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CN112415119B - Cold trap pre-concentration system and method - Google Patents

Cold trap pre-concentration system and method Download PDF

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Publication number
CN112415119B
CN112415119B CN202011201782.7A CN202011201782A CN112415119B CN 112415119 B CN112415119 B CN 112415119B CN 202011201782 A CN202011201782 A CN 202011201782A CN 112415119 B CN112415119 B CN 112415119B
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Prior art keywords
way valve
cold trap
trap
fid
mfc
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CN112415119A (en
Inventor
李虹杰
胡超
周洁
陈楠
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Wuhan Tianhong Environmental Protection Industry Co ltd
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Wuhan Tianhong Environmental Protection Industry Co ltd
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Priority to CN202011201782.7A priority Critical patent/CN112415119B/en
Publication of CN112415119A publication Critical patent/CN112415119A/en
Priority to PCT/CN2021/127851 priority patent/WO2022089630A1/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/12—Preparation by evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D8/00—Cold traps; Cold baffles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/64—Electrical detectors
    • G01N30/68—Flame ionisation detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N2030/042—Standards
    • G01N2030/047—Standards external
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/12—Preparation by evaporation
    • G01N2030/121—Preparation by evaporation cooling; cold traps
    • G01N2030/123—Preparation by evaporation cooling; cold traps using more than one trap
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to a cold trap pre-concentration system and a method, comprising a double cold trap component capable of realizing continuous uninterrupted sampling, analysis and heating back blowing, a four-way valve II connected with the input of the double cold trap component, a six-position valve I for switching air and an internal standard and an external standard, a four-way valve II, a plurality of electromagnetic valves, a gas flow control component and a pump component, wherein the output of the double cold trap component is connected with the output of the four-way valve II through a ten-way valve nine, the output of the gas flow control component is connected with a plurality of electromagnetic valves, the output of the gas flow control component and the pump component, in addition, the FID sample inlet of a hydrogen flame ion detector of a gas chromatograph GC and the MS sample inlet of a mass spectrum detector of the gas chromatograph GC are connected with the double cold trap component through a six-way valve seven, and finally the six-way valve eight is respectively connected with the MS detection component and the FID detection component of the hydrogen flame ion detector. Therefore, the invention has the advantages that the invention can ensure continuous uninterrupted sampling (the sampling time per hour can reach 60 min) and output 1h time resolution data.

Description

Cold trap pre-concentration system and method
Technical Field
The invention relates to cold trap pre-concentration equipment and a method, which are mainly used in the field of environmental monitoring, in particular to equipment and a method for continuously and uninterruptedly capturing volatile organic compounds.
Background
The volatile organic compounds in the air have various types, large differences in physicochemical properties (boiling point and polarity), low concentration and large differences (concentration range is ppt-ppb), and are difficult to directly measure by an analytical instrument, so that the organic compounds in the air need to be collected and concentrated and then measured.
Compared with the adsorbent, the cold trap concentration has the advantages of simple structure, high trapping efficiency, rapid thermal desorption, no residue and the like, and the principle of cold trap trapping analysis is that a sample is trapped and concentrated, then is heated and resolved, is carried into a chromatographic column by carrier gas of a GC sample inlet for separation, and is then detected by FID and MS detectors.
The HJ-2010 technical requirement and detection method of the continuous monitoring system for the environmental air volatile organic compound gas chromatography issued in 7 months in 2019 requires the sampling time of the volatile organic compound, namely the accumulated sampling time per hour is not less than 30 minutes, and the output of 1 hour time resolution data can be ensured.
The monitoring flow of the continuous monitoring system for the environmental air volatile organic compound gas chromatography comprises the processes of air sample collection, internal standard sample collection, analysis, instrument balance and the like, wherein in the process, the chromatographic-mass spectrum separation analysis time is at least more than 35 minutes, so that the prior single cold trap trapping mode in the market cannot meet the requirements of the existing standard.
Therefore, it is necessary to develop an apparatus and a method that can ensure continuous sampling (the cumulative sampling time per hour should be not less than 30 min) and output 1h of time resolution data.
Disclosure of Invention
The invention mainly solves the technical problems that the accumulated sampling time per hour is not less than 30min and the data of 1h time resolution can be output, and the method for realizing the requirement by adopting a double cold trap, which meet the requirements of the existing standard, and provides equipment and a method for continuously sampling and capturing volatile organic compounds.
The technical problems of the invention are mainly solved by the following technical proposal:
A cold trap pre-concentration system is characterized by comprising a double cold trap component capable of realizing continuous uninterrupted sampling, analysis and heating back blowing, a four-way valve II connected with the input of the double cold trap component, a six-position valve I for switching air and an internal standard and an external standard, a four-way valve II, a plurality of electromagnetic valves, a gas flow control component and a pump component, wherein the output of the double cold trap component is connected with the output of the four-way valve II through a ten-way valve nine, the output of the gas flow control component is connected with a plurality of electromagnetic valves, the output of the gas flow control component and the pump component, in addition, the FID sample inlet of a hydrogen flame ion detector of a gas chromatograph GC and the MS sample inlet of a mass spectrum detector of the gas chromatograph GC are connected with the double cold trap component through a six-way valve seven, and finally the six-way valve eight is respectively connected with the MS detection component and the FID detection component of the hydrogen flame ion detector.
The double cold trap pre-concentration device comprises at least two water traps, namely a first water trap and a second water trap, two trap traps, namely a first trap and a second trap, two ten-way valves and two twelve-way valves, wherein the first water trap is sequentially connected with the third ten-way valve and the fourth ten-way valve through a CO 2 removal pipe, the second water trap is sequentially connected with the first trap through a CO 2 removal pipe, and the third ten-way valve and the fourth ten-way valve are sequentially connected with the second trap through a CO 2 removal pipe.
The double cold trap pre-concentration device comprises two six-way valves, namely a six-way valve seven and a six-way valve eight, and two twelve-way valves, namely a twelve-way valve five and a twelve-way valve six, wherein carrier gas helium is connected with a seventh No. 4 of the six-way valve through an FID sample inlet of a GC, carrier gas helium is connected with a seventh No. 1 of the six-way valve through an MS sample inlet of the GC, a seventh No. 2 of the six-way valve is connected with a fifth No. 4 of the twelve-way valve, a seventh No. 3 of the six-way valve is connected with a fifth No. 9 of the twelve-way valve, a seventh No. 5 of the six-way valve is connected with a sixth No. 9 of the twelve-way valve, a seventh No. 6 of the six-way valve is connected with a sixth No. 4 of the twelve-way valve, a fifth No. 3 of the twelve-way valve is connected with a sixth No. 6 of the six-way valve eight, a fifth of the twelve-way valve is connected with a fifth No. 5 of the six-way valve, a sixth of the twelve-way valve is connected with a sixth No. 2 of the six-way valve, a sixth of the twelve-way valve is connected with a sixth No. 10 of the six-way valve, a tenth of the six-way valve is connected with a sixth No. 10 of the six-way valve, and a sixth valve is connected with a sixth of the six-way valve is connected with a sixth valve is a 6 of the six-way valve, and a 6 of the six-way valve is connected with a 6 of the six-way valve is a valve is connected.
