CN208043663U - On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment - Google Patents

On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment Download PDF

Info

Publication number
CN208043663U
CN208043663U CN201721786251.2U CN201721786251U CN208043663U CN 208043663 U CN208043663 U CN 208043663U CN 201721786251 U CN201721786251 U CN 201721786251U CN 208043663 U CN208043663 U CN 208043663U
Authority
CN
China
Prior art keywords
atomic
arsenic
temperature plasma
gas
analytical equipment
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.)
Active
Application number
CN201721786251.2U
Other languages
Chinese (zh)
Inventor
师荣光
王建华
张国良
郑向群
赵宗山
于永亮
田永
刘爱风
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.)
Northeastern University China
Qingdao Institute of Bioenergy and Bioprocess Technology of CAS
Agro Environmental Protection Institute Ministry of Agriculture
Original Assignee
Northeastern University China
Qingdao Institute of Bioenergy and Bioprocess Technology of CAS
Agro Environmental Protection Institute Ministry of Agriculture
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 Northeastern University China, Qingdao Institute of Bioenergy and Bioprocess Technology of CAS, Agro Environmental Protection Institute Ministry of Agriculture filed Critical Northeastern University China
Priority to CN201721786251.2U priority Critical patent/CN208043663U/en
Application granted granted Critical
Publication of CN208043663U publication Critical patent/CN208043663U/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The utility model discloses a kind of on-line preconcentration micro low-temperature plasma atomic-emissions to survey arsenic analytical equipment, including:On-line preconcentration-the sampling system being sequentially connected to, gas-liquid separator and micro low-temperature Plasma-Atomic system;After product in the on-line preconcentration-sampling system enters the gas-liquid separator, the component containing arsenic gas isolated enters the micro low-temperature Plasma-Atomic system, the micro low-temperature Plasma-Atomic system includes reaction tube, two parallel electrode plates and high voltagehigh frequency power supply, the analytical equipment further includes atomic emission detection system, the atomic emission detection system includes convex lens collimator, optical fiber, detector.Using the utility model detect arsenic element in a variety of environmental water samples and soil the result shows that, the present apparatus is suitable for quick, live, the accurate detection of arsenic element in a variety of water samples and soil.

