CN213875525U - Ion mobility spectrometry's pre-enrichment device - Google Patents

Ion mobility spectrometry's pre-enrichment device Download PDF

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Publication number
CN213875525U
CN213875525U CN202022846182.8U CN202022846182U CN213875525U CN 213875525 U CN213875525 U CN 213875525U CN 202022846182 U CN202022846182 U CN 202022846182U CN 213875525 U CN213875525 U CN 213875525U
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sample
membrane
enrichment
gas
electromagnetic valve
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蒋丹丹
李海洋
赵琨
李杨
厉梅
肖瑶
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Abstract

A pre-enrichment device of ion mobility spectrometry aims at the detection of high-humidity samples in the environment, solves the problems of interference of humidity on target samples and low sensitivity, mainly comprises a membrane separator for dehumidification and a filling column for sample enrichment, wherein the filling column for sample enrichment is an enrichment column filled with one or more than two of carbon black adsorbent, molecularly imprinted polymer adsorbent, metal organic framework compound adsorbent, covalent organic framework compound adsorbent and carbon-based adsorbent. By eliminating the interference of humidity and pre-enriching the sample, the direct photoionization detection of volatile organic compounds and the like in complex environments can be realized, and the detection sensitivity can be improved to the ppbv magnitude.

Description

Ion mobility spectrometry's pre-enrichment device
Technical Field
The utility model belongs to the analytical chemistry instrument field, concretely relates to pre-enrichment device of ion mobility spectrometry to the high wet sample in the environment, solves the problem that humidity disturbs target sample and sensitivity is low.
Background
The ion mobility spectrometry has the advantages of high detection speed, high sensitivity and the like, but for the detection of target compounds in a complex environment, if the pretreatment and enrichment of a sample are not carried out, the high-sensitivity detection is difficult to realize. For this purpose, a series of methods for pre-enrichment of samples were developed.
The invention relates to a gas molecule concentration and enrichment device invented by Zhao Zheng Ying et al, which adopts selective ionization, continuous ion retention and collection, and instantaneous concentrated ion release and neutralization to improve the concentration of molecules to be detected in original low-concentration sample gas, thereby realizing the concentration and enrichment of the gas to be detected.
The invention discloses an on-site on-line continuous collection, enrichment and analysis device for aerosol sample wafers. The impact collector is combined with a thermal analyzer and is used for on-site continuous collection and analysis of samples by a miniaturized portable instrument (such as ion mobility spectrometry, IMS).
Aiming at the situation that the enrichment device is not designed for analyzing a high-humidity sample in actual environment detection, the invention designs the pre-enrichment device of the ion mobility spectrometry, which can perform pre-enrichment detection on Volatile Organic Compounds (VOC) in the environment or exhaled air.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: the method aims at detecting a high-humidity sample in the environment, and solves the problems of interference of humidity on a target sample and low sensitivity.
The pre-enrichment device of the ion mobility spectrometry mainly comprises a membrane separator for dehumidification and a filling column for sample enrichment, wherein the membrane adopted by the membrane separator is a tubular gas separation membrane, a membrane layer gas inlet of the membrane separator is connected with a high-humidity sample gas source, and a membrane layer gas outlet of the membrane separator is connected with a gas inlet of a suction pump; a tube layer gas inlet of the membrane separator is connected with a carrier gas source, a tube layer gas outlet of the membrane separator is connected with a first gas inlet of a two-position three-way electromagnetic valve A, a second gas inlet of the two-position three-way electromagnetic valve A is connected with a purge gas source, a gas outlet of the two-position three-way electromagnetic valve A is connected with an inlet of a sample-enriched filling column, an outlet of the sample-enriched filling column is connected with a gas inlet of a two-position three-way electromagnetic valve B, and a first gas outlet of the two-position three-way electromagnetic valve B is connected with a sample gas inlet of an ion mobility spectrometry; and a second gas outlet of the two-position three-way electromagnetic valve B is emptied.
The membrane adopted by the membrane separator is a tubular polytetrafluoroethylene gas separation membrane.
The packed column for sample enrichment is an enrichment column which takes one or more than two of carbon black adsorbent, molecularly imprinted polymer adsorbent, metal organic framework compound adsorbent, covalent organic framework compound adsorbent and carbon-based adsorbent as fillers.
The specific content comprises the following steps:
a pre-enrichment device of ion mobility spectrometry is divided into automatic sampling and sample introduction processes, wherein a high-humidity sample enters a tubular gas separation membrane through pump sampling, water molecules in the sample are removed in the pump sampling process due to the hydrophobicity of the membrane, a back-flushing sample carrier gas is applied to purge the other side of the tubular membrane, volatile target molecules are purged to enter a sample enrichment filling column through a three-way two-position electromagnetic valve A and are discharged through a three-way two-position electromagnetic valve B due to concentration difference inside and outside the membrane, the three-way two-position electromagnetic valves A and B are switched after enrichment is carried out for a period of time, the enrichment filling column is heated and analyzed, and the purge carrier gas sequentially passes through the three-way two-position electromagnetic valve A, the sample enrichment filling column and the three-way two-position electromagnetic valve B and finally enters the ion mobility spectrometry for detection.
Flow rate range of sample carrier gas: 50-200ml/min, the sampling flow rate of the high-humidity sample is 100-: a carbon black adsorbent.
By eliminating the interference of humidity and pre-enriching the sample, the direct photoionization detection of volatile organic compounds and the like in complex environments can be realized, and the detection sensitivity can be improved to the ppbv magnitude.
Drawings
FIG. 1 is a schematic structural diagram of a pre-enrichment device for ion mobility spectrometry, wherein 1 is a sample carrier gas, 2 is a high-humidity sample, 3 is a sampling pump, 4 is a polytetrafluoroethylene tubular gas separation membrane, 5 is a two-position three- way solenoid valve 1, 6 is a sample enrichment packed column, 7 is a two-position three- way solenoid valve 2, 8 is an ion mobility spectrometry sample inlet;
FIG. 21, ion mobility spectrum of 4-dioxane.
Detailed Description
Example 1
A pre-enriching device for ion mobility spectrometry is composed of membrane separator for dehumidification and packed column for enriching sample. The membrane adopted by the membrane separator is a tubular gas separation membrane, a membrane layer gas inlet of the membrane separator is connected with a high-humidity sample gas source, and a membrane layer gas outlet of the membrane separator is connected with a gas inlet of a suction pump; a tube layer gas inlet of the membrane separator is connected with a carrier gas source, a tube layer gas outlet of the membrane separator is connected with a first gas inlet of a two-position three-way electromagnetic valve A, a second gas inlet of the two-position three-way electromagnetic valve A is connected with a purge gas source, a gas outlet of the two-position three-way electromagnetic valve A is connected with an inlet of a sample-enriched filling column, an outlet of the sample-enriched filling column is connected with a gas inlet of a two-position three-way electromagnetic valve B, and a first gas outlet of the two-position three-way electromagnetic valve B is connected with a sample gas inlet of an ion mobility spectrometry; and a second gas outlet of the two-position three-way electromagnetic valve B is emptied.
The membrane adopted by the membrane separator is a tubular polytetrafluoroethylene gas separation membrane; the packed column for sample enrichment is an enrichment column which takes one or more than two of carbon black adsorbent, molecularly imprinted polymer adsorbent, metal organic framework compound adsorbent, covalent organic framework compound adsorbent and carbon-based adsorbent as fillers.
The operation process is divided into automatic sampling and sample introduction processes, firstly, high-humidity 1, 4-dioxane enters a tubular porous hydrophobic membrane of polytetrafluoroethylene through pumping sampling, because of the hydrophobicity of the membrane, water molecules in the sample are removed in the process of pumping and sampling, and one path of back-blown sample carrier gas is additionally applied to purge the other side of the tubular membrane, due to the concentration difference between the inside and the outside of the membrane, volatile target molecules are swept and enter the sample enrichment packed column through the three-way two-position electromagnetic valve A, and is discharged through a three-way two-position electromagnetic valve B, after being enriched for a period of time, the three-way two-position electromagnetic valve A and the three-way two-position electromagnetic valve B are switched, meanwhile, the enrichment packed column is heated and analyzed, the purging carrier gas sequentially passes through the three-way two-position electromagnetic valve A, the sample enrichment packed column and the three-way two-position electromagnetic valve B, and finally enters the ion mobility spectrometry for detection, and the ion mobility spectrometry is shown in figure 2.
Flow rate range of sample carrier gas: 50-200ml/min, the sampling flow rate of the high-humidity sample is 100-500ml/min, the flow rate of the purging carrier gas is 50-150ml/min, the temperature of thermal desorption is 40-200 ℃, and the material of the packed column is carbon black adsorbent.