The gas flow control assembly comprises three mass flow meters, namely an MFC I, an MFC II and an MFC III, seven electromagnetic valves, namely an electromagnetic valve V1, an electromagnetic valve V2, an electromagnetic valve V3, an electromagnetic valve V4, an electromagnetic valve V5, an electromagnetic valve V6 and an electromagnetic valve V7, a ten-way valve nine, two pumps, namely a pump I and a pump II, respectively, wherein the output of the double cold trap assembly is connected with the electromagnetic valve V1, the MFC I, the electromagnetic valve V2 and the MFC II respectively through the ten-way valve nine and then is connected with the pump I through the V6, the back-flushing gas nitrogen is connected with the electromagnetic valve V4 and the electromagnetic valve V5 respectively after passing through the MFC III and the electromagnetic valve V3 in sequence and then is connected with the ten-way valve nine simultaneously, the electromagnetic valve V7 is connected with the four-way valve II and the pump II respectively,
A method of cold trap preconcentration, comprising:
Instrument calibration
Cold trap-sampling (external standard), cold trap analysis step specifically includes:
A1.1, sampling a cold trap I, pre-analyzing a cold trap II, triggering and operating a GC-FID/MS analyzer, specifically capturing an external standard sample gas by the cold trap I, switching an air passage by the cold trap II, and preparing for sample analysis
A1.2, sampling the cold trap I, analyzing the cold trap II, specifically, continuously trapping the external standard gas by the cold trap I, carrying the trapped substance into a chromatographic column in the GC by the cold trap II through rapid temperature rise to separate, and finally detecting by the FID and the MS
A1.3, sampling a cold trap I, heating and back-blowing a FID trapping path of the cold trap II and a water trap II, and specifically, continuously trapping external standard gas by the cold trap I;
A1.4, sampling a cold trap I, heating and back blowing an MS trapping path of the cold trap II and a water trap II, and particularly continuously trapping external standard gas by the cold trap I;
a1.5, sampling the first cold trap, and balancing the temperature of the second cold trap, wherein the first cold trap continuously collects external standard gas, the second cold trap keeps refrigeration, and the temperature is reduced to the set temperature required by trapping;
Cold trap one analysis, cold trap two sampling (external standard) step, specifically including:
A2.1, sampling a cold trap II, pre-analyzing the cold trap I, triggering and operating a GC-FID/MS analyzer, namely switching an air path by the cold trap I to prepare for sample analysis;
step A2.2, sampling a cold trap II, and analyzing the cold trap I, wherein the cold trap I carries trapped substances into a chromatographic column in the GC through carrier gas for separation by rapid temperature rise, and finally carries out detection by an FID and an MS, and the cold trap II continuously traps external standard gas;
A2.3, sampling a cold trap II, heating and back blowing the FID trapping paths of the cold trap I and a water trap I, and particularly purging water and other impurities through back blowing of heated nitrogen;
A2.4, sampling a cold trap II, heating and back blowing an MS trapping path of the cold trap I and a water trap I, and particularly purging water and other impurities through back blowing of heated nitrogen by the MS trapping paths of the cold trap I and the water trap I;
A2.5, sampling the cold trap II, and balancing the temperature of the cold trap I, namely keeping the cold trap cold and reducing the temperature to the set temperature required by trapping;
(II) air sample trapping and analysis
Cold trap one sampling, cold trap analysis step, specifically including:
B1.1, sampling a cold trap I, pre-analyzing the cold trap II, triggering and operating a GC-FID/MS analyzer, and particularly capturing air by the cold trap I;
b1.2, sampling a cold trap I, and analyzing the cold trap II, wherein the cold trap I continuously traps air, the cold trap II carries trapped substances into a chromatographic column in the GC through carrier gas for separation by rapid temperature rise, and finally the substances are detected by FID and MS;
b1.3, sampling a cold trap I, heating and back-blowing an FID trapping path of the cold trap II and a water trap II, and particularly continuously trapping air by the cold trap I, and blowing water and other impurities clean by the FID trapping paths of the cold trap II and the water trap II through back-blowing heated nitrogen;
B1.4, sampling a cold trap I, heating and back-blowing an MS trapping path by the cold trap II and a water removing trap II, wherein the cold trap I continuously traps air, and the MS trapping paths of the cold trap II and the water removing trap II clean water and other impurities by back-blowing heated nitrogen;
Step B1.5, sampling the first cold trap, and balancing the temperature of the second cold trap, wherein the first cold trap continuously collects air, the second cold trap keeps refrigeration, and the temperature is reduced to the set temperature required by trapping;
cold trap one analysis, cold trap two sampling steps, specifically including:
Step B2.1, sampling a cold trap II, pre-analyzing the cold trap I, triggering and operating the GC-FID/MS analyzer, specifically switching an air path by the cold trap I, preparing for sample analysis, and capturing air by the cold trap II;
B2.2, sampling a cold trap II, and analyzing the cold trap I, wherein the cold trap I carries trapped substances into a chromatographic column in the GC through carrier gas for separation by rapid temperature rise, and finally carries out detection by an FID and an MS, and the cold trap II continuously traps air;
B2.3, sampling a cold trap II, heating and back blowing the FID trapping paths of the cold trap I and a water trap I, specifically, purging water and other impurities through back blowing of heated nitrogen by the cold trap I and the water trap I, and continuously trapping air by the cold trap II;
b2.4, sampling a cold trap II, heating and back-blowing an MS trapping path of the cold trap I and a water trap I, and particularly purging water and other impurities through back-blowing heated nitrogen by the MS trapping paths of the cold trap I and the water trap I;
And B2.5, sampling the cold trap II, and balancing the temperature of the cold trap I, wherein the cold trap I is kept refrigerated, the temperature is reduced to the set temperature required by trapping, and the cold trap II continuously traps air.
The air sample in the step B1.1 sequentially comprises a six-position valve No. 5, a four-way valve No. two A, a water trap No. one, a ten-way valve No. three A, a ten-way valve No. four A, a twelve-way valve No. five, a ten-way valve No. nine A, V1 (on), V2 (on), MFC No. one (on), MFC No. two (on), V6 (COM and NC) and pump No. one (on), nitrogen sequentially comprises MFC No. three (off), helium sequentially comprises a GC sample inlet (FID), a GC sample inlet (MS), a six-way valve No. seven B, a ten-way valve No. six A, a six-way valve No. eight A, an MS detection assembly and a FID detection assembly
The flow direction of the gas in the step B1.2 is sequentially that the air sample is sequentially six-position valve No. 5, four-way valve No. two A, ten-way valve No. three A, ten-way valve No. four A, twelve-way valve No. five A, ten-way valve No. nine A, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC) and pump one (on), the nitrogen is sequentially MFC three (off), and the helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve No. seven B, ten-way valve No. six B, six-way valve No. eight A, MS detection component and FID detection component.