Description

On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment
Technical field
The utility model is related to a kind of on-line preconcentration micro low-temperature plasma atomic-emissions to survey arsenic analytical equipment, belong to ring Border analytical chemistry and Instrument technology field.
Background technology
Arsenic is that there are one of extensive toxic pollutants.Ground, the South Asia Countries such as Shanxi, the Inner Mongol of China face seriously Arsenic Contamination in Groundwater problem.The slow poisoning of Arsenic in Drinking Water element, which has become, influences South Asian nation and China some areas The important pollution threat of health of people.Pollution of sensitive, the quick measurement arsenic element for grasp arsenic, avoids the murder by poisoning of arsenic element from having It is significant.The detection of actual environment arsenic in sample element relies primarily on atomic absorption spectrum, hydride generation atomic at present Fluorescence spectrum, inductivity coupled plasma mass spectrometry etc..But such commercialization equipment instrument and weight are larger, operating condition requirement Harshness is unfavorable for carrying and on-site measurement.Currently, the measurement of arsenic element still suffer from can not scene quickly, sensitive analysis asks Topic.
The utility model is intended to, by using on-line preconcentration-micro low-temperature plasma technique, develop a kind of miniature atomic Emit arsenic apparatus, with overcome existing analytical technology can not scene, Sensitive Detection bottleneck, realize environmental sample in Trace Arsenic Accurate, quick, field assay.
Utility model content
For solve existing arsenic element analytical equipment can not field assay, detection sensitivity and anti-interference ability is poor asks Topic, the utility model provide arsenic element analytical equipment in a kind of on-line preconcentration micromation sensitive analysis water sample, the skill of use Art scheme is as follows:
A kind of on-line preconcentration micro low-temperature plasma atomic-emission survey arsenic analytical equipment, including:
On-line preconcentration-the sampling system being sequentially connected to, gas-liquid separator and micro low-temperature Plasma-Atomic system;
After product in the on-line preconcentration-sampling system enters the gas-liquid separator, the group containing arsenic gas isolated Divide and enter the micro low-temperature Plasma-Atomic system,
The micro low-temperature Plasma-Atomic system includes reaction tube, two parallel electrode plates and high voltagehigh frequency electricity Source, component containing arsenic gas under action of plasma, by atomization, form plasma torch into after reaction tube;
The analytical equipment further includes atomic emission detection system, and the atomic emission detection system includes convex lens collimation Device, optical fiber, detector, the convex lens collimator focusing plasma torch send out arsenic element characteristic spectrum, through fiber optic conduction, profit It is detected with detector.
Further, the on-line preconcentration-sampling system includes Liquid sample introduction channel, elute channel, selector valve, sample into Sample pumps, manganese dioxide enriching column, hydrochloric acid channel, sodium borohydride reagent passage, reagent sampling pump, carrier gas, arsenic steam generation reaction Device and reaction ring.
Further, the reaction ring is connected to the gas-liquid separator, is reacted the reaction product in ring and is entered gas-liquid point After device, component containing arsenic gas enters micro low-temperature Plasma-Atomic device, and product liquid is discharged via peristaltic pump.
Further, the reaction tube is quartz ampoule or ceramic tube.
Further, the manganese dioxide enriching column is to fill manganese dioxide, both ends filled glass fiber in PTFE tube;Two The arrival end of manganese oxide enriching column connects selector valve;The outlet end of manganese dioxide enriching column is converged with hydrochloric acid channel, after confluence, even Access an arrival end channel of hydride generator.
Further, it after in the manganese dioxide enriching column access flow path, is constantly rushed using hydrochloric acid and sodium hydroxide solution It is washed till efflux clarification, can be used.
Further, three arrival ends of the arsenic steam generation reactor respectively with carrier gas, sodium borohydride reagent passage, And hydrochloric acid channel and manganese dioxide enriching column converge after channel be connected, the outlet end of the arsenic steam generation reactor with instead Ring is answered to be connected.
Further, when the selector valve connects Liquid sample introduction channel, elution channel is automatically closed;When selector valve is connected When elution channel is eluted, Liquid sample introduction channel is closed.
Further, the reagent sampling pump starts running when selector valve is connected with elution channel;Selector valve and liquid When body sample intake passage is connected to, reagent sampling pump is out of service.
Further, the sample feeding pump and the reagent sampling pump are peristaltic pump or syringe pump.
The utility model on-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic in arsenic analytical equipment detection water sample The sensitivity of element is up to 0.5 μ g/L, and precision is less than 5%, and analysis time is less than 15 minutes, be suitable for a variety of ambient water samples and The analysis of arsenic element in pedotheque.
Description of the drawings
In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is Some embodiments of the utility model, for those of ordinary skill in the art, without creative efforts, Other drawings may also be obtained based on these drawings.
Fig. 1 is that the on-line preconcentration micro low-temperature plasma atomic-emission that the utility model embodiment provides surveys arsenic analysis dress Set overall structure diagram;
Fig. 2 is that the on-line preconcentration micro low-temperature plasma atomic-emission that the utility model embodiment provides surveys arsenic analysis dress The on-line preconcentration set-sampling system structural schematic diagram.
Specific implementation mode
It is new below in conjunction with this practicality to keep the purpose, technical scheme and advantage of the utility model embodiment clearer Attached drawing in type embodiment, the technical scheme in the utility model embodiment is clearly and completely described, it is clear that is retouched The embodiment stated is the utility model a part of the embodiment, instead of all the embodiments.Based on the implementation in the utility model Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to The range of the utility model protection.
As shown in Figure 1, the application on-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment, including:It is suitable On-line preconcentration-sampling system 1 of secondary connection, gas-liquid separator 2 and micro low-temperature Plasma-Atomic system;The online richness After product in collection-sampling system 1 enters the gas-liquid separator 2, the component containing arsenic gas isolated is into described miniature low Isothermal plasma atomization system, the micro low-temperature Plasma-Atomic system include 5, two parallel electrode plates of reaction tube 7,8 and high voltagehigh frequency power supply 6, component containing arsenic gas is into after reaction tube 5, under action of plasma, by atomization, formed etc. Gas ions torch 14;The analytical equipment further includes atomic emission detection system, and the atomic emission detection system includes convex lens Collimator 11, optical fiber 12, detector 13,11 focusing plasma torch of the convex lens collimator send out arsenic element characteristic spectrum, Through fiber optic conduction, detected using detector 13.
