CN106290650A - The gas chromatography of organic components in detection volatilization gas - Google Patents

The gas chromatography of organic components in detection volatilization gas Download PDF

Info

Publication number
CN106290650A
CN106290650A CN201610793283.9A CN201610793283A CN106290650A CN 106290650 A CN106290650 A CN 106290650A CN 201610793283 A CN201610793283 A CN 201610793283A CN 106290650 A CN106290650 A CN 106290650A
Authority
CN
China
Prior art keywords
gas
component
chromatography
chromatographic column
acetamide
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
CN201610793283.9A
Other languages
Chinese (zh)
Inventor
施伟利
胡春秀
杨洲
杨涛
张洋
王玉田
宋涛
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.)
Harbin Electric Machinery Co Ltd
Original Assignee
Harbin Electric Machinery 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 Harbin Electric Machinery Co Ltd filed Critical Harbin Electric Machinery Co Ltd
Priority to CN201610793283.9A priority Critical patent/CN106290650A/en
Publication of CN106290650A publication Critical patent/CN106290650A/en
Pending legal-status Critical Current

Links

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
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025Gas chromatography

Landscapes

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

Abstract

The invention discloses and a kind of detect the gas chromatography of organic components in volatilization gas, each component in sample is made to ionize in an ion source by chromatography of gases GC-MS, generate the positively charged ion of different charge-mass ratio (charge-to-mass ratio), the effect of accelerated electric field, form ion beam, enter mass analyzer, in the mass analyser, recycling electric field and magnetic field make the velocity dispersion that generation is contrary, they are focused on respectively and obtains mass spectrum, so that it is determined that its quality, and with this, compound is carried out qualitative.The present invention greatly advances the paces of nuclear power supporting insulant production domesticization, nuclear power End winding from bar insulation to fixtures such as supporting insulation, identify material exploration from material and all give help greatly, significantly improve scientific research efficiency, also ensure that the safety and reliability that material uses in the unit simultaneously.

