CN107561050A - Portable low-temp plasma automic fluorescence surveys arsenic analytical equipment - Google Patents
Portable low-temp plasma automic fluorescence surveys arsenic analytical equipment Download PDFInfo
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- CN107561050A CN107561050A CN201710970898.9A CN201710970898A CN107561050A CN 107561050 A CN107561050 A CN 107561050A CN 201710970898 A CN201710970898 A CN 201710970898A CN 107561050 A CN107561050 A CN 107561050A
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Abstract
The present invention provides a kind of Portable low-temp plasma automic fluorescence and surveys arsenic analytical equipment, including sampling system, arsenic steam reaction and piece-rate system, plasma generating system and the atomic fluorescence detecting system sequentially connected, the sample feeding system is respectively communicated to the arsenic steam reaction and piece-rate system with the reagent sampling system；The plasma generating system includes atomization pipe (12) and the loop being made up of two spaced copper coils (13,14) and high voltagehigh frequency power supply (11)；The atomic fluorescence detecting system includes detection window (15), excitation source (16), fluorescence detector (17).The analytical equipment of the present invention meets the requirement of Sensitivity and precision needed for actual environment arsenic in sample element determination, and significantly reduces the weight and volume of arsenic element analytical equipment, realizes the portable detection in situ of arsenic element.
Description
Technical field
The present invention relates to a kind of Portable low-temp plasma automic fluorescence to survey arsenic analytical equipment, belongs to Environmental Analytical Chemistry
With instrument and equipment field.
Background technology
Arsenic element is important heavy metal toxic contaminants component.The ground such as Shanxi Province, China, Inner Mongol face serious underground water outlet arsenic
Pollution problem, serious ecological environment and life health risk are brought to local resident.Accurate, the quick measure of arsenic element is existing
For environmental monitoring, safe diet superintendent office, analytical chemistry, Marine Sciences focus of attention.The detection of arsenic element at present
Rely primarily on large scale commercial product atom spectrum instrument, including atomic absorption spectrum, hydride generator atomic fluorescence spectrophotometry, inductance
Coupled plasma mass spectrometry etc..But these equipment instruments and weight are larger, operating condition requires harsh, is unfavorable for carrying and shows
Field recognition.At present, still suffer from can not scene be quick, the bottleneck problem accurately analyzed for the measure of arsenic element.
Present inventor has found under study for action, existing based on research and development such as chemiluminescence, ultraviolet-visible absorption spectroscopies
Portable arsenic element analytical equipment, still can not meet under complicated substrate concurrent conditions, the standard of trace (such as 1 μ g/L) arsenic element
Really analysis.
The content of the invention
The embodiment of the present application provides a kind of Portable low-temp plasma automic fluorescence and surveys arsenic analytical equipment, utilizes low temperature etc.
Ion body technique, overcome existing arsenic element analytical equipment can not field assay, detection sensitivity and antijamming capability is poor asks
Topic, the accurate, quick of Trace Arsenic, field assay in environmental sample can be achieved.
A kind of Portable low-temp plasma automic fluorescence survey arsenic analytical equipment of present invention offer, including what is sequentially connected are entered
Sample system, arsenic steam reaction and piece-rate system, plasma generating system and atomic fluorescence detecting system；The sampling system bag
Include the sample feeding system and reagent sampling system of parallel connection；The sample feeding system is respectively communicated with the reagent sampling system
To the arsenic steam reaction and piece-rate system, sample containing arsenic reacts and divided in arsenic steam reaction and piece-rate system with reagent
Separate out gas-phase product containing arsenic；The plasma generating system includes atomization pipe (12) and spaced by two
The loop that copper coil (13,14) and high voltagehigh frequency power supply (11) are formed, the gas-phase product containing arsenic enter the atomization
After managing (12), by atomization under action of plasma；The atomic fluorescence detecting system includes detection window (15), exciting light
Source (16), fluorescence detector (17), the detection window (15) is entered by atomizing arsenic element atom, passes through the exciting light
Source (16) irradiation produces fluorescence, and its fluorescence signal is detected by vertical direction of the fluorescence detector (17) in exciting light.
