shunt measurement gases of table 1. shunting gas
| Measure number of times | ??1 | ??2 | ??3 | ??4 | ??5 | Mean value | Standard deviation | Relative standard deviation % | Relative error % |
| Measurement result | ??3527.7 | ??3435.9 | ??3557.4 | ??3601.9 | ??3608.1 | ??3546.2 | ??69.9 | ??1.97 | ??-1.1 |
Can find out from table 1,5: 1 split samplings, repeatability and the accuracy of measuring gas are all fine.
2. different split ratios is measured the analysis result of same sample
With the conversion ratio of 100mg/L liquid standard specimen demodulating apparatus, get the 1mL sample with 1mL Germany gastight syringe, the total sulfur that back A liquefied gas is taken off in mensuration desulfurization (two) is 830.0mg/m
3, then with shunting gas sample injection device by closing shunting, shunting in 2: 1,4: 1,6: 1 and same sample is measured analysis result such as table 2:
The analysis result of table 2. syringe sampling and split sampling working sample
| The mensuration mode | Close shunting, advance 1mL | 1/2mL is advanced in shunting in 2: 1 | Shunting in 4: 1 advances 1/4 | Shunting in 6: 1 advances 1/6 | Mean value | Standard deviation | Relative standard deviation % | Relative deviation % |
| Measurement result | ??833.0 | ??799.3 | ??803.8 | ??823.4 | ??814.9 | ??15.98 | ??1.96 | ??-1.8 |
Can find out from table 2, close shunting and coincide better, and coincide with German gastight syringe measurement result by different split ratio shuntings.
3. the application of split sampling
Measure from several mg/m with shunting gas sample injection device (closing shunting, split ratio 2: 1,3: 1,5: 1,7: 1)
3To several thousand mg/m
3The all gases sample, result such as table 3:
The application of table 3. split sampling
Can find out that from table 3 the shunting gas sample injection device only needs to change split ratio, just can analyze sulfur content from several mg/m with a kind of liquid standard specimen
3To several thousand mg/m
3The all gases sample, analysis result and traditional method are coincide better, in method permissible variation scope (method requires relative deviation less than 15%).The analyst coverage of sulfur content in this method enlargement gas; improve the utilization factor of instrument; save the acquisition expenses of instrument and liquid standard specimen; save the instrument testing time; increase work efficiency; simultaneously can avoid of the pollution of the sulphur component of high-load, thereby influence the analysis of low-sulfur sample instrument, also very beneficial to the protection instrument.When split sampling was analyzed the high-sulfur sample, because sample size is few, the peak type was good, and it is fast to go out the peak, and analysis speed is fast, good reproducibility, and analysis result is accurate, and is very with practical value in middle control analysis, has broad application prospects in the petrochemical complex analysis.
The shunting gas sample injection device both can change sample size, can close shunting again, with the constant volume sample introduction, advantage with syringe (sample size can change) and gas sampler (good reproducibility), overcome their shortcoming (syringe repeatability and poor accuracy, the gas sampler sample size can not be regulated at any time), can substitute traditional syringe and gas sampler sample introduction fully, be a kind of utility model instrument.
Advantage of the present invention: with a shunting gas sample injection device, a kind of liquid standard specimen, a kind of Instrument operation parameter can be analyzed the different all gases samples of impurity content such as sulphur, and the analyst coverage of impurity such as sulphur simplifies the operation in the enlargement gas, improves analysis speed.Save the time of adjusting instrument, save liquid standard specimen and Instrument purchase expense, reduce production costs.By the flow of pressure maintaining valve and needle valve may command two-way gas, its flow can accurately be measured by the An Jielun digital flowmeter, thereby can accurately regulate the sample size of split ratio and gaseous sample, compares sample size scalable of the present invention with traditional gas sampler; Compare with syringe, sample size is accurate, good reproducibility.The present invention draws the advantage of traditional gas sampler and syringe, overcomes their shortcoming, thereby improves the repeatability and the accuracy of analysis result greatly.
Description of drawings
The injector organigram that Fig. 1 is traditional
Fig. 2 organigram of the present invention
Embodiment
According to shown in Figure 1, traditional injector is that sample introduction carrier gas pipe 1 links to each other with the import of needle valve 11 now, and the outlet of needle valve 11 links to each other with quantity tube 3 with six-way valve, and carrier gas and the sample sent by six-way valve and quantity tube 3 enter coulomb meter through delivery pipe 4.