The air flow direction in the step B1.3 is sequentially six-position valve No. 5, four-way valve No. two A, ten-way valve No. three A, ten-way valve No. four A, twelve-way valve No. five A, ten-way valve No. nine A, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC connection), pump one (on), nitrogen is sequentially MFC three (on), V3 (on), V4 (COM and NC connection), ten-way valve No. nine A, ten-way valve No. six A, ten-way valve No. four A, ten-way valve No. three A, water trap No. two, four-way valve No. two A, V7 (COM and NC connection), helium is sequentially GC inlet (FID), GC inlet (MS), six-way valve No. seven B, ten-way valve No. six A, six-way valve No. FID, six-way valve No. A, six-way valve No. eight-A, detection component, MS detection component
The air flow direction in the step B1.4 is sequentially six-position valve No. 5, four-way valve No. two A, ten-way valve No. three A, ten-way valve No. four A, twelve-way valve No. five A, ten-way valve No. nine A, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC connection), pump one (on), nitrogen is sequentially MFC three (on), V3 (on), V5 (COM and NC connection), ten-way valve No. nine A, ten-way valve No. six A, ten-way valve No. four A, ten-way valve No. three A, water trap No. two, four-way valve No. two A, V7 (COM and NC connection), helium is sequentially GC inlet (FID), GC inlet (MS), six-way valve No. seven B, ten-way valve No. six A, six-way valve No. FID, six-way valve No. A, six-way valve No. eight-A, detection component, MS detection component
The air flow direction in the step B1.5 is sequentially six-position valve No. 5, four-way valve No. two A, ten-way valve No. three A, ten-way valve No. four A, twelve-way valve No. five A, ten-way valve No. nine A, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC) and pump one (on), nitrogen is sequentially MFC three (off), helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve No. seven B, ten-way valve No. six A, six-way valve No. eight A, MS detection component and FID detection component
The air sample in the step B2.1 sequentially comprises a six-position valve No. 5, a four-way valve No. two B, a water trap No. two, a ten-way valve No. three B, a ten-way valve No. four B, a ten-way valve No. six A, a ten-way valve No. nine B, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC) and pump one (on), wherein the nitrogen sequentially comprises MFC three (off), and the helium sequentially comprises a GC sample inlet (FID), a GC sample inlet (MS), a six-way valve No. seven A, a twelve-way valve No. five A, a six-way valve No. eight B, an MS detection assembly and a FID detection assembly
The air sample in the step B2.2 sequentially comprises a six-position valve No. 5, a four-way valve No. two B, a water trap No. two, a ten-way valve No. three B, a ten-way valve No. four B, a ten-way valve No. six A, a ten-way valve No. nine B, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC) and pump one (on), wherein the nitrogen sequentially comprises MFC three (off), the helium sequentially comprises a GC sample inlet (FID), a GC sample inlet (MS), a six-way valve No. seven B, a twelve-way valve No. five B, a six-way valve No. eight B, an MS detection assembly and a FID detection assembly
The air sample in the step B2.3 sequentially comprises a six-position valve A5, a four-way valve B, a water trap B, a ten-way valve four B, a ten-way valve six A, a ten-way valve nine B, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM connected with NC), a pump one (on), nitrogen sequentially comprises a MFC three (on), V3 (on), V4 (COM connected with NO), a ten-way valve nine B, a twelve-way valve five A, a ten-way valve four B, a ten-way valve three B, a water trap one, a four-way valve two B, a V7 (COM connected with NC), a pump two (on), helium sequentially comprises a GC sample inlet (FID), a GC inlet (MS), a six-way valve seven B, a ten-way valve five A, a six-way valve eight B, a six-way valve eight-way valve B, and an MS detection assembly, and a detection assembly
The air sample in the step B2.4 sequentially comprises a six-position valve A5, a four-way valve B, a water trap B, a ten-way valve four B, a ten-way valve six A, a ten-way valve nine B, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM connected with NC), a pump one (on), nitrogen sequentially comprises a MFC three (on), V3 (on), V5 (COM connected with NO), a ten-way valve nine B, a twelve-way valve five A, a ten-way valve four B, a ten-way valve three B, a water trap one, a four-way valve two B, a V7 (COM connected with NC), a pump two (on), helium sequentially comprises a GC sample inlet (FID), a GC inlet (MS), a six-way valve seven B, a ten-way valve five A, a six-way valve eight B, a six-way valve eight-way valve detection assembly and a MS detection assembly
The air sample in the step B2.5 is sequentially six-position valve No. 5, four-way valve No. two B, water trap No. two, ten-way valve No. three B, ten-way valve No. four B, ten-way valve No. six A, ten-way valve No. nine B, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC) and pump one (on), nitrogen is sequentially MFC three (off), helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve No. seven B, ten-way valve No. five A, six-way valve No. eight B, MS detection component and FID detection component
In the cold trap pre-concentration method, the gas flow direction in the calibration step is identical to the air sample flow direction, and only the six-position valve is switched from the No.5 position to the No. 3 position.
The invention has the advantages that 1, the invention can ensure continuous uninterrupted sampling (the sampling time per hour can reach 60 min) and output data with 1h time resolution, 2, the invention provides sufficient time for analysis of chromatograph-mass spectrum, so that more substance types can be expanded and detected, 3, the invention can really realize orderly continuous uninterrupted sampling, analysis and back blowing by skillfully matching a plurality of valves and only needing one set of flow control and one set of analysis equipment, and has high efficiency and cost saving, 4, the invention directly captures a sample through a cold trap, and the sample directly enters analysis equipment through analysis, thereby avoiding the problems of uncertainty pollution, adsorption and the like possibly brought by other indirect sampling processes.
Drawings
FIG. 1 is a schematic diagram of the present invention;
Detailed Description
The technical scheme of the invention is further specifically described below through examples and with reference to the accompanying drawings.
Examples:
1.
The invention relates to a cold trap pre-concentration system which comprises a double cold trap component capable of realizing continuous uninterrupted sampling, analysis and heating back blowing, a four-way valve II connected with the input of the double cold trap component, a six-position valve I for switching air and an internal standard and an external standard, a four-way valve II, a plurality of electromagnetic valves, a gas flow control component and a pump component, wherein the output of the double cold trap component is connected with the four-way valve II through a ten-way valve nine, the FID sample inlet of a hydrogen flame ion detector of a gas chromatograph GC and the MS sample inlet of a mass spectrum detector of the gas chromatograph GC are connected with the double cold trap component through a six-way valve seven, and finally the six-way valve eight is respectively connected with the MS detection component and the FID detection component of the hydrogen flame ion detector.
The double cold trap assembly comprises at least two water traps, namely a water trap I and a water trap II, two trapping traps, namely a trapping trap I and a trapping trap II, and two twelve-way valves, wherein the water trap I is sequentially connected with the ten-way valve III and the ten-way valve IV through a CO 2 removing pipe I, is sequentially connected with the trapping trap I through a CO 2 removing pipe II, and is sequentially connected with the ten-way valve III and the ten-way valve IV through a CO 2 removing pipe II.
The analysis assembly comprises two six-way valves, namely a six-way valve seven and a six-way valve eight, and two twelve-way valves, namely a twelve-way valve five and a twelve-way valve six, wherein the carrier gas helium is connected with the seventh 4-bit of the six-way valve through an FID sample inlet of the GC, the carrier gas helium is connected with the seventh 1-bit of the six-way valve through an MS sample inlet of the GC, the seventh 2-bit of the six-way valve is connected with the fifth 4-bit of the twelve-way valve, the seventh 3-bit of the six-way valve is connected with the fifth 9-bit of the twelve-way valve, the seventh 5-bit of the six-way valve is connected with the sixth 9-bit of the twelve-way valve, the seventh 6-bit of the six-way valve is connected with the sixth 4-bit of the ten-way valve, the fifth 3-bit of the twelve-way valve is connected with the sixth 6-bit of the six-way valve eight, the fifth 10-bit of the twelve-way valve is connected with the eighth 5-bit of the six-way valve, the sixth 3-bit of the six-way valve is connected with the eighth 2-bit of the six-way valve, the sixth-bit of the six-way valve six-6, the seventh 10-bit of the six-way valve is connected with the sixth-bit of the six-way valve, the sixth-9, the seventh 5-bit of the six-th bit of the six-way valve is connected with the six-way valve, the sixth-bit of the six-way valve, and the six-bit of the six-bit valve, and the six-bit valve 6 valve and the six-port valve and 6 valve and the six valve and 6.
