CN109580816A - It is a kind of for analyzing the gas chromatographic column of benzene homologues - Google Patents

It is a kind of for analyzing the gas chromatographic column of benzene homologues Download PDF

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Publication number
CN109580816A
CN109580816A CN201811508923.2A CN201811508923A CN109580816A CN 109580816 A CN109580816 A CN 109580816A CN 201811508923 A CN201811508923 A CN 201811508923A CN 109580816 A CN109580816 A CN 109580816A
Authority
CN
China
Prior art keywords
column
chromatographic column
benzene homologues
tube
analyzing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811508923.2A
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Chinese (zh)
Inventor
常诚
张青
张佳
杨辰轩
李仲琴
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LANZHOU ZKAT ANALYSIS TECHNOLOGY Co Ltd
Original Assignee
LANZHOU ZKAT ANALYSIS TECHNOLOGY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LANZHOU ZKAT ANALYSIS TECHNOLOGY Co Ltd filed Critical LANZHOU ZKAT ANALYSIS TECHNOLOGY Co Ltd
Priority to CN201811508923.2A priority Critical patent/CN109580816A/en
Publication of CN109580816A publication Critical patent/CN109580816A/en
Pending legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/065Preparation using different phases to separate parts of sample

Abstract

The invention discloses a kind of for analyzing the gas chromatographic column of benzene homologues, including gc column tube, carrier and fixer, the gc column tube column length is 1.5m, internal diameter 3mm, the carrier is the Chromosorb WAW DMCS of 80-100 mesh, the fixed liquid proportional is 3.7% bentonite and 2.3% dinonyl phthalate, and the gc column tube is stainless steel tube.Benzene homologues are efficiently separated compared with prior art, the present invention can be realized in the case where chromatographic column is shorter, it is convenient, fast, reliable.