According to shown in Figure 2, the present invention is provided with pressure maintaining valve 2 on sample introduction carrier gas pipe 1, sample introduction carrier gas pipe 1 is connected with six-way valve and quantity tube 3, six-way valve and quantity tube 3 outlets are connected with sample introduction carrier gas and sample delivery pipe 4, a three-way shunt 5 is set on sample introduction carrier gas and sample delivery pipe 4, the shunting outlet of three-way shunt 5 is provided with needle valve 6, the outlet of three-way shunt is provided with needle valve 7, needle valve 7 outlets are connected with three-way pipe 8 imports of the carrier gas of advancing coulomb meter, three-way pipe 8 outlets are communicated with coulomb meter, and the carrier gas inlet of advancing coulomb meter of three-way pipe is provided with needle valve 9 and coupled logical pressure maintaining valve 10.
Concrete operations of the present invention:
1, the jointing of needle valve 7 and second threeway 8 is pulled down (getting final product) with two finger manipulations, regulate needle valve 7, making into, the sample introduction flow rate of carrier gas of coulomb meter (needle valve 7 exit velocities) is 100mL/ minute, counting the constant flow meter with An Jielun accurately measures, then jointing is connected, nut is tightened (getting final product),, guarantee air tight with leak test liquid leak test with two finger manipulations.This road gas flow rate is when constant pressure, and its flow velocity is constant usually, does not need all to measure at every turn.
2, regulate needle valve 6 (needle valve 7 keeps motionless), making the flow velocity of shunting outlet is 400mL/ minute, counts the constant flow meter with An Jielun and accurately measures, and then split ratio is 5: 1.When transferring other split ratio, only need to regulate needle valve 6, the flow velocity that changes the shunting outlet gets final product.When sulphur impurity content was very low in the gaseous sample, the flow velocity that needle valve 6 is exported was adjusted to 0 (promptly closing needle valve 6), closes shunting.
3, regulate needle valve 9, make into that the flow rate of carrier gas of coulomb meter is about 100mL/ minute (being with spinner-type flowmeter on the coulomb meter, in needle valve 9 outlets), its flow velocity does not need accurate mensuration.Set the operating conditions of coulomb meter, regulate the flow velocity of oxygen, inject the liquid standard specimen of a certain amount of 100mg/L, start instrument simultaneously, begin to analyze with fluid injector.Instrument is measured conversion ratio automatically, according to the size of conversion ratio, regulates needle valve 9, suitably reduces or increase the flow velocity of carrier gas (the accent conversion ratio) flow velocity and oxygen, makes the conversion ratio of sulphur liquid standard specimen reach 80～120% (identical with traditional control method).
4, the volume of setting buret is 1mL, actual sample size is 0.2mL after shunting, import 0.2mL in the parameter of coulomb meter sample size and (or the sample size parameter still imported 1mL, the instrument result displayed be multiply by 5 promptly get analysis result), six-way valve knob with gas sampler places the sampling location then, allows the sample displacement quantity tube approximately after half a minute, and the six-way valve knob of gas sampler is placed the sample introduction position, start instrument simultaneously, begin to analyze.Carrier gas is brought the sample (0.2mL) of six-way valve quantity tube 3 into coulomb meter, and other has the 0.8mL sample to flow out from the shunting outlet.After analysis finished, instrument was according to the total sulfur quality (representing with ng) in the gaseous sample of measuring and advance the volume (representing with mL) of the gaseous sample of coulomb meter, prints analysis result automatically (with mg/m
3Expression is equivalent to ng/mL).
5, if will close the shunting gas sampler, only need close needle valve 6, making the shunting exit velocity is 0, sample introduction as stated above, then sample size is 1mL.
6, the pressure of 2 controls of the pressure maintaining valve before the six-way valve quantity tube is greater than the pressure of pressure maintaining valve 10 controls.
The effect of pressure maintaining valve 10 mainly is a pressure of regulating carrier gas, and the pressure P 1 that makes its control is less than the pressure P 2 by the sample introduction carrier gas of pressure maintaining valve 2 controls, i.e. P2＞P1, otherwise sample can be all from the shunting outlet outflow of isocon, and sample can't be analyzed.