The gas flow control assembly comprises three mass flow meters, namely an MFC I, an MFC II and an MFC III, seven electromagnetic valves, namely an electromagnetic valve V1, an electromagnetic valve V2, an electromagnetic valve V3, an electromagnetic valve V4, an electromagnetic valve V5, an electromagnetic valve V6 and an electromagnetic valve V7, a ten-way valve nine and two pumps, namely a pump I and a pump II, wherein the output of the double cold trap assembly is respectively connected with the electromagnetic valve V1, the MFC I, the electromagnetic valve V2 and the MFC II through the ten-way valve nine and then is connected with the pump I through the V6, the back-blowing nitrogen is respectively connected with the electromagnetic valve V4 and the electromagnetic valve V5 after passing through the MFC III and the electromagnetic valve V3 in sequence and is simultaneously connected with the ten-way valve nine, the electromagnetic valve V7 is respectively connected with the four-way valve II and the pump II,
2. A cold trap pre-concentration method adopting the system comprises the following steps:
Instrument calibration
Cold trap-sampling (external standard), cold trap analysis step specifically includes:
A1.1, sampling a cold trap I, pre-analyzing a cold trap II, triggering and operating a GC-FID/MS analyzer, specifically capturing an external standard sample gas by the cold trap I, switching an air passage by the cold trap II, and preparing for sample analysis
A1.2, sampling the cold trap I, analyzing the cold trap II, specifically, continuously trapping the external standard gas by the cold trap I, carrying the trapped substance into a chromatographic column in the GC by the cold trap II through rapid temperature rise to separate, and finally detecting by the FID and the MS
A1.3, sampling a cold trap I, heating and back-blowing a FID trapping path of the cold trap II and a water trap II, and specifically, continuously trapping external standard gas by the cold trap I;
A1.4, sampling a cold trap I, heating and back blowing an MS trapping path of the cold trap II and a water trap II, and particularly continuously trapping external standard gas by the cold trap I;
a1.5, sampling the first cold trap, and balancing the temperature of the second cold trap, wherein the first cold trap continuously collects external standard gas, the second cold trap keeps refrigeration, and the temperature is reduced to the set temperature required by trapping;
Cold trap one analysis, cold trap two sampling (external standard) step, specifically including:
A2.1, sampling a cold trap II, pre-analyzing the cold trap I, triggering and operating a GC-FID/MS analyzer, namely switching an air path by the cold trap I to prepare for sample analysis;
step A2.2, sampling a cold trap II, and analyzing the cold trap I, wherein the cold trap I carries trapped substances into a chromatographic column in the GC through carrier gas for separation by rapid temperature rise, and finally carries out detection by an FID and an MS, and the cold trap II continuously traps external standard gas;
A2.3, sampling a cold trap II, heating and back blowing the FID trapping paths of the cold trap I and a water trap I, specifically, purging water and other impurities through back blowing of heated nitrogen, and continuously trapping external standard gas by the cold trap II;
A2.4, sampling a cold trap II, heating and back blowing an MS trapping path of the cold trap I and a water trap I, and particularly purging water and other impurities through back blowing of heated nitrogen by the MS trapping paths of the cold trap I and the water trap I;
A2.5, sampling the cold trap II, and balancing the temperature of the cold trap I, namely keeping the cold trap cold and reducing the temperature to the set temperature required by trapping;
(II) air sample trapping and analysis
Cold trap one sampling, cold trap analysis step, specifically including:
B1.1, sampling a cold trap I, pre-analyzing the cold trap II, triggering and operating a GC-FID/MS analyzer, and particularly capturing air by the cold trap I;
b1.2, sampling a cold trap I, and analyzing the cold trap II, wherein the cold trap I continuously traps air, the cold trap II carries trapped substances into a chromatographic column in the GC through carrier gas for separation by rapid temperature rise, and finally the substances are detected by FID and MS;
b1.3, sampling a cold trap I, heating and back-blowing an FID trapping path of the cold trap II and a water trap II, and particularly continuously trapping air by the cold trap I, and blowing water and other impurities clean by the FID trapping paths of the cold trap II and the water trap II through back-blowing heated nitrogen;
B1.4, sampling a cold trap I, heating and back-blowing an MS trapping path by the cold trap II and a water removing trap II, wherein the cold trap I continuously traps air, and the MS trapping paths of the cold trap II and the water removing trap II clean water and other impurities by back-blowing heated nitrogen;
Step B1.5, sampling the first cold trap, and balancing the temperature of the second cold trap, wherein the first cold trap continuously collects air, the second cold trap keeps refrigeration, and the temperature is reduced to the set temperature required by trapping;
cold trap one analysis, cold trap two sampling steps, specifically including:
Step B2.1, sampling a cold trap II, pre-analyzing the cold trap I, triggering and operating the GC-FID/MS analyzer, specifically switching an air path by the cold trap I, preparing for sample analysis, and capturing air by the cold trap II;
B2.2, sampling a cold trap II, and analyzing the cold trap I, wherein the cold trap I carries trapped substances into a chromatographic column in the GC through carrier gas for separation by rapid temperature rise, and finally carries out detection by an FID and an MS, and the cold trap II continuously traps air;
B2.3, sampling a cold trap II, heating and back blowing the FID trapping paths of the cold trap I and a water trap I, specifically, purging water and other impurities through back blowing of heated nitrogen by the cold trap I and the water trap I, and continuously trapping air by the cold trap II;
b2.4, sampling a cold trap II, heating and back-blowing an MS trapping path of the cold trap I and a water trap I, and particularly purging water and other impurities through back-blowing heated nitrogen by the MS trapping paths of the cold trap I and the water trap I;
And B2.5, sampling the cold trap II, and balancing the temperature of the cold trap I, wherein the cold trap I is kept refrigerated, the temperature is reduced to the set temperature required by trapping, and the cold trap II continuously traps air.
3. The air flow direction is set forth below.
The flow direction of the gas in the step B1.1 is sequentially that the air sample is sequentially six-position valve A5, four-way valve B A, water trap A, ten-way valve A, twelve-way valve five, ten-way valve nine A, V1 (opening), V2 (opening), MFC one (opening), MFC two (opening), V6 (COM and NC connection), pump one (opening), nitrogen is sequentially MFC three (closing), and helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve seven B, ten-way valve six A, six-way valve eight A, MS detection component and FID detection component
The flow direction of the gas in the step B1.2 is sequentially that the air sample is sequentially six-position valve A5, four-way valve B A, ten-way valve three A, ten-way valve four A, twelve-way valve five A, ten-way valve nine A, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC), pump one (on), nitrogen is sequentially MFC three (off), helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve seven B, ten-way valve six B, six-way valve eight A, MS detection component and FID detection component.
