CN102620957A - Chromatographic analyzing and sampling system for bottled silane sample - Google Patents
Chromatographic analyzing and sampling system for bottled silane sample Download PDFInfo
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- CN102620957A CN102620957A CN2012101116345A CN201210111634A CN102620957A CN 102620957 A CN102620957 A CN 102620957A CN 2012101116345 A CN2012101116345 A CN 2012101116345A CN 201210111634 A CN201210111634 A CN 201210111634A CN 102620957 A CN102620957 A CN 102620957A
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Abstract
The invention discloses a chromatographic analyzing and sampling system for a bottled silane sample. The system comprises a chromatographic analyzer, a helium gas steel cylinder, a standard gas steel cylinder, a vacuum pump, a helium gas valve V1, a standard gas valve V2, a one-way valve, a sample gas valve V3, a pressure reducing valve, a vacuum pump valve V4 and an emptying valve V5, wherein the one-way valve, the sample gas valve V3, the vacuum pump valve V4 and the emptying valve V5 are connected in parallel to the pressure reducing valve; the helium gas valve V1 and the standard gas valve V2 are connected in parallel to the one-way valve; the helium gas valve V1 is connected with the helium gas steel cylinder; the standard gas valve V2 is connected with the standard helium gas steel cylinder; the vacuum pump valve V4 is connected with the vacuum pump; and the pressure reducing valve is connected with the chromatographic analyzer. In the system, helium gas blowing and vacuumizing replacement are performed repeatedly, so that rapid gas replacement of the sampling system is realized. The chromatographic analyzing and sampling system has the characteristics of short replacing time and low sampling loss, and is suitable for the technical field of chromatographic analyzing and sampling applications to bottling requiring frequent replacement of samples, multipoint online sampling and product delivery inspection for gas samples such as silane and the like with pyrophorisity, high toxicity and high corrosion.
Description
Technical field
The present invention relates to a kind of stratographic analysis sampling system that is used for silane sample.Be used for the silane sample stratographic analysis sampling of frequent change specimen specifically, adopt the mode of helium purge, vacuum displacement reach quick, pollution-free, system not with the silane sample stratographic analysis sampling system of characteristics such as air contacts.
Background technology
Silane belongs to a kind of of electronic gas, and its character is special, when its with after air contacts, spontaneous combustion and produce SiO 2 powder.So the stratographic analysis sampling of silane is different from the analytical sampling of common gases, need avoid sample directly or indirectly to contact with air, the sample pollution-free, representative silane sample gets into chromatographic analysis system.
Usually, electronics industry and online detection are used for the sampling of silane sample, can adopt helium purge after, long-time with silane sample, big flow ground purges sampling line to carry out stratographic analysis and takes a sample.But when needing the frequent change sample, it is long just to expose sample time, and the sample wastage is big, owing to need long silane discharging, causes the also big shortcoming of environmental pollution simultaneously.
Summary of the invention
Problem to be solved by this invention is, overcomes the defective that prior art exists, and has proposed a kind of bottled silane sample stratographic analysis sampling system, has time swap weak point, the little characteristics of sample sampling loss.
The bottled silane sample stratographic analysis of the present invention sampling system comprises chromatograph, helium steel cylinder, calibrating gas steel cylinder, vacuum pump, helium valve V1, standard air valve V2, retaining valve, sample gas valve V3, reduction valve, vacuum pump valve V4, emptying valve V5; It is characterized in that: retaining valve, sample gas valve V3, vacuum pump valve V4, atmospheric valve V5 are connected in parallel on the reduction valve, and helium valve V1 and standard air valve V2 are connected in parallel on the retaining valve; Helium valve V1 connects the helium steel cylinder, and standard air valve V2 connects the calibrating gas steel cylinder, and vacuum pump valve V4 connects vacuum pump, and reduction valve connects chromatograph.
