CN202929002U - Molecular sieve packed column based on high-purity and ultrahigh-purity gas trace impurity component separation - Google Patents
Molecular sieve packed column based on high-purity and ultrahigh-purity gas trace impurity component separation Download PDFInfo
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- CN202929002U CN202929002U CN 201220547348 CN201220547348U CN202929002U CN 202929002 U CN202929002 U CN 202929002U CN 201220547348 CN201220547348 CN 201220547348 CN 201220547348 U CN201220547348 U CN 201220547348U CN 202929002 U CN202929002 U CN 202929002U
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Abstract
The utility model relates to a molecular sieve packed column for analyzing of a gas chromatograph, and discloses a molecular sieve packed column based on high-purity and ultrahigh-purity gas trace impurity component separation. The molecular sieve packed column comprises a stainless steel pipe body (2), a chromatographing supporter (4) and silanized glass fibers (3); the silanized glass fibers (3) are placed at two ends of an inner chamber (5) of the stainless steel pipe body (2); and the chromatographing supporter (4) is arranged between the silanized glass fibers (3) at the two ends. The molecular sieve packed column based on the high-purity and ultrahigh-purity gas trace impurity component separation is reasonable and practical in structure and has the advantages of being high in column efficiency, excellent in separation characteristic, low in background value of a chromatographic column base flow, and low in baseline noise.
Description
Technical field
The utility model relates to gas chromatograph analysis molecular sieve packed column, has related in particular to a kind of molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component.
Background technology
Existing gas chromatographic analysis 5A molecular sieve chromatography post commonly used is generally commonly used the common stainless steel pipe and fills commercially available 60-80 order 5A molecular sieve through aging formation, is mainly used in (X%) number percent and separates with the component of hundreds of to several thousand PPM content; Belong to conventional component isolation technics; High-purity gas industry fast development along with China, high-purity gas, ultra-pure gaseous impurities analysis adopt the gas chromatograph of outfit helium ionization detector in the widespread use of industry, people are more and more higher to the requirement that is used for trace detection accuracy, stalling characteristic and express-analysis of instrument, and existing conventional 5A chromatographic column has been to satisfy the requirement of the trace impurity separation of Analysis of Gases of High Purity fully.And fixedly the phase body is super pure to require 5A for high-purity gas, the separatory 5A molecular sieve column of ultra-pure gaseous impurities component, absorption without trace water, airfree absorption is without the absorption of harmful speciality, without features such as the intrapore diffusion absorption of the 5A of trickle smalls.
Summary of the invention
The requirement that the utility model separates for the trace impurity that can't satisfy Analysis of Gases of High Purity in prior art, provide a kind of helium ionized gas phase chromatographic instrument that can effectively solve to the basic demand that high-purity, ultra-pure gas trace impurity component separates, can also effectively separate hydrogen and neon component; Suitable high-purity, ultra-pure gas trace impurity separates, and has rational in infrastructurely and practical, has the advantages such as the post effect is high, stalling characteristic good, chromatographic column base flow background values is low, and baseline noise is little.
In order to solve the problems of the technologies described above, the utility model is solved by following technical proposals:
Molecular sieve packed column based on high-purity, ultra-pure gas trace impurity component separation, comprise stainless steel body, stratographic analysis carrier and silanized glass fiber, the two ends of the tube cavity of described stainless steel body are equipped with the silanized glass fiber, and stratographic analysis is arranged between the silanized glass fiber at two ends with carrier.Stainless steel body, stratographic analysis be with carrier and silanized glass fiber, at the two ends of the inner chamber of body, the silanized glass fiber is installed, and the 5A stratographic analysis carrier that can be blocked by glass fibre is arranged in the inner chamber of the body between the silanized glass fiber.The 5A molecular sieve namely refers to the molecular sieve of 5A pore size.
As preferably, described stratographic analysis carrier is that two ends are silylated the 5A stratographic analysis carrier that glass fibre blocks.Molecular sieve packed column in the utility model is the 5A molecular sieve packed column, and the 5A stratographic analysis is 5A molecular sieve carrier with carrier, and its technology of preparing scheme realizes by following measures: choose the high-quality PSA type 5A molecular screen material of selling on the market; Sieve through 60-80 order stainless steel sift again after smalls, obtain a certain amount of 60-80 order typing molecular sieve; Then activate new 5A carrier at resistance furnace with certain (T=a ℃, the material of a value depending on 5A is separately decided with reference to the absorption entropy feature of O2 N2 CH4 CO) roasting temperature; Aging and eliminate material on the 5A that is attracted to smalls, purify the 5A molecular sieve carrier that makes new advances; Be 5A substance active state, to complete the preparation to new 5A molecular sieve carrier.