The flow direction of the gas in the step B1.3 is sequentially six-position valve A5, four-way valve B A, ten-way valve three A, ten-way valve four A, twelve-way valve five A, ten-way valve nine A, V1 (open), V2 (open), MFC one (open), MFC two (open), V6 (COM and NC connection), pump one (open), nitrogen is sequentially MFC three (open), V3 (open), V4 (COM and NC connection), ten-way valve nine A, ten-way valve six A, ten-way valve four A, ten-way valve three A, water trap two, four-way valve two A, V7 (COM and NC connection), pump two (open), helium is sequentially GC inlet (FID), GC inlet (MS), six-way valve seven B, ten-way valve six A, six-way valve eight A, MS detection assembly and FID detection assembly
The flow direction of the gas in the step B1.4 is sequentially six-position valve A5, four-way valve B A, ten-way valve three A, ten-way valve four A, twelve-way valve five A, ten-way valve nine A, V1 (open), V2 (open), MFC one (open), MFC two (open), V6 (COM and NC connection), pump one (open), nitrogen is sequentially MFC three (open), V3 (open), V5 (COM and NC connection), ten-way valve nine A, ten-way valve six A, ten-way valve four A, ten-way valve three A, water trap two, four-way valve two A, V7 (COM and NC connection), pump two (open), helium is sequentially GC inlet (FID), GC inlet (MS), six-way valve seven B, ten-way valve six A, six-way valve eight A, MS detection assembly and FID detection assembly
The flow direction of the gas in the step B1.5 is sequentially six-position valve A5, four-way valve B A, ten-way valve three A, ten-way valve four A, twelve-way valve five A, ten-way valve nine A, V1 (on), V2 (on), MFC one (on), MFC two (on), V6 (COM and NC) and pump one (on), nitrogen is sequentially MFC three (off), helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve seven B, ten-way valve six A, six-way valve eight A, MS detection component and FID detection component
The flow direction of the gas in the step B2.1 is sequentially that the air sample is sequentially six-position valve A5, four-way valve B, water trap B, ten-way valve A, ten-way valve B, V1 (open), V2 (open), MFC one (open), MFC two (open), V6 (COM and NC are connected), pump one (open), nitrogen is sequentially MFC three (closed), and helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve A, twelve-way valve A, six-way valve B, MS detection component and FID detection component
The flow direction of the gas in the step B2.2 is sequentially that the air sample is sequentially six-position valve A5, four-way valve B, water trap B, ten-way valve A, ten-way valve B, V1 (open), V2 (open), MFC one (open), MFC two (open), V6 (COM and NC are connected), pump one (open), nitrogen is sequentially MFC three (closed), and helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve seven B, twelve-way valve five B, six-way valve eight B, MS detection component and FID detection component
The flow direction of the gas in the step B2.3 is sequentially that the air sample is sequentially six-position valve I5, four-way valve II B, water trap II, ten-way valve III B, ten-way valve IV B, ten-way valve six A, ten-way valve nine B, V1 (open), V2 (open), MFC I (open), MFC II (open), V6 (COM and NC connection), pump I (open), nitrogen is sequentially MFC III (open), V3 (open), V4 (COM and NO connection), ten-way valve nine B, twelve-way valve five A, ten-way valve four B, ten-way valve three B, water trap I, four-way valve II B, V7 (COM and NC connection), pump II (open), helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve seven B, ten-way valve five A, six-way valve eight B, MS detection component and FID detection component
The flow direction of the gas in the step B2.4 is sequentially that the air sample is sequentially six-position valve I5, four-way valve II B, water trap II, ten-way valve III B, ten-way valve IV B, ten-way valve six A, ten-way valve nine B, V1 (open), V2 (open), MFC I (open), MFC II (open), V6 (COM and NC connection), pump I (open), nitrogen is sequentially MFC III (open), V3 (open), V5 (COM and NO connection), ten-way valve nine B, twelve-way valve five A, ten-way valve four B, ten-way valve three B, water trap I, four-way valve II B, V7 (COM and NC connection), pump II (open), helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve seven B, ten-way valve five A, six-way valve eight B, MS detection component and FID detection component
The flow direction of the gas in the step B2.5 is sequentially that the air sample is sequentially six-position valve A5, four-way valve B, water trap B, ten-way valve A, ten-way valve B, V1 (open), V2 (open), MFC one (open), MFC two (open), V6 (COM and NC are connected), pump one (open), nitrogen is sequentially MFC three (closed), and helium is sequentially GC sample inlet (FID), GC sample inlet (MS), six-way valve B, ten-way valve A, six-way valve B, MS detection component and FID detection component
The gas flow direction in the calibration step is identical to the air sample flow direction, but the six-position valve one is switched from the No. 5 position to the No.3 position.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.

Claims (13)

1.一种冷阱预浓缩系统，其特征在于，包括一个能够实现连续不间断采样、解析以及加热反吹的双冷阱组件以及与双冷阱组件的输入连接的四通阀二，用于切换空气和内、外标的六位阀一与四通阀二连接双冷阱组件的输出通过十通阀九与若干电磁阀、气体流量控制组件以及泵组件连接；另外气相色谱GC的氢火焰离子检测器FID进样口和气相色谱GC的质谱检测器MS进样口通过六通阀七与双冷阱组件相连，最后通过六通阀八分别与质谱检测器MS检测组件和氢火焰离子检测器FID检测组件连接；1. A cold trap pre-concentration system, characterized in that it comprises a double cold trap assembly capable of realizing continuous and uninterrupted sampling, analysis and heating backblowing, and a four-way valve 2 connected to the input of the double cold trap assembly, a six-position valve 1 for switching air and internal and external standards connected to the four-way valve 2, and the output of the double cold trap assembly is connected to a plurality of solenoid valves, a gas flow control assembly and a pump assembly through a ten-way valve 9; in addition, a hydrogen flame ionization detector FID inlet of a gas chromatograph GC and a mass spectrometer MS inlet of the gas chromatograph GC are connected to the double cold trap assembly through a six-way valve 7, and finally connected to a mass spectrometer MS detection assembly and a hydrogen flame ionization detector FID detection assembly respectively through a six-way valve 8; 所述双冷阱组件包括至少两个除水阱，分别为除水阱一和除水阱二，两个捕集阱，分别是捕集阱一和捕集阱二，以及两个十通阀，两个十二通阀；除水阱一通过除CO2管一依次连接十通阀三和十通阀四，再通过十二通阀五与捕集阱一相连除水阱二通过除CO2管二依次连接十通阀三和十通阀四，再通过十二通阀六与捕集阱二相连；The double cold trap assembly includes at least two water removal traps, namely water removal trap 1 and water removal trap 2, two capture traps, namely capture trap 1 and capture trap 2, and two ten-way valves and two twelve-way valves; the water removal trap 1 is connected to the ten-way valve 3 and the ten-way valve 4 in sequence through the CO2 removal pipe 1, and then connected to the capture trap 1 through the twelve-way valve 5; the water removal trap 2 is connected to the ten-way valve 3 and the ten-way valve 4 in sequence through the CO2 removal pipe 2, and then connected to the capture trap 2 through the twelve-way valve 6; 分析组件包括为两个六通阀，分别为六通阀七和六通阀八；以及两个十二通阀，分别为十二通阀五和十二通阀六；载气氦气通过GC的FID进样口与六通阀的七的4号位连接，载气氦气通过GC的MS进样口与六通阀七的1号位相连；六通阀七的2号位与十二通阀五的4号位相连，六通阀七的3号位与十二通阀五的9号位相连，六通阀七的5号位与十二通阀六的9号位相连，六通阀七的6号位与十二通阀六的4号位相连；十二通阀五的3号位与六通阀八的6号位相连，十二通阀五的10号位与六通阀八的5号位相连，十二通阀六的3号位与六通阀八的2号位相连，十二通阀六的10号位与六通阀八的3号位相连；MS检测组件与六通阀八的1号位相连，FID检测组件与六通阀八的4号位相连；The