The present invention; Take helium purge, vacuumize displacement, again helium purge, vacuumize the repeatable operation of displacement again; Reach the quick displacement of sampling system; Native system has that time swap is short, the little characteristics of sample sampling loss, has solved the deficiency of prior art, is applicable to that bottled, the online sampling of multiple spot that needs the frequent change sample, the silane of product export check etc. have pyrophorisity, toxicity and reach the strong gaseous sample stratographic analysis sampling applied technical field of corrosivity greatly.
Description of drawings
Fig. 1 is the bottled silane sample stratographic analysis of a present invention sampling system pipeline structure synoptic diagram.
Embodiment
As shown in Figure 1; Bottled silane sample stratographic analysis sampling system comprises chromatograph 3, helium steel cylinder, calibrating gas steel cylinder, vacuum pump, helium valve V1, standard air valve V2, retaining valve 1, sample gas valve V3, reduction valve 2, vacuum pump valve V4, atmospheric valve V5.Retaining valve, sample gas valve V3, vacuum pump valve V4, emptying valve V5 are connected in parallel on the reduction valve, and helium valve V1 and standard air valve V2 are connected in parallel on the retaining valve; Helium valve V1 connects the helium steel cylinder, and standard air valve V2 connects calibrating gas (silane) steel cylinder, and vacuum pump valve V4 connects vacuum pump, and reduction valve connects chromatograph.
The sampling system pipeline adopts 1/8 inch 316L EP grade stainless steel pressure piping, bite type connected mode.Vacuum pump system, exhaust emissions system install the nitrogen dilution bleeder line additional, and chromatogram sampling exhaust emissions system installs the nitrogen dilution bleeder line equally additional.
It is qualified before native system uses first through vacuum and high pressure leak test.The silane sample gas cylinder is connected on the sample gas valve V3, checks all valves, comprise that the steel cylinder valve is in closed condition.
One, sampling operation
1, closes all valves, comprise reduction valve.Open vacuum-pump power supply, the observing system tensimeter, system does not have under the pressure condition, opens vacuum pump valve V4, helium valve V1 and sample gas valve V3 successively.
2, vacuumize 2min after, close vacuum pump valve V4.Open helium valve V1, slowly regulate V1 to the system pressure 2MPa, close helium valve V1, open atmospheric valve V5, bleed off system's helium.Close atmospheric valve V5, open vacuum pump valve V4 once more, system is vacuumized 2min.
3, repeating step 1～2, carry out 3～5 times after, system charges into helium, more than the pressure 2MPa, closes helium valve V1.Open emptying valve V5, the emptying helium is also closed V5.Open vacuum valve V4, after system vacuumizes 2min, close vacuum pump valve V4.
4, slowly open the silane gas cylinder valve, charge into silane sample gas in the system, the system pressure table shows the silane sample pressure of the inside of a bottle.Regulate reduction valve clockwise, observe sample flow meter on the chromatograph, the adjusting flow is 100ml/min, sweeps sampling pipe and quantity tube 3～5min with the silane sample air-blowing.
5, start the chromatograph sampling system, begin to analyze.
Annotate: when demarcating chromatograph,, replace V3 to operate with standard air valve V2 with above-mentioned 1～5 step.
Two, change sample
1, closes the silane cylinder valve, slowly open atmospheric valve V5, silane emptying under nitrogen protection.
2, close atmospheric valve V5, open helium valve V1, charge into the helium of 3～4MPa.Open atmospheric valve V5 again.
3, repeating step 1～2 is operated 3～5 times.Close atmospheric valve V5, open vacuum pump valve V4, close vacuum pump valve V4 after system is vacuumized 2～3min.System charges into the helium of 3～4MPa again, slowly unclamps silane gas cylinder joint, and the protection of taking care is no abnormal, unloads the silane gas cylinder.
4, change new silane sample gas cylinder.System charges into high-pressure helium leak detection (soap lye or helium leak check appearance), hunt leak qualified after, open atmospheric valve, the system of draining helium.
