CN105403616A - Detection method for gaseous sulfuric acid and sulfate and ion source used for detecting - Google Patents

Detection method for gaseous sulfuric acid and sulfate and ion source used for detecting Download PDF

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Publication number
CN105403616A
CN105403616A CN201510725645.6A CN201510725645A CN105403616A CN 105403616 A CN105403616 A CN 105403616A CN 201510725645 A CN201510725645 A CN 201510725645A CN 105403616 A CN105403616 A CN 105403616A
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China
Prior art keywords
valve
air
ion
detection method
ion gun
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Pending
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CN201510725645.6A
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Chinese (zh)
Inventor
郑军
杨栋森
马嫣
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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Priority to CN201510725645.6A priority Critical patent/CN105403616A/en
Publication of CN105403616A publication Critical patent/CN105403616A/en
Pending legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/68—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns

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

Abstract

The invention discloses a detection method for gaseous sulfuric acid and sulfate and an ion source used for detecting. The detection method comprises the following steps: (1) ionizing air under high tension electricity and generating O<-> and O2<->; (2) enabling NO2, O<-> and O2<-> to have ionic reaction and generating NO3<-> reaction ions; (3) enabling the NO3<-> reaction ions to react with H2SO4 and generating HSO4<->; and (4) detecting the HSO4<-> through a mass spectrometer. According to the detection method disclosed by the invention, no radioactive material is used, no corrosive nitric acid gas is used, and the detection method is safer.

Description

The detection method of a kind of gaseous sulfuric acid and sulfate and detection ion gun
Technical field
The present invention relates to the detection method of a kind of gaseous sulfuric acid and sulfate.
Background technology
In recent years, China's most area atmospheric pollution is on the rise, and atmospheric visibility sharply declines, and heavy haze lock city event frequently occurs, and the research of atmospheric aerosol qualitative and quantitative is faded in important.And it has been generally acknowledged that gasoloid sulfate is one of aerocolloidal principal component, and affect climate change by the formation of the radiation between the participation sun and land and cloud.So Accurate Determining gaseous sulfuric acid contributes to understanding atmospheric aerosol new particle formation mechenism and gasoloid Particle density.
The principle that chemical ionization mass spectrometry measures sulfuric acid generates NO by ion gun 3 -, then with H 2sO 4reaction generates HSO 4 -(E1), Mass Spectrometer Method is entered.Now widely used method be with the harmful radioactive materials such as isotopic ion source (as Am-241) and X-Ray bombardment gaseous state nitric acid and make its charged and then and sulfuric acid reaction, thus measure sulfuric acid.But due to the severe corrosive of the radioactive material safety problem that day by day increases and nitric acid, Long-Time Service or unexpected leakage can cause irremediable infringement to mass spectrometer user and hardware thereof.
（E1）。
Summary of the invention
The object of the invention is, in order to solve the defect existed in prior art, to provide the detection method of a kind of safety, non-radioactive material.
In order to achieve the above object, the invention provides the detection method of a kind of gaseous sulfuric acid and sulfate, comprise the following steps:
(1) air ionizes and produces O under high-tension electricity -and O 2 -;
(2) NO 2with O -and O 2 -ionic reaction produces NO 3 -reactive ion;
(3) NO 3 -reactive ion and H 2sO 4reaction produces HSO 4 -;
(4) HSO is detected by mass spectrometer 4 -.
Present invention also offers and produce above-mentioned NO 3 -the ion gun of reactive ion, comprises stainless pin, air T-valve, NO 2t-valve, trustship; Termination-1700V voltage under stainless pin, air T-valve lower end is stretched in upper end, and the lower end of air T-valve is by trustship insulated enclosure; The upper end of air T-valve and NO 2the lower end of T-valve is connected; Ion gun passes through NO 2the upper end of T-valve is connected with ion molecule reaction room.
Wherein, air T-valve and NO 2t-valve is connected by two stainless-steel tubes.Air T-valve adopts PFA T-valve; NO 2t-valve adopts stainless steel T-valve.
Air T-valve and NO 2the pipe diameter size of T-valve is 6.4mm; The external diameter of stainless-steel tube is 6.4mm, length is 25mm; Gap between the needle point of stainless pin and trustship is 1.5mm.
The present invention has the following advantages compared to existing technology:
1, the present invention does not adopt radioactive source, uses corona discharge method, is conducive to healthy and safe.
2, the present invention without nitric acid as reagent ion, and by two steps by zero air and NO 2the NO that common generation is stable 3 -, effectively prevent HNO 3pollute instrument hardware.
3, the present invention has with low cost, simple structure and firmly and be suitable for the advantages such as field observation.Traditional air ion source chemical ionization mass spectrometry (API-CIMS) adopts large diameter injection port (~ 10cm) to reduce tube wall loss, and high sampling flow velocity (>10SLPM) maintains the laminar condition in ion molecule reaction district.Novel corona electric discharge based on high resolving power flight time mass spectrum does not use ion gun, has high degree of flexibility.
Accompanying drawing explanation
Fig. 1 is the ionogenic structural representation of the present invention;
Fig. 2 is the mass spectrometer spectrogram adopting detection method to carry out gaseous sulfuric acid detection.
In figure, 1-stainless pin, 2-air T-valve, 3-NO 2t-valve, 4-trustship, 5-stainless-steel tube.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
As shown in Figure 1, the air T-valve 2 of stainless pin 1, a 6.4 millimeter generation Wei Luoke production PFA material of corona discharge ion source of the present invention primarily of 30 millimeters long and the NO of the stainless steel of 6.4 millimeters of generation Wei Luoke production 2t-valve 3 forms, and is connected by the generation Wei Luoke stainless-steel tube 5 of two long 25mm, external diameter 6.4mm.Stainless pin 1 is by trustship 4 insulated enclosure, and the gap between needle point and pipe is 1.5mm.Apply about-1700V voltage to stainless pin 1, make it discharge, stainless-steel tube 5 is through the resistance eutral grounding of a 1.0M.The electric current of corona discharge remains on ~ 1.6mA, makes reagent ion concentration keep stable.Not only the left end of air T-valve 2 passes into zero air of 0.42SLPM, as protecting gas but also being reagent gas.NO 2the left end of T-valve 3 passes into 0.38SLPM, the NO of 200ppmv 2, produce NO 3 -ion, reacts with OH free radical and some other unstable leading ion simultaneously and generates NO 3 -and HNO 3, eliminate the interference to experiment.Corona discharge ion source is through the stainless steel pipe access ion molecule reaction room of a 3.2mm.Before the injection port of ion molecule reaction room, adding a teflon pin hole, remaining on 1.94SLPM for controlling sample introduction flow velocity.The Stress control of ion molecule reaction room at 93mbar, thus the ion molecule reaction time be about 0.1s.The NO produced 3 -indoor and the H in ion molecule reaction 2sO 4reaction produces HSO 4 -, effectively HSO can be detected by mass spectrometer 4 -, be illustrated in figure 2 the spectrogram (200 mass unit) obtained for mass spectrometer.NO wherein 3 -for mainly producing ion, HSO 4 -it is the sulfuric acid signal that reaction produces.