Pressure maintaining valve also can make the constant pressure of carrier gas, prevents supply pressure fluctation, causes the flow rate of carrier gas fluctuation that enters storehouse, storehouse instrument, influences the conversion ratio of instrument, thus the impact analysis result.
The effect of three-way pipe 8 is with the carrier gas of the carrier gas of demodulating apparatus conversion ratio and split sampling separately, does not disturb mutually, can avoid a large amount of carrier gas to flow out from the shunting outlet of three-way shunt simultaneously.
Claims (4)
1. shunt gas sample injection device for one kind, it comprises sample introduction carrier gas pipe, the six-way valve quantity tube, carrier gas and sample enter the delivery pipe of coulomb meter, it is characterized in that described sample introduction carrier gas pipe is provided with a pressure maintaining valve, described delivery pipe is provided with two threeways that communicate, and first threeway is provided with the device of regulating split ratio, second threeway is provided with the adjusting and the stable-pressure device of the flow rate of carrier gas of demodulating apparatus conversion ratio, and the outlet of second threeway is connected with gas analyzer.
2. a kind of shunting gas sample injection device according to claim 1, the device that it is characterized in that the adjusting split ratio of described first threeway setting is, in the shunting outlet of described first threeway, connect a needle valve, be connected in its outlet and another needle valve with the import connection of second threeway.
3. a kind of shunting gas sample injection device according to claim 1, the adjusting and the stable-pressure device of flow rate of carrier gas that it is characterized in that the demodulating apparatus conversion ratio of described second threeway setting is, carrier gas inlet place at the demodulating apparatus conversion ratio of described second threeway is communicated with a needle valve, and described needle valve is connected with a pressure maintaining valve.
4. a kind of shunting gas sample injection device according to claim 1 is characterized in that described gas analyzer is a coulomb meter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101264865A CN101793863B (en) | 2010-03-15 | 2010-03-15 | Split gas sample injection device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101264865A CN101793863B (en) | 2010-03-15 | 2010-03-15 | Split gas sample injection device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101793863A true CN101793863A (en) | 2010-08-04 |
| CN101793863B CN101793863B (en) | 2012-11-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101264865A Active CN101793863B (en) | 2010-03-15 | 2010-03-15 | Split gas sample injection device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109283264A (en) * | 2017-07-21 | 2019-01-29 | 日本株式会社日立高新技术科学 | It generates gas analyzing apparatus and generates analysis method for gases |
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| US3400585A (en) * | 1964-07-23 | 1968-09-10 | Bendix Balzers Vacuum Inc | Method of measuring the output of a source of a certain gas |
| CN2268257Y (en) * | 1996-05-23 | 1997-11-19 | 徐春明 | Quick-acting analysis instrument for smoke |
| CN201653973U (en) * | 2010-03-15 | 2010-11-24 | 中国石油化工股份有限公司 | Diverted gas sample injecting device |
-
2010
- 2010-03-15 CN CN2010101264865A patent/CN101793863B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3400585A (en) * | 1964-07-23 | 1968-09-10 | Bendix Balzers Vacuum Inc | Method of measuring the output of a source of a certain gas |
| CN2268257Y (en) * | 1996-05-23 | 1997-11-19 | 徐春明 | Quick-acting analysis instrument for smoke |
| CN201653973U (en) * | 2010-03-15 | 2010-11-24 | 中国石油化工股份有限公司 | Diverted gas sample injecting device |
Non-Patent Citations (3)
| Title |
|---|
| 《化工自动化及仪表》 19941231 彭家轩 二氧化硫分析器的改进 第55-56页 1-4 第21卷, 第6期 * |
| 《有机化学》 19820831 陈明灿等 毛细管气体色谱分析及毛细管柱动态涂渍两用仪 第307-309页 1-4 , 第4期 * |
| 《炼油与化工》 20031231 梁景程 合成气中总硫含量的测定 第30-31页 1-4 第14卷, 第4期 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109283264A (en) * | 2017-07-21 | 2019-01-29 | 日本株式会社日立高新技术科学 | It generates gas analyzing apparatus and generates analysis method for gases |
| CN109283264B (en) * | 2017-07-21 | 2023-02-28 | 日本株式会社日立高新技术科学 | Generated gas analyzing apparatus and generated gas analyzing method |
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| Publication number | Publication date |
|---|---|
| CN101793863B (en) | 2012-11-14 |
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