5, open vacuum pump valve V4, system is vacuumized 2～3min, close vacuum pump valve V4, open helium valve V1, system charges into 3～4MPa helium, opens atmospheric valve V5 emptying system pressure again.Open vacuum pump valve V4 once more, close vacuum valve V4 after vacuumizing 2～3min.
6, after repeating step 5 is operated 3～5 times, slowly open the silane gas cylinder valve, after the system pressure balance, slowly open reduction valve and purge sampling line.
7, other steps can be referring to one, sampling operation step 4～5.
Claims (1)
1. a bottled silane sample stratographic analysis sampling system comprises chromatograph, helium steel cylinder, calibrating gas steel cylinder, vacuum pump, helium valve V1, standard air valve V2, retaining valve, sample gas valve V3, reduction valve, vacuum pump valve V4, emptying valve V5; It is characterized in that: retaining valve, sample gas valve V3, vacuum pump valve V4, atmospheric valve V5 are connected in parallel on the reduction valve, and helium valve V1 and standard air valve V2 are connected in parallel on the retaining valve; Helium valve V1 connects the helium steel cylinder, and standard air valve V2 connects the calibrating gas steel cylinder, and vacuum pump valve V4 connects vacuum pump, and reduction valve connects chromatograph.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101116345A CN102620957A (en) | 2012-04-17 | 2012-04-17 | Chromatographic analyzing and sampling system for bottled silane sample |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101116345A CN102620957A (en) | 2012-04-17 | 2012-04-17 | Chromatographic analyzing and sampling system for bottled silane sample |
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| CN102620957A true CN102620957A (en) | 2012-08-01 |
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| CN2012101116345A Pending CN102620957A (en) | 2012-04-17 | 2012-04-17 | Chromatographic analyzing and sampling system for bottled silane sample |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645269A (en) * | 2013-11-19 | 2014-03-19 | 苏州丹百利电子材料有限公司 | Analysis method and apparatus of ultra pure arsine |
| CN103852352A (en) * | 2012-12-06 | 2014-06-11 | 中国人民解放军空军航空医学研究所 | Gas production negative-pressure equipment and gas detection system |
| CN104062153A (en) * | 2014-06-17 | 2014-09-24 | 中国船舶重工集团公司第七一八研究所 | Blowing sampling system and blowing sampling method for analysis of content of impurities gas |
| CN104155404A (en) * | 2014-09-03 | 2014-11-19 | 中国科学院广州地球化学研究所 | Atmosphere methane and carbon monoxide analysis system and method |
| CN104181015A (en) * | 2014-08-22 | 2014-12-03 | 上海延锋江森座椅有限公司 | Novel automatic sampling system used in bag method |
| CN104316625A (en) * | 2014-11-06 | 2015-01-28 | 上海华爱色谱分析技术有限公司 | Sampling system for silane chromatographic analysis |
| CN105738549A (en) * | 2015-01-06 | 2016-07-06 | 南京特种气体厂有限公司 | Ammonia gas monitoring alarming and switching method based on chromatographic analysis |
| CN105784863A (en) * | 2016-03-09 | 2016-07-20 | 广东华特气体股份有限公司 | Toxic or harmful gas analysis system and using method |
| CN106124790A (en) * | 2016-08-30 | 2016-11-16 | 吴江梅塞尔工业气体有限公司 | The sampler of a kind of toxic gas analysis and simple sampling method |
| CN106596823A (en) * | 2016-12-22 | 2017-04-26 | 邯郸派瑞节能控制技术有限公司 | Gas sampling and analyzing device and method |