Claims (5)

1. a detection method for gaseous sulfuric acid and sulfate, is characterized in that: described detection method comprises the following steps:
(1) air ionizes and produces O under high-tension electricity -and O 2 -;
(2) NO 2with O -and O 2 -ionic reaction produces NO 3 -reactive ion;
(3) NO 3 -reactive ion and H 2sO 4reaction produces HSO 4 -;
(4) HSO is detected by mass spectrometer 4 -.
2. gaseous sulfuric acid and a sulfate detection ion gun, described ion gun is for generation of NO according to claim 1 3 -reactive ion; It is characterized in that: described ion gun comprises stainless pin, air T-valve, NO 2t-valve, trustship; Termination-1700V voltage under described stainless pin, described air T-valve lower end is stretched in upper end, and the lower end of air T-valve is by described trustship insulated enclosure; The upper end of described air T-valve and NO 2the lower end of T-valve is connected; Described ion gun is by described NO 2the upper end of T-valve is connected with ion molecule reaction room.
3. ion gun according to claim 2, is characterized in that: described air T-valve and NO 2t-valve is connected by two stainless-steel tubes.
4. ion gun according to claim 2, is characterized in that: described air T-valve adopts PFA T-valve; Described NO 2t-valve adopts stainless steel T-valve.
5. ion gun according to claim 3, is characterized in that: described air T-valve and NO 2the pipe diameter size of T-valve is 6.4mm; The external diameter of described stainless-steel tube is 6.4mm, length is 25mm; Gap between the needle point of described stainless pin and trustship is 1.5mm.
CN201510725645.6A 2015-12-08 2015-12-08 Detection method for gaseous sulfuric acid and sulfate and ion source used for detecting Pending CN105403616A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510725645.6A CN105403616A (en) 2015-12-08 2015-12-08 Detection method for gaseous sulfuric acid and sulfate and ion source used for detecting

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510725645.6A CN105403616A (en) 2015-12-08 2015-12-08 Detection method for gaseous sulfuric acid and sulfate and ion source used for detecting

Publications (1)

Publication Number Publication Date
CN105403616A true CN105403616A (en) 2016-03-16

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2874764Y (en) * 2005-12-16 2007-02-28 广州禾信自动化***有限公司 Single particle Gerosol online ionizing source
CN101663726A (en) * 2007-04-14 2010-03-03 史密斯探测-沃特福特有限公司 detectors and ion sources
WO2014074701A1 (en) * 2012-11-07 2014-05-15 Ohio University Ionization of chemicals in mixture at low ph by ambient ionization / mass spectrometry

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2874764Y (en) * 2005-12-16 2007-02-28 广州禾信自动化***有限公司 Single particle Gerosol online ionizing source
CN101663726A (en) * 2007-04-14 2010-03-03 史密斯探测-沃特福特有限公司 detectors and ion sources
WO2014074701A1 (en) * 2012-11-07 2014-05-15 Ohio University Ionization of chemicals in mixture at low ph by ambient ionization / mass spectrometry

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JUN ZHENG等: "Development of a new corona discharge based ion source for high resolution time-of-flight chemical ionization mass spectrometer to measure gaseous H2SO4 and aerosol sulfate", 《ATMOSPHERIC ENVIRONMENT》 *

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