Description

It is a kind of for analyzing the gas chromatographic column of benzene homologues
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a kind of for analyzing the gas chromatographic column of benzene homologues.
Background technique
Gas chromatographic column petroleum, chemical industry, biochemistry, medical and health, in terms of application it is very wide, in gas phase In chromatography, whether component to be measured, which can efficiently separate, depends primarily on stationary phase, and stationary phase has with each component in sample Different affinity, when carrier gas with sample continually by chromatographic column when, the big component of affinity mobile speed in the chromatography column Degree is slow, and the small then movement of affinity is fast, and the separating property for being commonly used in the chromatographic column of analysis benzene homologues at present is general, chromatographic column Longer, amount of filler is more, and appearance time is longer.
Summary of the invention
It is an object of the invention to: to solve the above problems, providing a kind of for analyzing the gas chromatographic column of benzene homologues, make Obtaining fixer has better choice separating property to benzene homologues, and chromatographic column specification is shorter, and amount of filler is less, and appearance time is more Fastly.
The technical solution adopted by the invention is as follows:
It is a kind of for analyzing the gas chromatographic column of benzene homologues, including gc column tube, carrier and fixer, the gc column tube Column length is 1.5m, internal diameter 3mm, and the carrier is the Chromosorb WAW DMCS of 80-100 mesh, and the fixed liquid proportional is 3.7% bentonite and 2.3% dinonyl phthalate.
Preferably, the gc column tube is stainless steel tube.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
By optimizing fixed liquid proportional, so that fixer has better choice separating property to benzene homologues.In chromatographic column Chromatographic column specification can be made shorter in production, amount of filler is less.Production cost is not only saved, in analysis detection, because of column Length shortens, and can also obtain cracking appearance time, provides more convenient, quick, reliable chromatographic column product for detection work.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this A little attached drawings obtain other relevant attached drawings.
Fig. 1 is spectrogram of the To Determine Benzene Standard Samples Using Jing Guo chromatography post separation of the invention;
Fig. 2 is To Determine Benzene Standard Samples Using by the spectrogram of the chromatographic column prepared according to national standards;
Fig. 3 is To Determine Benzene Standard Samples Using by the spectrogram of the lengthening chromatographic column prepared according to national standards.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not For limiting the present invention, i.e., described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is logical The component for the embodiment of the present invention being often described and illustrated herein in the accompanying drawings can be arranged and be designed with a variety of different configurations.
Therefore, the detailed description of the embodiment of the present invention provided in the accompanying drawings is not intended to limit below claimed The scope of the present invention, but be merely representative of selected embodiment of the invention.Based on the embodiment of the present invention, those skilled in the art Member's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
It should be noted that the relational terms of term " first " and " second " or the like be used merely to an entity or Operation is distinguished with another entity or operation, and without necessarily requiring or implying between these entities or operation, there are any This actual relationship or sequence.Moreover, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that including described There is also other identical elements in the process, method, article or equipment of element.
General to solve the current chromatographic column separating property for being commonly used in analysis benzene homologues, chromatographic column is longer, and filler is used Measure more, the longer problem of appearance time, the present invention provides a kind of for analyzing the gas chromatographic column of benzene homologues, including chromatographic column Pipe, carrier and fixer, the gc column tube column length is 1.5m, internal diameter 3mm, and the carrier is 80-100 purpose Chromosorb WAW DMCS, the fixed liquid proportional are 3.7% bentonite and 2.3% dinonyl phthalate. The gc column tube is stainless steel tube.
In order to which the present invention is further explained, below in conjunction with specific Application Example to feature and performance of the invention make into The detailed description of one step.
Embodiment 1
To Determine Benzene Standard Samples Using is detected using chromatogram column analysis of the invention.
One, equipment and equipment
Gas chromatograph, ageing device, vacuum pump (gas velocity rate: 8L/S), spillikin, triangular funnel, thin metal rod (are used for column two End plug mineral wool use), beaker (100ml), triangular flask (100ml), medicine spoon;Reagent: methylene chloride, acetone, pentane, benzene are (molten Solution be analysis it is pure), To Determine Benzene Standard Samples Using.
Two, operating procedure
1. column tube
Column length is 1.5m, and internal diameter is the stainless steel gc column tube of 3mm.
2. the selection of carrier
Chromosorb WAW DMCS 80-100 mesh.
3. the preparation of fixer
3.7% bentonite and 2.3% dinonyl phthalate (DNP).
4. filling column
Distance pole first understands sample introduction end and detector end before dress column, and a little glass is filled in the detector end of void column, deep Degree is about 1cm or so, starts vacuum pump, a little carrier is added in funnel, about 1ml or so is added every time, and slowly tap column The different location of pipe keeps carrier filling close.Finally make the one of connection injection port to bring out 4-5cm, fills in a little glass, glass Tampon is filled out closely to prevent carrier leakage, and the metal label for performing label extension is carried out aging afterwards on a column.