Description

The gas chromatography of organic components in detection volatilization gas
Technical field: the present invention relates to a kind of detect the gas chromatography of organic components in volatilization gas.
Background technology: nuclear power Half Speed steam turbine generator applies a large amount of insulant, in the fabrication process including paint Glue class, sheet material class, glass fibre class, rubber class etc., part epoxy can add amine curing agent, and bandage tied rope can add Entering the wetting agent containing amino, along with the longtime running of unit, these Ammonia Organic substances may evaporate into inside unit other Material corrodes, thus extreme influence electrical machinery life, the method not detecting corrosive gas before this, therefore unit There is hidden danger in long-term normal operation.
Summary of the invention: it is an object of the invention to provide and a kind of detect the gas chromatographic analysis of organic components in volatilization gas Method, it is possible to effectively detect the composition of insulant volatilization gas, and the insulant choosing non-volatile corrosive gas is carried out Manufacture, it is ensured that the safe operation of motor.
The technical scheme is that
A. firstly the need of carrying out insulant according to actual process heating and collect the gas volatilized;
B. with nitrogen, the gas in gas collecting bottle is transferred in test tube to be measured;
C. carry out separating analysis to gas by chromatography of gases analytic process, gas to be measured is imported to chromatography of gases mass spectrum connection With in instrument, the chromatographic column in gas chromatograph is for separating the critical component of mixing determinand, chromatographic column in gas chromatograph In containing fixing phase, i.e. there is the adsorbent of high surface area, after multi-component biased sample enters chromatographic column, due to adsorbent Different to the absorption affinity of each component, after certain time, each component speed of service in the chromatography column is also the most different, absorption The weak component of power easily is desorbed, and leaves chromatographic column at first and enters detector, and the strongest component of absorption affinity is the easiest Being desorbed, the most finally leave chromatographic column, so, each component is able to the most separated from one another, and order enters detection Device is detected, records;
D. by chromatographic control, the architectural feature shown according to result of the test, thus it is speculated that go out that this type of material contains like base Group.As structure contains silylation, epoxide and phenyl ring, then this type of matter-pole is like siloxanes, and siloxanes is chromatographic column One of composition, in the case of usual collection capacity is less, the group in the detected volatile substance of this type of material, test can be got rid of Interference;As in fruit structure containing amido, and by chromatographic control, group is like acetamide, and acetamide must not be instrument color The one of spectrum post composition, therefore acetamide must for one of the composition of survey volatile matter, and the material containing acetamide is most There is corrosivity, then just to focus more on the attached attribute of material according to actual condition when material selection.With crossing volatilization The qualitative analysis of gas, the attached attribute of Knowing material itself, do not interfere with electromotor with guarantee the most properly functioning, and be new Developing material gives a hand.
The present invention is technically characterized by comprising the steps as follows:
1) for nuclear power end banding material, the existence to specifying group is identified
Conventional analytic process, is only capable of the feature for group itself to analyze the type of group, and the present invention is directed to nuclear power End banding material glass squeeze, carries out the collection of hot volatilization gas to it, by chromatography of gases analytic process to gas to be measured Group detect, checking material whether there is corrosivity.
2) chemically component layers surface analysis current material
Chromatography of gases analytic process is to start with from material body, detects its composition group, by composition radical species and group Composition form analyzes the performance that this material may possess further, finally from material essence Knowing material performance, distinguishes further Materials application is in the feasibility using position.
3) explore for new material
Chromatography of gases analytic process can also be used for material and explores, and according to the actual requirement of production technology, the anti-material requested that pushes away should Some performances and manufacturability, form group analysis from material, carries out theory analysis, and in selecting electromotor, diverse location is the suitableeest Material, substantially reduce the number scientific research engineer testing, reach maximum Expected Results with the shortest time.
The present invention greatly advances the paces of nuclear power supporting insulant production domesticization, and nuclear power End winding is from bar insulation To fixtures such as supporting insulation, though material high temperature resistant, high performance, but in there is corrosive gaseous environment, its life-span Inevitable greatly shortening.Therefore fixing in materials process choosing colligation, whether material has corrosivity becomes nuclear power end and joins What cover material was chosen one examines greatly emphasis, uses the chromatography of gases analytic process glass fiber for nuclear power end banding of this patent Goods (restrict, carry) and part bonded adhesives, the volatile matter under the high temperature of nominal situation has carried out analyzing qualitatively, has got rid of and replace Change and wherein volatilized acidity, corrosivity etc. there is the material of destructive performance, it is ensured that the safety of nuclear power generating sets end banding Property and persistency.This patent identifies material exploration from material and all gives help greatly, significantly improves scientific research efficiency, with Time also ensure that the safety and reliability that material uses in the unit.
Fig. 1 is heater
Fig. 2 is the method collecting gas
Detailed description of the invention:
A. such as Fig. 1, it is necessary first to carry out heating and collecting volatilization in gas collecting bottle 1 according to actual process by insulant 2 The gas gone out;
B. such as Fig. 2, from air inlet end 3 nitrogen injection of gas collecting bottle, after being heated by material with blind enema, volatilization gas is from giving vent to anger End 4 is transferred in test tube to be measured;
C. carry out separating analysis to gas by chromatography of gases analytic process, gas to be measured is imported to chromatography of gases mass spectrum connection With in instrument, the chromatographic column in gas chromatograph is for separating the critical component of mixing determinand, chromatographic column in gas chromatograph In containing fixing phase, i.e. there is the adsorbent of high surface area, after multi-component biased sample enters chromatographic column, due to adsorbent Different to the absorption affinity of each component, after certain time, each component speed of service in the chromatography column is also the most different, absorption The weak component of power easily is desorbed, and leaves chromatographic column at first and enters detector, and the strongest component of absorption affinity is the easiest Being desorbed, the most finally leave chromatographic column, so, each component is able to the most separated from one another, and order enters detection Device is detected, records;
D. by chromatographic control, the architectural feature shown according to result of the test, thus it is speculated that go out that this type of material contains like base Group.As structure contains silylation, epoxide and phenyl ring, then this type of matter-pole is like siloxanes, and siloxanes is chromatographic column One of composition, in the case of usual collection capacity is less, the group in the detected volatile substance of this type of material, test can be got rid of Interference;As in fruit structure containing amido, and by chromatographic control, group is like acetamide, and acetamide must not be instrument color The one of spectrum post composition, therefore acetamide must for one of the composition of survey volatile matter, and the material containing acetamide is most There is corrosivity, then just to focus more on the attached attribute of material according to actual condition when material selection.With crossing volatilization The qualitative analysis of gas, the attached attribute of Knowing material itself, do not interfere with electromotor with guarantee the most properly functioning, and be new Developing material gives a hand.
In sum, by chromatography of gases analytic process determining the hot volatilization gas composition of nuclear power winding overhang Binding material Property analyze, eliminate the use with Corrosive Materia, it is ensured that long-term properly functioning of nuclear power generating sets, and open for new material Send out and give a hand.

Claims (1)

1. detect a gas chromatography for organic components in volatilization gas, it is characterized in that:
A. firstly the need of carrying out insulant according to actual process heating and collect the gas volatilized;
B. with nitrogen, the gas in gas collecting bottle is transferred in test tube to be measured;
C. carry out separating analysis to gas by chromatography of gases analytic process, gas to be measured is imported to chromatography of gases GC-MS In, the chromatographic column in gas chromatograph is for separating the critical component of mixing determinand in gas chromatograph, contains in chromatographic column There is fixing phase, i.e. there is the adsorbent of high surface area, after multi-component biased sample enters chromatographic column, owing to adsorbent is to often The absorption affinity of individual component is different, and after certain time, each component speed of service in the chromatography column is also the most different, and absorption affinity is weak Component easily be desorbed, leave chromatographic column at first and enter detector, and the strongest component of absorption affinity is the most easily solved Suction is got off, and the most finally leaves chromatographic column, and so, each component is able to the most separated from one another, and order enters in detector It is detected, records;
D. by chromatographic control, the architectural feature shown according to result of the test, thus it is speculated that go out that this type of material contains like group, as Containing silylation, epoxide and phenyl ring in structure, then this type of matter-pole is like siloxanes, and siloxanes is that the one-tenth of chromatographic column divides it One, in the case of usual collection capacity is less, the group in the detected volatile substance of this type of material, test interference can be got rid of; As in fruit structure containing amido, and by chromatographic control, group is like acetamide, and acetamide must not be instrument chromatographic column one-tenth Point one, therefore acetamide must for one of the composition of survey volatile matter, and the material containing acetamide has corruption mostly Erosion property, then just to focus more on the attached attribute of material according to actual condition when material selection, by volatilization gas Qualitative analysis, the attached attribute of Knowing material itself, do not interfere with electromotor with guarantee the most properly functioning, and open for new material Send out and give a hand.
CN201610793283.9A 2016-08-31 2016-08-31 The gas chromatography of organic components in detection volatilization gas Pending CN106290650A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610793283.9A CN106290650A (en) 2016-08-31 2016-08-31 The gas chromatography of organic components in detection volatilization gas