| CN106769245A (en) * | 2016-12-22 | 2017-05-31 | 安徽亚格盛电子新材料有限公司 | Pyrophorisity liquid gas sample obturator |
| CN110187017A (en) * | 2019-05-09 | 2019-08-30 | 中触媒新材料股份有限公司 | A kind of propylene oxide on-line period device and method |
| CN111141458A (en) * | 2019-12-25 | 2020-05-12 | 兰州空间技术物理研究所 | Helium recovery device and recovery method for leak detection of high-pressure gas cylinder |
| CN112629951A (en) * | 2020-12-14 | 2021-04-09 | 内蒙古兴洋科技有限公司 | High-purity silane metal ion detection sampling device |
| CN113970064A (en) * | 2021-10-09 | 2022-01-25 | 全椒亚格泰电子新材料科技有限公司 | Treatment device for residual disilane gas cylinders |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103852352A (en) * | 2012-12-06 | 2014-06-11 | 中国人民解放军空军航空医学研究所 | Gas production negative-pressure equipment and gas detection system |
| CN103645269A (en) * | 2013-11-19 | 2014-03-19 | 苏州丹百利电子材料有限公司 | Analysis method and apparatus of ultra pure arsine |
| CN104062153A (en) * | 2014-06-17 | 2014-09-24 | 中国船舶重工集团公司第七一八研究所 | Blowing sampling system and blowing sampling method for analysis of content of impurities gas |
| CN104181015A (en) * | 2014-08-22 | 2014-12-03 | 上海延锋江森座椅有限公司 | Novel automatic sampling system used in bag method |
| CN104181015B (en) * | 2014-08-22 | 2016-06-29 | 上海延锋江森座椅有限公司 | A kind of novel sack method adopts system automatically |
| CN104155404A (en) * | 2014-09-03 | 2014-11-19 | 中国科学院广州地球化学研究所 | Atmosphere methane and carbon monoxide analysis system and method |
| CN104155404B (en) * | 2014-09-03 | 2016-01-27 | 中国科学院广州地球化学研究所 | Atmospheric methane and carbon monoxide analytic system and method |
| CN104316625A (en) * | 2014-11-06 | 2015-01-28 | 上海华爱色谱分析技术有限公司 | Sampling system for silane chromatographic analysis |
| CN105738549A (en) * | 2015-01-06 | 2016-07-06 | 南京特种气体厂有限公司 | Ammonia gas monitoring alarming and switching method based on chromatographic analysis |
| CN105738549B (en) * | 2015-01-06 | 2018-04-17 | 南京特种气体厂股份有限公司 | A kind of ammonia monitoring, alarming and switching method based on chromatography |
| CN105784863A (en) * | 2016-03-09 | 2016-07-20 | 广东华特气体股份有限公司 | Toxic or harmful gas analysis system and using method |
| CN106124790A (en) * | 2016-08-30 | 2016-11-16 | 吴江梅塞尔工业气体有限公司 | The sampler of a kind of toxic gas analysis and simple sampling method |
| CN106596823A (en) * | 2016-12-22 | 2017-04-26 | 邯郸派瑞节能控制技术有限公司 | Gas sampling and analyzing device and method |
| CN106769245A (en) * | 2016-12-22 | 2017-05-31 | 安徽亚格盛电子新材料有限公司 | Pyrophorisity liquid gas sample obturator |
| CN110187017A (en) * | 2019-05-09 | 2019-08-30 | 中触媒新材料股份有限公司 | A kind of propylene oxide on-line period device and method |
| CN111141458A (en) * | 2019-12-25 | 2020-05-12 | 兰州空间技术物理研究所 | Helium recovery device and recovery method for leak detection of high-pressure gas cylinder |
| CN111141458B (en) * | 2019-12-25 | 2022-01-21 | 兰州空间技术物理研究所 | Helium recovery device and recovery method for leak detection of high-pressure gas cylinder |
| CN112629951A (en) * | 2020-12-14 | 2021-04-09 | 内蒙古兴洋科技有限公司 | High-purity silane metal ion detection sampling device |
| CN113970064A (en) * | 2021-10-09 | 2022-01-25 | 全椒亚格泰电子新材料科技有限公司 | Treatment device for residual disilane gas cylinders |
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Application publication date: 20120801 |