5. aging
Ageing device program is set, rises to 150 DEG C with 5 DEG C/min journey, aging chromatographic column 10h.
6. chromatographic column is evaluated
Fixer: 3.7% bentonite and 2.3% dinonyl phthalate (DNP).
Chromatographic column specification: 1.5m × 3mm stainless stee l packed column.
Chromatographic column evaluation condition: column temperature: 75 DEG C, vapourizing temperature: 150 DEG C, detector temperature: 150 DEG C.
Spectrogram of the To Determine Benzene Standard Samples Using Jing Guo chromatography post separation of the invention is as shown in Figure 1, data result such as 1 institute of table Show, chromatographic column of the invention is by optimizing fixed liquid proportional, so that fixer has better choice separating property to benzene homologues. Chromatographic column specification can be made shorter in chromatographic column production, amount of filler is less.Production cost is not only saved, in analysis detection In, because column length shortens, cracking appearance time can also be obtained, provides more convenient, quick, reliable color for detection work Compose column product.
The experimental data table of 1 embodiment 1 of table
Embodiment 2
To Determine Benzene Standard Samples Using is detected using the chromatogram column analysis of national standard preparation.
One, equipment and equipment
The equipment and equipment that embodiment 2 uses are identical as the equipment and equipment that embodiment 1 uses.
Two, operating procedure
1. column tube
Column length is 2m, and internal diameter is the stainless steel gc column tube of 3mm.
2. the selection of carrier
Chromosorb G DMCS 80-100 mesh.
3. the preparation of fixer
2.5% bentonite and 2.5% dinonyl phthalate (DNP).
4. filling column
It is identical as the dress column process of embodiment 1 to fill column process.
5. aging
Ageing device program is set, rises to 150 DEG C with 5 DEG C/min journey, aging chromatographic column 10h.
6. chromatographic column is evaluated
Fixer: 2.5% bentonite and 2.5% dinonyl phthalate (DNP).
Chromatographic column specification: 2m × 3mm stainless stee l packed column.
Chromatographic column evaluation condition: column temperature: 75 DEG C, vapourizing temperature: 150 DEG C, detector temperature: 150 DEG C.
To Determine Benzene Standard Samples Using passes through the spectrogram using the chromatography post separation of national standard preparation as shown in Fig. 2, from Fig. 2 As can be seen that cannot be effectively separated according to chromatographic column prepared by national standard to sample, to reach sample separating effect, by column length 3.5m is changed to further to test.
Embodiment 3
Column's length prepared by national standard is lengthened to 3.5m, to analysis detection To Determine Benzene Standard Samples Using.
One, equipment and equipment
The equipment and equipment that embodiment 3 uses are identical as the equipment and equipment that embodiment 2 uses.
Two, operating procedure
1. column tube
Column length is 3.5m, and internal diameter is the stainless steel gc column tube of 3mm.
2. the selection of carrier
Chromosorb G DMCS 80-100 mesh.
3. the preparation of fixer
2.5% bentonite and 2.5% dinonyl phthalate (DNP).
4. filling column
It is identical as the dress column process of embodiment 2 to fill column process.
5. aging
Ageing device program is set, rises to 150 DEG C with 5 DEG C/min journey, aging chromatographic column 10h.
6. chromatographic column is evaluated
Fixer: 2.5% bentonite and 2.5% dinonyl phthalate (DNP).
Chromatographic column specification: 3.5m × 3mm stainless stee l packed column.
Chromatographic column evaluation condition: column temperature: 75 DEG C, vapourizing temperature: 150 DEG C, detector temperature: 150 DEG C.
To Determine Benzene Standard Samples Using passes through the spectrogram using the lengthening chromatography post separation of national standard preparation as shown in figure 3, number According to as shown in table 2, from experimental result as can be seen that after chromatographic column is lengthened to 3.5m, chromatographic column can effectively divide sample From.
The experimental data table of 2 embodiment 3 of table
From the testing result of embodiment 1, embodiment 2 and embodiment 3, it is apparent that the color prepared using national standard Spectrum column is not effectively separated To Determine Benzene Standard Samples Using, and needing to increase to column length after 3.5m could be by benzene homologues standard Sample is effectively separated, and needs the chromatographic column of 1.5m can be effective by To Determine Benzene Standard Samples Using using chromatographic column of the invention Ground separation.The fixation liquid proportional optimized with prior art ratio, the present invention, so that fixer has better choice to benzene homologues Separating property can make chromatographic column specification shorter in chromatographic column production, and amount of filler is less, not only save production cost, In analysis detection, because column length shortens, cracking appearance time can also be obtained, for detection work provide it is more convenient, quick, Reliable chromatographic column product.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (2)

1. a kind of for analyzing the gas chromatographic column of benzene homologues, including gc column tube, carrier and fixer, it is characterised in that: institute State gc column tube column length be 1.5m, internal diameter 3mm, the carrier is the Chromosorb WAW DMCS of 80-100 mesh, described solid Determining liquid proportional is 3.7% bentonite and 2.3% dinonyl phthalate.
2. as described in claim 1 a kind of for analyzing the gas chromatographic column of benzene homologues, it is characterised in that: the gc column tube For stainless steel tube.
CN201811508923.2A 2018-12-11 2018-12-11 It is a kind of for analyzing the gas chromatographic column of benzene homologues Pending CN109580816A (en)

Priority Applications (1)

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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811508923.2A CN109580816A (en) 2018-12-11 2018-12-11 It is a kind of for analyzing the gas chromatographic column of benzene homologues

Publications (1)

Publication Number Publication Date
CN109580816A true CN109580816A (en) 2019-04-05

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Application publication date: 20190405