analysis component includes two six-way valves, namely six-way valve seven and six-way valve eight; and two twelve-way valves, namely twelve-way valve five and twelve-way valve six; the carrier gas helium is connected to position 4 of six-way valve seven through the FID injection port of GC, and the carrier gas helium is connected to position 1 of six-way valve seven through the MS injection port of GC; position 2 of six-way valve seven is connected to position 4 of twelve-way valve five, position 3 of six-way valve seven is connected to position 9 of twelve-way valve five, and position 5 of six-way valve seven is connected to The No. 9 position of the twelve-way valve six is connected, and the No. 6 position of the six-way valve seven is connected to the No. 4 position of the twelve-way valve six; the No. 3 position of the twelve-way valve five is connected to the No. 6 position of the six-way valve eight, the No. 10 position of the twelve-way valve five is connected to the No. 5 position of the six-way valve eight, the No. 3 position of the twelve-way valve six is connected to the No. 2 position of the six-way valve eight, and the No. 10 position of the twelve-way valve six is connected to the No. 3 position of the six-way valve eight; the MS detection component is connected to the No. 1 position of the six-way valve eight, and the FID detection component is connected to the No. 4 position of the six-way valve eight; 所述气体流量控制组件包括三个质量流量计，分别是MFC一、MFC二和MFC三；七个电磁阀，分别是电磁阀V1、电磁阀V2、电磁阀V3、电磁阀V4、电磁阀V5、电磁阀V6、电磁阀V7；十通阀九；以及两个泵，分别是泵一和泵二；双冷阱组件的输出通过十通阀九分别与电磁阀V1、MFC一和电磁阀V2、MFC二连接后再通过V6与泵一相连；反吹气氮气依次通过MFC三、电磁阀V3后分别与电磁阀V4和电磁阀V5连接，再同时与十通阀九连接；电磁阀V7分别与四通阀二和泵二连接。The gas flow control component includes three mass flow meters, namely MFC 1, MFC 2 and MFC 3; seven solenoid valves, namely solenoid valve V1, solenoid valve V2, solenoid valve V3, solenoid valve V4, solenoid valve V5, solenoid valve V6 and solenoid valve V7; ten-way valve nine; and two pumps, namely pump one and pump two; the output of the double cold trap component is connected to the solenoid valve V1, MFC 1 and solenoid valve V2, MFC 2 respectively through the ten-way valve nine, and then connected to the pump one through V6; the back-blowing nitrogen passes through MFC 3 and solenoid valve V3 in turn, and is connected to the solenoid valve V4 and solenoid valve V5 respectively, and then is connected to the ten-way valve nine at the same time; the solenoid valve V7 is connected to the four-way valve two and pump two respectively. 2.一种冷阱预浓缩方法，其特征在于，包括：2. A cold trap pre-concentration method, characterized in that it comprises: (一)仪器标定(I) Instrument calibration 冷阱一外标采样，冷阱二分析步骤，具体包括：Cold trap one external standard sampling, cold trap two analysis steps, specifically including: 步骤A1.1、冷阱一进行采样，冷阱二进行预解析，GC-FID/MS分析仪被触发并运行,具体是冷阱一将外标样气捕集，冷阱二将气路切换过来，为样品解析做好就绪准备；Step A1.1, cold trap 1 performs sampling, cold trap 2 performs pre-analysis, and the GC-FID/MS analyzer is triggered and runs. Specifically, cold trap 1 captures the external standard sample gas, and cold trap 2 switches the gas path to prepare for sample analysis; 步骤A1.2、冷阱一进行采样，冷阱二进行解析；具体是冷阱一继续捕集外标气，冷阱二通过快速升温将捕集的物质通过载气带入GC中的色谱柱进行分离，最后交由FID和MS进行检测；Step A1.2, cold trap one performs sampling, and cold trap two performs analysis; specifically, cold trap one continues to capture the external standard gas, and cold trap two rapidly heats up the captured substances and carries them into the chromatographic column in the GC through the carrier gas for separation, and finally delivers them to FID and MS for detection; 步骤A1.3、冷阱一进行采样，冷阱二及除水阱二进行FID捕集路加热反吹；具体是冷阱一继续捕集外标气，冷阱二和除水阱二的FID捕集路通过加热氮气反吹将水分和其他杂质吹扫干净；Step A1.3, cold trap 1 is sampled, cold trap 2 and dewatering trap 2 are heated and backflushed in the FID capture path; specifically, cold trap 1 continues to capture the external standard gas, and the FID capture paths of cold trap 2 and dewatering trap 2 are backflushed with heated nitrogen to purge moisture and other impurities; 步骤A1.4、冷阱一进行采样，冷阱二及除水阱二进行MS捕集路加热反吹；具体是冷阱一继续捕集外标气，冷阱二和除水阱二的MS捕集路通过加热氮气反吹将水分和其他杂质吹扫干净；Step A1.4, cold trap 1 is sampled, cold trap 2 and dewatering trap 2 are heated and backflushed in the MS capture path; specifically, cold trap 1 continues to capture the external standard gas, and the MS capture paths of cold trap 2 and dewatering trap 2 are backflushed with heated nitrogen to purge moisture and other impurities; 步骤A1.5、冷阱一进行采样，冷阱二进行温度平衡；具体是冷阱一继续采集外标气，冷阱二保持制冷，将温度降至捕集所需要的设定温度；Step A1.5, cold trap one performs sampling, and cold trap two performs temperature balance; specifically, cold trap one continues to collect external standard gas, and cold trap two maintains refrigeration, and the temperature is lowered to the set temperature required for capture; 冷阱一分析，冷阱二外标采样步骤，具体包括：Cold trap one analysis and cold trap two external standard sampling steps specifically include: 步骤A2.1、冷阱二进行采样，冷阱一进行预解析，GC-FID/MS分析仪被触发并运行；具体是冷阱一将气路切换过来，为样品解析做好就绪准备，冷阱二将外标样气捕集；Step A2.1, cold trap 2 performs sampling, cold trap 1 performs pre-analysis, and GC-FID/MS analyzer is triggered and runs; specifically, cold trap 1 switches the gas path to prepare for sample analysis, and cold trap 2 captures the external standard sample gas; 步骤A2.2、冷阱二进行采样，冷阱一进行解析；具体是冷阱一通过快速升温将捕集的物质通过载气带入GC中的色谱柱进行分离，最后交由FID和MS进行检测，冷阱二继续捕集外标气；Step A2.2, cold trap 2 performs sampling, and cold trap 1 performs analysis; specifically, cold trap 1 rapidly heats up the captured substances and carries them into the chromatographic column in GC through carrier gas for separation, and finally delivers them to FID and MS for detection, while cold trap 2 continues to capture external standard gas; 步骤A2.3、冷阱二进行采样，冷阱一及除水阱一进行FID捕集路加热反吹；具体是冷阱一和除水阱一通过加热氮气反吹将水分和其他杂质吹扫干净，冷阱二继续捕集外标气；Step A2.3, cold trap 2 is sampled, cold trap 1 and dewatering trap 1 are heated and backflushed in the FID capture path; specifically, cold trap 1 and dewatering trap 1 are backflushed with heated nitrogen to purge moisture and other impurities, and cold trap 2 continues to capture external standard gas; 步骤A2.4、冷阱二进行采样，冷阱一及除水阱一进行MS捕集路加热反吹；具体是冷阱一和除水阱一的MS捕集路通过加热氮气反吹将水分和其他杂质吹扫干净；冷阱二继续捕集外标气；Step A2.4, cold trap 2 is sampled, cold trap 1 and dewatering trap 1 are heated and backflushed for MS capture path; specifically, the MS capture paths of cold trap 1 and dewatering trap 1 are backflushed with heated nitrogen to purge moisture and other impurities; cold trap 2 continues to capture external standard gas; 步骤A2.5、冷阱二进行采样，冷阱一进行温度平衡；具体是冷阱一保持制冷，将温度降至捕集所需要的设定温度，冷阱二继续捕集外标气；Step A2.5, cold trap 2 performs sampling, and cold trap 1 performs temperature balance; specifically, cold trap 1 maintains refrigeration, lowers the temperature to the set temperature required for capture, and cold trap 2 continues to capture the external standard gas; (二)空气样捕集与分析(II) Air sample collection and analysis 冷阱一采样，冷阱二分析步骤，具体包括：Cold trap one sampling and cold trap two analysis steps specifically include: 步骤B1.1、冷阱一进行采样，冷阱二进行预解析，GC-FID/MS分析仪被触发并运行,具体是冷阱一将空气捕集，冷阱二将气路切换过来，为样品解析做好就绪准备；Step B1.1, cold trap 1 performs sampling, cold trap 2 performs pre-analysis, and the GC-FID/MS analyzer is triggered and runs. Specifically, cold trap 1 captures air, and cold trap 2 switches the gas path to prepare for sample analysis; 步骤B1.2、冷阱一进行采样，冷阱二进行解析；具体是冷阱一继续捕集空气，冷阱二通过快速升温将捕集的物质通过载气带入GC中的色谱柱进行分离，最后交由FID和MS进行检测；Step B1.2, cold trap one performs sampling, and cold trap two performs