Further, the sample feeding system includes the first pumping installations (4) and sample intake passage (1), the reagent enter
Sample system includes the second pumping installations (5) and reagent passage (2), and the sample intake passage (1) and the reagent passage (2) are
PTFE material flexible pipes, internal diameter 1mm, external diameter 1.6mm.
Further, the reagent sampling system is sodium borohydride derivative reagent sampling system, and sodium borohydride solution is now matched somebody with somebody
It is current, it is of short duration to be stored in alkaline solution.
Further, the arsenic steam reaction and piece-rate system include：
Arsenic steam generation reactor (6), inert gas carrier device (3), reaction ring (7) and gas-liquid separator (8)；
The arsenic steam generation reactor (6) respectively with the sample feeding system, the reagent sampling system, described lazy
Property gas carrier device (3), it is described reaction ring (7) connection, it is described reaction ring (7) connected with the gas-liquid separator (8), containing arsenic
After sample mixes with reagent, carrier gas, continue to react into the reaction ring (7), reaction product enters the gas-liquid separator (8)
Carry out gas-liquid separation.
Further, the gas-liquid separator (8) connects with the atomization pipe (12), described after gas-liquid separation
Gas-phase product containing arsenic enters the atomization pipe (12) from the gas-liquid separator (8).
Further, the gas-liquid separator (8) is connected with peristaltic pump (9), and the product liquid after gas-liquid separation is via institute
State peristaltic pump (9) and be discharged into sewer pipe (10).
Further, the atomization pipe (12) is quartz ampoule or earthenware.
Further, the excitation source (16) is arsenic element hollow cathode lamp；The fluorescence detector (17) is optical fiber
Spectrometer or photomultiplier.
Further, the sample filters by 0.45 micron membrane filter, addition 3.0 mole hydrochlorides acidifying, each sample introduction body
Product 0.50mL.
Further, the reaction ring (7) is PTFE material flexible pipes, internal diameter 1mm, external diameter 1.6mm, length 50cm, is wound
For diameter 5cm ring-types.
The Portable low-temp plasma automic fluorescence of the present invention surveys arsenic analytical equipment, detects the spirit of arsenic element in water sample
Sensitivity is up to 0.05 μ g/L, and precision is less than 3%, and analysis time is less than 3 minutes, suitable for a variety of ambient water samples and pedotheque
The Direct Analysis of middle arsenic element.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are this hairs
Some bright embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can be with root
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is a kind of structural representation of low-temp plasma automic fluorescence arsenic apparatus provided in an embodiment of the present invention；
Fig. 2 is a kind of arsenic fluorescence signal intensity of low-temp plasma automic fluorescence arsenic apparatus provided in an embodiment of the present invention
Schematic diagram；
Fig. 3 obtains the micro- gram per liters of 0-25 for a kind of low-temp plasma automic fluorescence arsenic apparatus provided in an embodiment of the present invention
Arsenic solution canonical plotting.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
Part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
Fig. 1 is the structural representation that Portable low-temp plasma automic fluorescence of the present invention surveys arsenic analytical equipment.Such as Fig. 1 institutes
Show, the analytical equipment includes sampling system, arsenic steam reaction and piece-rate system, the plasma system sequentially connected
System and atomic fluorescence detecting system.The sampling system includes sample feeding system in parallel and reagent sampling system.
Sample feeding system includes Liquid sample introduction passage 1 and pumping installations 4, and Liquid sample introduction passage 1 is PTFE material flexible pipes,
Internal diameter 1mm, external diameter 1.6mm, sample are fluid sample, preferably need to filter by 0.45 micron membrane filter, add 3.0 mole hydrochlorides
Acidifying, each sampling volume 0.50mL；Pumping installations 4 can be peristaltic pump or syringe pump, and preferably syringe pump, flow velocity is
10.0mL/min。
Sodium borohydride derivative reagent sampling system includes reagent passage 2 and pumping installations 5.Reagent passage 2 is PTFE materials
Flexible pipe, internal diameter 1mm, external diameter 1.6mm, the now with the current concentration of sodium borohydride solution are 1% (w/w), are stored in 0.5% (w/w) alkali
In property solution, pumping installations 5 can be peristaltic pump or syringe pump, preferably syringe pump, flow velocity 5.0mL/min.