Claims (2)

1. A pre-enrichment device of ion mobility spectrometry is characterized in that: mainly comprises a membrane separator for dehumidification and a packed column for sample enrichment; the membrane adopted by the membrane separator is a tubular gas separation membrane, a membrane layer gas inlet of the membrane separator is connected with a high-humidity sample gas source, and a membrane layer gas outlet of the membrane separator is connected with a gas inlet of a suction pump; a tube layer gas inlet of the membrane separator is connected with a carrier gas source, a tube layer gas outlet of the membrane separator is connected with a first gas inlet of a two-position three-way electromagnetic valve A, a second gas inlet of the two-position three-way electromagnetic valve A is connected with a purge gas source, a gas outlet of the two-position three-way electromagnetic valve A is connected with an inlet of a sample-enriched filling column, an outlet of the sample-enriched filling column is connected with a gas inlet of a two-position three-way electromagnetic valve B, and a first gas outlet of the two-position three-way electromagnetic valve B is connected with a sample gas inlet of an ion mobility spectrometry; and a second gas outlet of the two-position three-way electromagnetic valve B is emptied.
2. The pre-enrichment device of claim 1, wherein: the membrane adopted by the membrane separator is a tubular polytetrafluoroethylene gas separation membrane.
CN202022846182.8U 2020-12-01 2020-12-01 Ion mobility spectrometry's pre-enrichment device Active CN213875525U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023115847A1 (en) * 2021-12-24 2023-06-29 同方威视技术股份有限公司 Trace particle and steam detection system

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023115847A1 (en) * 2021-12-24 2023-06-29 同方威视技术股份有限公司 Trace particle and steam detection system

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