analysis; specifically, cold trap one continues to capture air, and cold trap two rapidly heats up the captured substances and carries them into the chromatographic column in the GC through the carrier gas for separation, and finally delivers them to FID and MS for detection; 步骤B1.3、冷阱一进行采样，冷阱二及除水阱二进行FID捕集路加热反吹；具体是冷阱一继续捕集空气，冷阱二和除水阱二的FID捕集路通过加热氮气反吹将水分和其他杂质吹扫干净；Step B1.3, cold trap 1 is sampled, and cold trap 2 and dewatering trap 2 are heated and backflushed in the FID capture path; specifically, cold trap 1 continues to capture air, and the FID capture paths of cold trap 2 and dewatering trap 2 are backflushed with heated nitrogen to purge moisture and other impurities; 步骤B1.4、冷阱一进行采样，冷阱二及除水阱二进行MS捕集路加热反吹；具体是冷阱一继续捕集空气，冷阱二和除水阱二的MS捕集路通过加热氮气反吹将水分和其他杂质吹扫干净；Step B1.4, cold trap 1 is sampled, and cold trap 2 and dewatering trap 2 are heated and backflushed in the MS capture path; specifically, cold trap 1 continues to capture air, and the MS capture paths of cold trap 2 and dewatering trap 2 are backflushed with heated nitrogen to purge moisture and other impurities; 步骤B1.5、冷阱一进行采样，冷阱二进行温度平衡；具体是冷阱一继续采集空气，冷阱二保持制冷，将温度降至捕集所需要的设定温度；Step B1.5, cold trap one performs sampling, and cold trap two performs temperature balance; specifically, cold trap one continues to collect air, and cold trap two maintains refrigeration, and the temperature is lowered to the set temperature required for capture; 冷阱一分析，冷阱二采样步骤，具体包括：Cold trap one analysis and cold trap two sampling steps specifically include: 步骤B2.1、冷阱二进行采样，冷阱一进行预解析，GC-FID/MS分析仪被触发并运行；具体是冷阱一将气路切换过来，为样品解析做好就绪准备，冷阱二将空气捕集；Step B2.1, cold trap 2 performs sampling, cold trap 1 performs pre-analysis, and the GC-FID/MS analyzer is triggered and runs; specifically, cold trap 1 switches the gas path to prepare for sample analysis, and cold trap 2 captures air; 步骤B2.2、冷阱二进行采样，冷阱一进行解析；具体是冷阱一通过快速升温将捕集的物质通过载气带入GC中的色谱柱进行分离，最后交由FID和MS进行检测，冷阱二继续捕集空气；Step B2.2, cold trap 2 performs sampling, and cold trap 1 performs analysis; specifically, cold trap 1 rapidly heats up the captured substances and carries them into the chromatographic column in GC through carrier gas for separation, and finally delivers them to FID and MS for detection, while cold trap 2 continues to capture air; 步骤B2.3、冷阱二进行采样，冷阱一及除水阱一进行FID捕集路加热反吹；具体是冷阱一和除水阱一通过加热氮气反吹将水分和其他杂质吹扫干净，冷阱二继续捕集空气；Step B2.3, cold trap 2 is sampled, cold trap 1 and dewatering trap 1 are heated and back-flushed in the FID capture path; specifically, cold trap 1 and dewatering trap 1 are back-flushed with heated nitrogen to purge moisture and other impurities, and cold trap 2 continues to capture air; 步骤B2.4、冷阱二进行采样，冷阱一及除水阱一进行MS捕集路加热反吹；具体是冷阱一和除水阱一的MS捕集路通过加热氮气反吹将水分和其他杂质吹扫干净；冷阱二继续捕集空气；Step B2.4, cold trap 2 is sampled, cold trap 1 and dewatering trap 1 are heated and backflushed for MS capture path; specifically, the MS capture paths of cold trap 1 and dewatering trap 1 are backflushed with heated nitrogen to purge moisture and other impurities; cold trap 2 continues to capture air; 步骤B2.5、冷阱二进行采样，冷阱一进行温度平衡；具体是冷阱一保持制冷，将温度降至捕集所需要的设定温度，冷阱二继续捕集空气。Step B2.5, cold trap 2 performs sampling, and cold trap 1 performs temperature balance; specifically, cold trap 1 maintains refrigeration, lowers the temperature to the set temperature required for capture, and cold trap 2 continues to capture air. 3.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B1.1中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二A号位，除水阱一，十通阀三A号位，十通阀四A号位，十二通阀五，号位、十通阀九A号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三关；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀六A号位，六通阀八A号位，MS检测组件、FID检测组件。3. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in the step B1.1 are as follows: for air, the flow directions are as follows: six-way valve position 5, four-way valve position A, dewatering trap one, ten-way valve position A, ten-way valve position A, twelve-way valve position five, ten-way valve position A, V1 open, V2 open, MFC one open, MFC two open, COM of V6 connected to NC, pump one open; for nitrogen, the flow directions are as follows: MFC three closed; for helium, the flow directions are as follows: GC inlet with FID, GC inlet with MS, six-way valve position B, twelve-way valve position A, six-way valve position A, MS detection component, FID detection component. 4.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B1.2中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二A号位，十通阀三A号位，十通阀四A号位，十二通阀五A号位，十通阀九A号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三关；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀六B号位，六通阀八A号位，MS检测组件、FID检测组件。4. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in the step B1.2 are as follows: for air, the flow directions are as follows: six-way valve position 5, four-way valve position A, ten-way valve position A, ten-way valve position A, twelve-way valve position A, ten-way valve position A, V1 open, V2 open, MFC open, MFC open, V6's COM and NC connected, pump open; for nitrogen, the flow directions are as follows: MFC closed three times; for helium, the flow directions are as follows: GC inlet with FID, GC inlet with MS, six-way valve position B, twelve-way valve position B, six-way valve position A, MS detection component, FID detection component. 5.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B1.3中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二A号位，十通阀三A号位，十通阀四A号位，十二通阀五A号位，十通阀九A号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三开、V3开、V4的COM与NC连，十通阀九A号位，十二通阀六A号位，十通阀四A号位，十通阀三A号位，除水阱二，四通阀二A号位，V7的COM与NC连，泵二开；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀六A号位，六通阀八A号位，MS检测组件、FID检测组件。5. A cold trap pre-concentration method according to claim 2, characterized in that the flow direction of the gas in the step B1.3 is as follows: the air sample is as follows: six-way valve one No. 5 position, four-way valve two A position, ten-way valve three A position, ten-way valve four A position, twelve-way valve five A position, ten-way valve nine A position, V1 open, V2 open, MFC one open, MFC two open, V6 COM and NC connected, pump one open; nitrogen is as follows: MFC three open, V3 open, V4 COM and NC connected, ten-way valve nine A position, twelve-way valve six A position, ten-way valve four A position, ten-way valve three A position, dewatering trap two, four-way valve two A position, V7 COM and NC connected, pump two open; helium is as follows: GC inlet with FID, GC inlet with MS, six-way valve seven B position, twelve-way valve six A position, six-way valve eight A position, MS detection component, FID detection component. 6.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B1.4中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二A号位，十通阀三A号位，十通阀四A号位，十二通阀五A号位，十通阀九A号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三开、V3开、V5的COM与NC连，十通阀九A号位，十二通阀六A号位，十通阀四A号位，十通阀三A号位，除水阱二，四通阀二A号位，V7的COM与NC连，泵二开；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀六A号位，六通阀八A号位，MS检测组件、FID检测组件。6. A cold trap pre-concentration method according to claim 2, characterized in that the flow direction of the gas in the step B1.4 is as follows: the air sample is as follows: six-way valve one No. 5 position, four-way valve two A position, ten-way valve three A position, ten-way valve four A position, twelve-way valve five A position, ten-way valve nine A position, V1 open, V2 open, MFC one open, MFC two open, V6 COM and NC connected, pump one open; nitrogen is as follows: MFC three open, V3 open, V5 COM and NC connected, ten-way valve nine A position, twelve-way valve six A position, ten-way valve four A position, ten-way valve three A position, dewatering trap two, four-way valve two A position, V7 COM and NC connected, pump two open; helium is as follows: GC inlet with FID, GC inlet with MS, six-way valve seven B position, twelve-way valve six A position, six-way valve eight A position, MS detection component, FID detection component. 