5A molecular sieve packed column technology of preparing scheme realizes by following measures: the gas chromatographic analysis that a kind of applicable high-purity, ultra-pure gas trace impurity component separates comprises 316L stainless steel body, stratographic analysis 5A molecular sieve carrier, high-air-tightness metal ferrule joint with 5A molecular sieve special filling post; Two ends at the inner chamber of body are equipped with the shutoff of silanized glass fiber, and the used in chromatograph 5A molecular sieve carrier that can be blocked by glass fibre is arranged in the inner chamber of the long volume body between the silanized glass fiber.
As preferably, described stainless steel tube wall diameter is 1/8th inches, and stainless steel body inner diameter is 2.1 millimeters.
As preferably, described stainless steel body is inboard wall of tube body light and seamless 316L stainless steel.
As preferably, described stainless-steel tube body length is 2-3 rice, and body adopts spiral coiling typing.According to actual operating position, but stainless steel body pitch of the laps shape, be convenient to be arranged in instrument or the aluminium calandria on.
As preferably, the two ends of described stainless steel body are respectively equipped with high-air-tightness metal ferrule joint.
As preferably, the stratographic analysis carrier of filling in described tube cavity is 60 to 80 purpose 5A molecular sieve chromatography analysis carriers.Above-mentioned stratographic analysis also can be fixedly phase of 80-100 purpose smalls 5A molecular sieve with carrier.According to the actual needs of stratographic analysis, stratographic analysis can be the 6.9-10.35 milliliter with the packing volume of 5A molecular sieve carrier.
The utility model is owing to having adopted above technical scheme, and have significant technique effect: the utility model is rational in infrastructure and practical, has the advantages such as the post effect is high, stalling characteristic good, chromatographic column base flow background values is low, and baseline noise is little.
Description of drawings
Fig. 1 is the one-piece construction schematic diagram of the utility model embodiment 1.
Fig. 2 is the sectional view of stainless steel body in Fig. 1.
Fig. 3 is 5A molecular sieve separating effect collection of illustrative plates.
The toponym that in above accompanying drawing, each number designation refers to is as follows: wherein 1-high-air-tightness metal ferrule joint, 2-stainless steel body, 3-silanized glass fiber, 4-stratographic analysis are with carrier, 5-body, 6-tube cavity.
Embodiment
Below in conjunction with accompanying drawing 1 to Fig. 3 and embodiment, the utility model is described in further detail:
Molecular sieve packed column based on high-purity, ultra-pure gas trace impurity component separation, as shown in Figure 1 to Figure 3, comprise stainless steel body 2, stratographic analysis carrier 4 and silanized glass fiber 3, the two ends of the tube cavity 6 of described stainless steel body 2 are equipped with silanized glass fiber 3, and stratographic analysis is arranged between the silanized glass fiber 3 at two ends with carrier 4.
Stratographic analysis is silylated for two ends the 5A stratographic analysis carrier that glass fibre 3 blocks with carrier 4.Stainless steel body 2 outer diameters are 1/8th inches, and stainless steel body 2 inner diameters are 2.1 millimeters.
The stratographic analysis of tube cavity 6 interior fillings is 60 to 80 purpose 5A molecular sieve chromatography analysis carriers with carrier 4.
The standby use procedure of this practical system is as follows:
(I) choose on the market sell high-quality PSA type 5A molecular screen material; After smalls, then sieve through 60-80 order stainless steel sift, obtain a certain amount of 60-80 order typing molecular sieve; Then resistance furnace with certain (T=a ℃, the material of a value depending on 5A is separately decided with reference to the absorption entropy feature of O2, N2, CH4, CO) high-temperature under the new 5A carrier of calcination activation; Aging and eliminate material on the 5A that is attracted to smalls, purify the 5A molecular sieve carrier that makes new advances; Be 5A substance active state, to complete the preparation to new 5A molecular sieve carrier.
(II) is interior according to analyzing 60 to the 80 purpose 5A molecular sieve chromatography analyses carrier 4 that requires filling to prepare at the tube cavity 6 of body 5, during filling, the stainless steel body must first be coiled into circle, one end with silanized glass fiber 3 with the sealing of column jecket mouth, then add one section same specification bumper post in case carrier go out.With body 5 one termination vacuum pumps, another termination pressure vessel, slowly be depressed into a stationary value and keep before lifting column in filling process, be loaded into uniformly 5A molecular sieve chromatography noted earlier analysis in the tube cavity 6 of body 5 with carrier under the effect of vacuum pump negative-pressure sucking, after installing, unload lower tube body 5, other one is also sealed with silanized glass fiber 3.During filling, guarantee that chromatographic grade analysis carrier 4 is uniformly distributed in the tube cavity 6 of whole body 5, and degree of tightness is moderate.Can not beat body 5 by gravity in whole vacuum pump filling process, cause column performance to degenerate in order to avoid cause the 5A stratographic analysis to pulverize with the carrier mechanicalness; And it is fast that whole filling process time is wanted.To prevent that vacuum pump from extracting the 5A molecular sieve and too much absorbed air for a long time.