As shown in Fig. 2, on-line preconcentration-the sampling system 1 includes Liquid sample introduction channel 16, channel 18, selector valve are eluted 17, sample feeding pump 19, manganese dioxide enriching column 20, hydrochloric acid channel 15, sodium borohydride reagent passage 21, reagent sampling pump 22, Carrier gas 23, arsenic steam generation reactor 24 and reaction ring 25.The sample feeding pump 19 and the reagent sampling pump 22 are to wriggle Pump or syringe pump.In this application, sample is filtered fluid sample, need to pass through 0.45 micron membrane filter and filter, be enriched with sample every time Product volume is 5mL, and flow velocity 0.5mL/min, hydrochloric acid channel concentration of hydrochloric acid is 6mol/L, elutes hydrochloric acid volume 0.2mL, flow velocity is 0.5mL/min.Sodium borohydride solution is now with the current, of short duration to be stored in alkaline solution, and peristaltic pump and syringe pump are interchangeable, injection Pump is optimum condition.The manganese dioxide enriching column is that manganese dioxide is filled in PTFE tube (internal diameter 1.6mm, outer diameter 2.0mm) (0.15g), both ends filled glass fiber, prevention manganese dioxide are lost in.Enriching column accesses in flow path, constantly utilizes hydrochloric acid and hydrogen-oxygen Change sodium solution to rinse to efflux clarification, can use.
The reaction ring 25 is connected to the gas-liquid separator 2, after the reaction product in reaction ring enters gas-liquid separator, Component containing arsenic gas enters micro low-temperature Plasma-Atomic device, and product liquid is discharged via peristaltic pump 3.
The reaction tube 5 is quartz ampoule or ceramic tube, internal diameter 3.0mm, outer diameter 6mm, length 7.0cm, component containing arsenic gas Into after atomizer quartz ampoule 5, under action of plasma, by atomization, plasma torch 14 is formed.
The manganese dioxide enriching column 20 is to fill manganese dioxide, both ends filled glass fiber in PTFE tube;Manganese dioxide The arrival end of enriching column connects selector valve 17;The outlet end of manganese dioxide enriching column is converged with hydrochloric acid channel, after confluence, connect into One arrival end channel of hydride generator.
After the manganese dioxide enriching column 20 accesses in flow path, constantly rinsed to outflow using hydrochloric acid and sodium hydroxide solution Liquid is clarified, and can be used.
Three arrival ends of the arsenic steam generation reactor 24 respectively with carrier gas 23, sodium borohydride reagent passage 21, with And hydrochloric acid channel 15 is connected with the channel after the confluence of manganese dioxide enriching column 20, the outlet end of the arsenic steam generation reactor 24 It is connected with ring 25 is reacted.
When the selector valve 17 connects Liquid sample introduction channel 16, elution channel 18 is automatically closed;When selector valve 17 is connected When elution channel 18 is eluted, Liquid sample introduction channel 16 is closed.
The reagent sampling pump 22 starts running when selector valve 17 is connected with elution channel 18;Selector valve 17 and liquid When sample intake passage 16 is connected to, reagent sampling pump 22 is out of service.
It further includes waste liquid discharge system that the application on-line preconcentration micro low-temperature plasma atomic-emission, which surveys arsenic analytical equipment, 3,4.The carrier gas 23 is argon gas, flow velocity 400mL/min.
Embodiment 1
It includes river water sample, spring, rainwater, discharge of industrial wastes water, five kinds of representativenesses of agricultural land soil sample to acquire actual sample Actual sample.It is simply pre-processed respectively, including:1) water sample directly utilizes 0.45 micron membrane filter filtering, 2) pedotheque, 1.000 grams of pedotheques are weighed, 10mL water is added and carries out ultrasonic extraction.Leaching liquor is filtered using 0.45 micron membrane filter.
After the completion of sample treatment directly quantitative analysis, acquired results and this reality are carried out using inductivity coupled plasma mass spectrometry Result comparison is carried out with new device testing result.
The specific detection and analysis step of utility model device is:
Step 1:It is spare to 10mL centrifuge tube with cover that 5mL samples are accurately pipetted using pipettor.
Step 2:Sodium borohydride solution is prepared, 0.5% (w/w) NaOH aqueous solutions is prepared first, is then dissolved in NaBH4 The alkaline solution, a concentration of 1% (w/w) of NaBH4.
Step 3:Prepare 6mol/L aqueous hydrochloric acid solutions.
Step 4:2mol/L sodium hydroxide solutions are prepared, it is spare to 1mL centrifuge tubes accurately to pipette 0.2mL.
Step 5:Enriching column is filled using 0.15g manganese dioxide, column material is PTFE tube, internal diameter 1.6mm, outer diameter 2.0mm, both ends filled glass fiber, prevention manganese dioxide are lost in.Enriching column accesses in flow path, constantly utilizes hydrochloric acid and hydroxide Sodium solution is clarified to efflux again.
Step 5:All channels pump first enters deionized water solution, irrigation channel.
Step 6:Selector valve is connected to sample channel, is pumped into 5mL samples and passes through manganese dioxide enriching column.
Step 7:Remaining device is opened, selector valve is connected to sodium hydroxide and elutes channel, is pumped into quantitative (0.2mL) hydroxide Sodium solution is eluted by enriching column, is entered hydride generator after eluent and mixed in hydrochloric acid in channel 15, is hydrogenated Object occurs.
Step 8:Record transmitting signal.
Step 9:It repeats Step 6: seven and eight measure to all standard arsenic solutions and practical sample to be tested and terminate.
Step 10:Sample channel and sodium borohydride channel are converted into deionized water solution, and cleaning system closes system.
Analysis result is as shown in table 1.The result shows that the present apparatus analyzes a variety of environmental water sample results and inductively coupled plasma Body mass spectrometry results are consistent, it was demonstrated that this method result is reliable, accurate.
1 analysis result table of table
Finally it should be noted that:Above example is only to illustrate the technical solution of the utility model, rather than its limitations; Although the utility model is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: It still can be with technical scheme described in the above embodiments is modified, or is carried out to which part technical characteristic etc. With replacement;And these modifications or replacements, various embodiments of the utility model technology that it does not separate the essence of the corresponding technical solution The spirit and scope of scheme.