Arsenic steam generation reactor 6 respectively with sample feeding system, sodium borohydride derivative reagent sampling system, inert gas
Carrier gas device 3 and reaction ring 7 are connected.Connecting tube is PTFE materials, internal diameter 1mm, external diameter 1.6mm, sample and sodium borohydride, load
After gas mixing, continue to react into reaction ring 7, reaction product enters gas-liquid separator 8 and carries out gas-liquid separation.Reacting ring 7 is
PTFE material flexible pipes, internal diameter 1mm, external diameter 1.6mm, length 50cm, it is wound up as diameter 5cm ring-types.Inert gas uses argon gas, stream
Fast 500mL/min.The gas-liquid separator 8 is connected with reaction ring 7, plasma generating system, peristaltic pump 9 respectively.React ring 7
In reaction product enter gas-liquid separator 8 after, gas-phase product enters plasma generating system, and product liquid is via peristaltic pump
9 are discharged into sewer pipe 10.The flow velocity of peristaltic pump 9 is 16.0mL/min, slightly larger than pumping installations 4 and the sum of pumping installations 5.
Plasma generating system, it is connected respectively with gas-liquid separator 8 and atomic fluorescence detecting system.Plasma occurs
What system was formed including atomization pipe 12 and by two copper coils 13,14 for being spaced 4.0cm and high voltagehigh frequency power supply 11
Loop.Atomization pipe 12 can be quartz ampoule or earthenware, preferably quartz ampoule, the internal diameter 3.0mm of atomization pipe 12, outer
Footpath 6mm, length 7.0cm.High-frequency and high-voltage power supply is 1.5Kv, 40KHz.After component containing arsenic gas enters atomization pipe 12,
Under action of plasma, by atomization.
The atomic fluorescence detecting system 15,16,17 includes detection window 15, excitation source 16, fluorescence detector 17.Through
By plasma generating system, enter detection window 15 after arsenic element atomization, irradiated by excitation source 16 and produce fluorescence, can
Its fluorescence signal is detected in the vertical direction of exciting light by fluorescence detector 17, waste gas is directly discharged into logical by flue gas leading 18
Wind cupboard.Excitation source 16 is arsenic element hollow cathode lamp；Fluorescence detector 17 can be fiber spectrometer or photomultiplier, preferably
For fluorescent type fiber spectrometer, detection window 15 is built for quartz glass plate, bonded using epoxy resin.
Gathering actual sample includes river sample, spring, rainwater, discharge of industrial wastes water, five kinds of representativenesses of agricultural land soil sample
Actual sample.Simply pre-processed respectively, including：
1) water sample, directly filtered using 0.45 micron membrane filter, add certain volume hydrochloric acid acidified sample, final acidity is
3mol/L；
2) pedotheque, 1.000 grams of pedotheques are weighed, adds 10mL water and carry out ultrasonic extraction.Leaching liquor utilizes 0.45
Micron membrane filter filters.
Directly quantitative analysis, acquired results and this hair are carried out after the completion of sample treatment using inductivity coupled plasma mass spectrometry
Bright Portable low-temp plasma automic fluorescence surveys arsenic analytical equipment testing result and carries out result comparison, referring to Fig. 2 and Fig. 3.
Portable low-temp plasma automic fluorescence of the present invention surveys arsenic analytical equipment, and specifically detection and analytical procedure are：
Step 1：It is standby to 1.5mL centrifuge tube with cover that 0.50mL samples are accurately pipetted using pipettor.
Step 2：Sodium borohydride solution is prepared, 0.5% (w/w) NaOH aqueous solution is prepared first, then by NaBH4It is dissolved in
The alkaline solution, NaBH4Concentration be 1% (w/w).