5A molecular sieve chromatography pillar after (III) filled in is wanted aging good could the use, and aging is for the molecular sieve in purification pipe intracoelomic cavity 6.Also can make simultaneously the 5A molecular sieve activate into fixedly phase of 5A in body 5 interior location.Aging method adopts high-purity inertia N2 gas flow sweeping method, body 5 entrances are connected with the instrument injection port, outlet does not connect detecting device, logical N2 carrier gas is with the flow of 30ml/min, it is specific (T=b ℃ in post case temperature, b value depending on 5A molecular sieve are for separating of the degree of separation of Ne, H2, O2 (Ar), N2, CH4, CO) under column temperature aging some hours, until 5A fixing location mutually is shaped.
(IV) preparation load and aging after good high-purity, the special-purpose 5A molecular sieve of ultra high purity gas analysis pillar must be through the post effect assessment of performance of helium ion gas chromatography, whether chromatographic column subbase stream satisfies the requirement of the low base flow that high-purity gas analyzes; Concrete operations are such: on instrument, high-purity helium of (7N) after logical purification the, constant temperature also purge and purify the chromatogram pillar with high-air-tightness metal ferrule jiont treatment 5A chromatographic column; Column temperature is equal to T=b ℃, repetition test until base flow drop to below 50-70mv, and without larger noise<30 uv; Then make the gas sample introduction gas of spirit with helium, test 5A molecular sieve pillar when column temperature 60 or 70 ℃ to the separating power of Ne H2 O2 (Ar) N2 CH4 CO.Following Fig. 3 is the 5A molecular sieve separating effect collection of illustrative plates of stand the test.
In a word, the above is only preferred embodiment of the present utility model, and all equalizations of doing according to the utility model claim change and modify, and all should belong to the covering scope of the utility model patent.
Claims (7)
1. the molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component, comprise stainless steel body (2), stratographic analysis carrier (4) and silanized glass fiber (3), it is characterized in that: the two ends of the tube cavity (6) of described stainless steel body (2) are equipped with silanized glass fiber (3), and stratographic analysis is arranged between the silanized glass fiber (3) at two ends with carrier (4).
2. the molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component according to claim 1, it is characterized in that: described stratographic analysis is silylated for two ends the 5A stratographic analysis carrier that glass fibre (3) blocks with carrier (4).
3. the molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component according to claim 1, it is characterized in that: described stainless steel body (2) outer diameter is 1/8th inches, and stainless steel body (2) inner diameter is 2.1 millimeters.
4. the molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component according to claim 1, it is characterized in that: described stainless steel body (2) is inboard wall of tube body light and seamless 316L stainless steel.
5. the molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component according to claim 1, it is characterized in that: described stainless steel body (2) length is 2-3 rice, body adopts spiral coiling typing.
6. the molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component according to claim 1, it is characterized in that: the two ends of described stainless steel body (2) are respectively equipped with high-air-tightness metal ferrule joint (1).
7. the molecular sieve packed column that separates based on high-purity, ultra-pure gas trace impurity component according to claim 1, it is characterized in that: the stratographic analysis of filling in described tube cavity (6) is 60 to 80 purpose 5A molecular sieve chromatography analysis carriers with carrier (4).
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103926343A (en) * | 2014-04-16 | 2014-07-16 | 常州仪盟核芯仪器有限公司 | Application of silica-gel chromatographic column to detection of high-purity gas via gas chromatography |
CN113804535A (en) * | 2020-06-11 | 2021-12-17 | 中国石油大学(北京) | Wellhead dry gas C15-C32 molecular marker enrichment method and device |
-
2012
- 2012-10-24 CN CN 201220547348 patent/CN202929002U/en not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103926343A (en) * | 2014-04-16 | 2014-07-16 | 常州仪盟核芯仪器有限公司 | Application of silica-gel chromatographic column to detection of high-purity gas via gas chromatography |
CN113804535A (en) * | 2020-06-11 | 2021-12-17 | 中国石油大学(北京) | Wellhead dry gas C15-C32 molecular marker enrichment method and device |
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Granted publication date: 20130508 |