7.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B1.5中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二A号位，十通阀三A号位，十通阀四A号位，十二通阀五A号位，十通阀九A号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三关；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀六A号位，六通阀八A号位，MS检测组件、FID检测组件。7. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in the step B1.5 are as follows: for air, the flow directions are as follows: six-way valve position 5, four-way valve position A, ten-way valve position A, ten-way valve position A, twelve-way valve position A, ten-way valve position A, V1 open, V2 open, MFC open, MFC open, V6's COM and NC connected, pump open; for nitrogen, the flow directions are as follows: MFC closed three times; for helium, the flow directions are as follows: GC inlet with FID, GC inlet with MS, six-way valve position B, twelve-way valve position A, six-way valve position A, MS detection component, FID detection component. 8.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B2.1中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二B号位，除水阱二，十通阀三B号位，十通阀四B号位，十二通阀六A号位、十通阀九B号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三关；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七A号位，十二通阀五A号位，六通阀八B号位，MS检测组件、FID检测组件。8. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in the step B2.1 are as follows: for air, the flow directions are as follows: six-way valve 1, position 5; four-way valve 2, position B; water trap 2; ten-way valve 3, position B; ten-way valve 4, position B; twelve-way valve 6, position A; ten-way valve 9, position B; V1 is on, V2 is on, MFC 1 is on, MFC 2 is on, COM of V6 is connected to NC, and pump 1 is on; for nitrogen, the flow directions are as follows: MFC 3 is off; for helium, the flow directions are as follows: GC inlet with FID, GC inlet with MS, six-way valve 7, position A; twelve-way valve 5, position A; six-way valve 8, position B; MS detection component and FID detection component. 9.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B2.2中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二B号位，除水阱二，十通阀三B号位，十通阀四B号位，十二通阀六A号位、十通阀九B号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三关；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀五B号位，六通阀八B号位，MS检测组件、FID检测组件。9. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in the step B2.2 are as follows: for air, the flow directions are as follows: six-way valve 1, position 5; four-way valve 2, position B; water trap 2; ten-way valve 3, position B; ten-way valve 4, position B; twelve-way valve 6, position A; ten-way valve 9, position B; V1 is on; V2 is on; MFC 1 is on; MFC 2 is on; COM of V6 is connected to NC; pump 1 is on; nitrogen is as follows: MFC 3 is off; helium is as follows: GC inlet with FID, GC inlet with MS, six-way valve 7, position B; twelve-way valve 5, position B; six-way valve 8, position B; MS detection component; FID detection component. 10.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B2.3中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二B号位，除水阱二，十通阀三B号位，十通阀四B号位，十二通阀六A号位、十通阀九B号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三开、V3开、V4的COM与NO连，十通阀九B号位，十二通阀五A号位，十通阀四B号位，十通阀三B号位，除水阱一，四通阀二B号位，V7的COM与NC连，泵二开；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀五A号位，六通阀八B号位，MS检测组件、FID检测组件。10. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in step B2.3 are as follows: the air sample is as follows: six-way valve 1, position 5, four-way valve 2, position B, dewatering trap 2, ten-way valve 3, position B, ten-way valve 4, position B, twelve-way valve 6, position A, ten-way valve 9, position B, V1 is on, V2 is on, MFC 1 is on, MFC 2 is on, COM of V6 is connected to NC, pump 1 is on; nitrogen is as follows: : MFC three is on, V3 is on, COM of V4 is connected to NO, ten-way valve nine is in B position, twelve-way valve five is in A position, ten-way valve four is in B position, ten-way valve three is in B position, water trap one, four-way valve two is in B position, COM of V7 is connected to NC, pump two is on; helium gas is in the following order: GC inlet with FID, GC inlet with MS, six-way valve seven is in B position, twelve-way valve five is in A position, six-way valve eight is in B position, MS detection component, FID detection component. 11.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B2.4中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二B号位，除水阱二，十通阀三B号位，十通阀四B号位，十二通阀六A号位、十通阀九B号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三开、V3开、V5的COM与NO连，十通阀九B号位，十二通阀五A号位，十通阀四B号位，十通阀三B号位，除水阱一，四通阀二B号位，V7的COM与NC连，泵二开；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀五A号位，六通阀八B号位，MS检测组件、FID检测组件。11. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in step B2.4 are as follows: the air sample is as follows: six-way valve 1, position 5, four-way valve 2, position B, dewatering trap 2, ten-way valve 3, position B, ten-way valve 4, position B, twelve-way valve 6, position A, ten-way valve 9, position B, V1 is on, V2 is on, MFC 1 is on, MFC 2 is on, COM of V6 is connected to NC, pump 1 is on; nitrogen is as follows: : MFC three is on, V3 is on, COM of V5 is connected to NO, ten-way valve nine is in B position, twelve-way valve five is in A position, ten-way valve four is in B position, ten-way valve three is in B position, water trap one, four-way valve two is in B position, COM of V7 is connected to NC, pump two is on; helium gas is in the following order: GC inlet with FID, GC inlet with MS, six-way valve seven is in B position, twelve-way valve five is in A position, six-way valve eight is in B position, MS detection component, FID detection component. 12.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述步骤B2.5中的气体的流向依次为：空气样依次为：六位阀一5号位，四通阀二B号位，除水阱二，十通阀三B号位，十通阀四B号位，十二通阀六A号位、十通阀九B号位，V1开、V2开、MFC一开、MFC二开、V6的COM与NC连，泵一开；氮气依次为：MFC三关；氦气依次为：带FID的GC进样口、带MS的GC进样口，六通阀七B号位，十二通阀五A号位，六通阀八B号位，MS检测组件、FID检测组件。12. A cold trap pre-concentration method according to claim 2, characterized in that the flow directions of the gases in the step B2.5 are as follows: for air, the flow directions are as follows: six-way valve 1, position 5; four-way valve 2, position B; water trap 2; ten-way valve 3, position B; ten-way valve 4, position B; twelve-way valve 6, position A; ten-way valve 9, position B; V1 is on, V2 is on, MFC 1 is on, MFC 2 is on, COM of V6 is connected to NC, and pump 1 is on; for nitrogen, the flow directions are as follows: MFC 3 is off; for helium, the flow directions are as follows: GC inlet with FID, GC inlet with MS, six-way valve 7, position B; twelve-way valve 5, position A; six-way valve 8, position B; MS detection component and FID detection component. 13.根据权利要求2所述的一种冷阱预浓缩方法，其特征在于，所述仪器标定的气体流向与空气样流向一致，只是六位阀一从5号位切换到3号位。13. A cold trap pre-concentration method according to claim 2, characterized in that the gas flow direction calibrated by the instrument is consistent with the air sample flow direction, except that the six-position valve 1 is switched from position 5 to position 3.
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