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610793283.9A CN106290650A (en) 2016-08-31 2016-08-31 The gas chromatography of organic components in detection volatilization gas

Publications (1)

Publication Number Publication Date
CN106290650A true CN106290650A (en) 2017-01-04

Family

ID=57673094

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610793283.9A Pending CN106290650A (en) 2016-08-31 2016-08-31 The gas chromatography of organic components in detection volatilization gas

Country Status (1)

Country Link
CN (1) CN106290650A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060123883A1 (en) * 2004-12-09 2006-06-15 Shimadzu Corporation Gas chromatography/mass spectrometry system
CN102998380A (en) * 2012-10-15 2013-03-27 上海谱尼测试技术有限公司 Method for detecting 21 volatile organic compounds (VOC) in tobacco packing box
CN105067717A (en) * 2015-07-03 2015-11-18 中华人民共和国台州出入境检验检疫局 Method for measuring 32 volatile substances in plastic product with gas chromatography/mass spectrometry

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060123883A1 (en) * 2004-12-09 2006-06-15 Shimadzu Corporation Gas chromatography/mass spectrometry system
CN102998380A (en) * 2012-10-15 2013-03-27 上海谱尼测试技术有限公司 Method for detecting 21 volatile organic compounds (VOC) in tobacco packing box
CN105067717A (en) * 2015-07-03 2015-11-18 中华人民共和国台州出入境检验检疫局 Method for measuring 32 volatile substances in plastic product with gas chromatography/mass spectrometry

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
小蜗牛0427: "气相色谱", 《百度文库》 *
王立等: "《色谱分析样品处理》", 30 September 2001 *
申丽红等: "热解吸_气相色谱质谱法测定汽车零部件挥发性有机化合物_申丽红", 《化学推进剂与高分子材料》 *
钱津旺: "挥发性有机物的气相色谱分析研究", 《当代化工》 *

Similar Documents

Publication Publication Date Title
Materić et al. Methods in plant foliar volatile organic compounds research
CN105954441B (en) Dioxin organic micro-pollutant on-line detecting system in a kind of practical flue gas
US2959677A (en) Gas analysis
CN104458986A (en) Gas chromatography multichannel sample introduction system and realized atmosphere detection method thereof
CN103380362A (en) Introducing an analyte into a chemical analyzer
CN102353737A (en) Detection device for detecting sulfur hexafluoride electrical equipment fault gas
Lambertus et al. Rapid determination of complex mixtures by dual-column gas chromatography with a novel stationary phase combination and spectrometric detection
CN102192959B (en) Thermal cracker, thermal cracking gas chromatograph and thermal cracking analysis method
US20170343517A1 (en) Micro-device for detecting volatile organic compounds, and method for detecting at least one volatile organic compound contained in a gas sample
Parshintsev et al. Methods for characterization of organic compounds in atmospheric aerosol particles
JP2008139130A (en) Real time analyzer and real time analyzing method
Carlin et al. Forensic applications of gas chromatography
Borusiewicz et al. Comparison of the effectiveness of Tenax TA® and Carbotrap 300® in concentration of flammable liquids compounds
GB2569138A (en) Systems and methods of determining isotopic composition of gaseous samples
CN107703247A (en) Method that is a kind of while detecting volatile organic matter in coating
CN106290650A (en) The gas chromatography of organic components in detection volatilization gas
CN104677976B (en) Magnetic powder adsorbent and the combination analysis method in normal pressure mass spectrum source
US8196449B2 (en) Micro discharge device capable of low voltage discharges in a variety of carrier gases for detection and/or ionization
CN205786518U (en) Dioxin organic micro-pollutant on-line detecting system in actual flue gas
Coopersmith et al. Rapid paper spray mass spectrometry characterization of uranium and exemplar molecular species
Schütze et al. A novel low-cost pre-concentrator concept to boost sensitivity and selectivity of gas sensor systems
Anderson Mass spectrometry of spacecraft contamination using direct analysis in real-time ion source
Fan et al. Portable multi-dimensional gas chromatography device for rapid field analysis of chemical compounds
Capeans et al. Gas mixture monitoring techniques for the LHC detector muon systems
DeWitt Advancements in compact gas collection and analysis from IARPA’s MAEGLIN program

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170104

WD01 Invention patent application deemed withdrawn after publication