Claims (7)

1. a kind of on-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment, which is characterized in that including:
On-line preconcentration-the sampling system (1) being sequentially connected to, gas-liquid separator (2) and micro low-temperature Plasma-Atomic system;
After product in the on-line preconcentration-sampling system (1) enters the gas-liquid separator (2), that isolates contains arsenic gas Component enters the micro low-temperature Plasma-Atomic system,
The micro low-temperature Plasma-Atomic system includes reaction tube (5), two parallel electrode plates (7,8) and high voltagehigh frequency Power supply (6), component containing arsenic gas is into after reaction tube (5);
The analytical equipment further includes atomic emission detection system, and the atomic emission detection system includes convex lens collimator (11), optical fiber (12), detector (13).
2. analytical equipment according to claim 1, which is characterized in that the on-line preconcentration-sampling system (1) include liquid into Sample channel (16) elutes channel (18), selector valve (17), and sample feeding pumps (19), manganese dioxide enriching column (20), hydrochloric acid channel (15), sodium borohydride reagent passage (21), reagent sampling pump (22), carrier gas (23), arsenic steam generation reactor (24) and reaction Ring (25).
3. analytical equipment according to claim 2, which is characterized in that the reaction ring (25) and the gas-liquid separator (2) It is connected to, after the reaction product in reaction ring enters gas-liquid separator, component containing arsenic gas enters micro low-temperature Plasma-Atomic Change device, product liquid is discharged via peristaltic pump (3).
4. according to one of the claim 1-3 analytical equipments, which is characterized in that the reaction tube (5) is quartz ampoule or ceramics Pipe.
5. analytical equipment according to claim 2, which is characterized in that the manganese dioxide enriching column (20) is to be filled out in PTFE tube Fill manganese dioxide, both ends filled glass fiber;The arrival end connection selector valve (17) of manganese dioxide enriching column;Manganese dioxide is enriched with The outlet end of column is converged with hydrochloric acid channel, after confluence, connects an arrival end channel into hydride generator.
6. analytical equipment according to claim 2, which is characterized in that three entrances of the arsenic steam generation reactor (24) Respectively with carrier gas (23), sodium borohydride reagent passage (21) and hydrochloric acid channel (15) and manganese dioxide enriching column (20) are converged at end Channel after stream is connected, and the outlet end of the arsenic steam generation reactor (24) is connected with ring (25) is reacted.
7. analytical equipment according to claim 2, which is characterized in that the sample feeding pump (19) and the reagent sampling pump (22) it is peristaltic pump or syringe pump.
CN201721786251.2U 2017-12-19 2017-12-19 On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment Active CN208043663U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201721786251.2U CN208043663U (en) 2017-12-19 2017-12-19 On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201721786251.2U CN208043663U (en) 2017-12-19 2017-12-19 On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment

Publications (1)

Publication Number Publication Date
CN208043663U true CN208043663U (en) 2018-11-02

Family

ID=63955533

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201721786251.2U Active CN208043663U (en) 2017-12-19 2017-12-19 On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment

Country Status (1)

Country Link
CN (1) CN208043663U (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110398403A (en) * 2019-07-29 2019-11-01 华北电力大学(保定) A kind of preparation method and device of stable arsenic trioxide standard gas

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110398403A (en) * 2019-07-29 2019-11-01 华北电力大学(保定) A kind of preparation method and device of stable arsenic trioxide standard gas

Similar Documents

Publication Publication Date Title
CN103234778B (en) Device for enriching semi-volatile organic compounds in underground water
CN100541172C (en) The method of fastly analyzing chemical oxygen demand by high-pressure flowing injection
CN101793902A (en) Device for fluidly injecting and rapidly analyzing residual chlorine of water quality and analysis method thereof
CN103091262A (en) Miniaturized optical device for detecting ammonia nitrogen in water and detecting method
CN208043663U (en) On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment
CN108008048A (en) The pollution source discrimination of emerging pollutant and application in a kind of ground water regime
CN107290189B (en) Portable multi-mode sampler
CN104792769B (en) The dynamic micro-extraction of compound, detection combined unit and method in aqueous sample
CN107917909A (en) On-line preconcentration micro low-temperature plasma atomic-emission surveys arsenic analytical equipment
CN203216848U (en) Sample injection device of atomic fluorescence spectrometer
CN110470650A (en) A kind of multi-mode water quality heavy metal on-line monitoring system
CN101514985A (en) Local surface plasma resonance reinforced biochemical detector
CN101509893A (en) Measuring method and device for volatile organic in water
CN111141885A (en) Automatic detection device and detection method for gas mercury detector
CN101358924B (en) Morphological analysis apparatus for mercury element and analysis method thereof
CN104977420B (en) A kind of water quality analytical system
CN201527389U (en) Detection device of performance of preventing infiltration of chemicals for relief protective clothing materials
Trujillo et al. Chemical analysis and sampling techniques for geothermal fluids and gases at the Fenton Hill Laboratory
CN1584581A (en) Micro-current chip capillary electrophoresis and atom fluorescent online combniation
CN202033291U (en) Liquid driving sampling device capable of realizing steam reaction under constant voltage and constant current
CN202599840U (en) Sample injection device of two-injection-pump contrast ventriculography (CVG) system
US20210364435A1 (en) Atomic fluorescence analysis method and device using water as carrier fluid
CN210269762U (en) Automatic detection device for gas mercury detector
Liu et al. A liquid drop: what is it good for?
CN109596603B (en) Method for simultaneously measuring trace arsenic and multiple metal elements in soil

Legal Events

Date Code Title Description
GR01 Patent grant
GR01 Patent grant