Step 3：Instrument is opened, sample intake passage pump first enters deionized water solution, detects blank signal.
Step 4：After signal stabilization, arsenic containing solution, system is pumped into by sample intake passage (1).After the completion of sample is pumped into, enter
Sample passage continues pump and enters deionized water solution.
Step 5：Record fluorescence signal.
Step 6：Repeat step four and step 5 to all standard arsenic solutions and actual testing sample measure terminate.
Step 7：Sample channel and sodium borohydride passage are converted into deionized water solution, purging system, close system.
Analysis result is as shown in table 1.As a result show 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 reliable results, accurate.
The analysis result contrast table of table 1
| Sample | Inductivity coupled plasma mass spectrometry detects arsenic concentration | Present invention detection arsenic concentration |
| River | 11.40±1.23μg/L | 11.92±1.10μg/L |
| Rainwater | 1.41±0.22μg/L | 1.52±0.20μg/L |
| Spring | Do not detect | Do not detect |
| Trade effluent | 71.4±3.2μg/L | 70.2±2.6μg/L |
| Agricultural land soil | 1.91±0.37μg/g | 1.89±0.29μg/g |
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：It still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical scheme spirit and
Scope.
Claims (10)
1. a kind of Portable low-temp plasma automic fluorescence surveys arsenic analytical equipment, it is characterised in that enters including what is sequentially connected
Sample system, arsenic steam reaction and piece-rate system, plasma generating system and atomic fluorescence detecting system；
The sampling system includes sample feeding system in parallel and reagent sampling system；
The sample feeding system is respectively communicated to the arsenic steam reaction and piece-rate system with the reagent sampling system, containing arsenic
Sample and reagent react in arsenic steam reaction and piece-rate system and isolate gas-phase product containing arsenic；
The plasma generating system includes atomization pipe (12) and by two spaced copper coil (13,14)
The loop formed with high voltagehigh frequency power supply (11), after the gas-phase product containing arsenic enters the atomization pipe (12), waiting
By atomization under gas ions effect；
The atomic fluorescence detecting system includes detection window (15), excitation source (16), fluorescence detector (17), by atomization
Arsenic element atom enter the detection window (15), by the excitation source (16) irradiate produce fluorescence, by described glimmering
Photodetector (17) detects its fluorescence signal in the vertical direction of exciting light.
2. analytical equipment according to claim 1, it is characterised in that the sample feeding system includes the first pumping installations
(4) lead to sample intake passage (1), the reagent sampling system including the second pumping installations (5) and reagent passage (2), the sample introduction
Road (1) and the reagent passage (2) are PTFE material flexible pipes.
3. analytical equipment according to claim 1 or claim 2, it is characterised in that the reagent sampling system derives for sodium borohydride
Reagent sampling system, sodium borohydride solution is now with the current, of short duration to be stored in alkaline solution.
4. according to one of the claim 1-3 analytical equipments, it is characterised in that the arsenic steam reaction and piece-rate system bag
Include：
Arsenic steam generation reactor (6), inert gas carrier device (3), reaction ring (7) and gas-liquid separator (8)；
The arsenic steam generation reactor (6) respectively with the sample feeding system, the reagent sampling system, the indifferent gas
Body carrier gas device (3), reaction ring (7) connection, the reaction ring (7) connect with the gas-liquid separator (8), sample containing arsenic
After mixing with reagent, carrier gas, continue to react into the reaction ring (7), reaction product is carried out into the gas-liquid separator (8)
Gas-liquid separation.
5. analytical equipment according to claim 4, it is characterised in that the gas-liquid separator (8) and the atomization
(12) connection is managed, the gas-phase product containing arsenic after gas-liquid separation enters the atomization from the gas-liquid separator (8)
Manage (12).
6. analytical equipment according to claim 4, it is characterised in that the gas-liquid separator (8) is connected with peristaltic pump (9),
Product liquid after gas-liquid separation is discharged into sewer pipe (10) via the peristaltic pump (9).
7. according to one of the claim 1-6 analytical equipments, it is characterised in that the atomization pipe (12) is quartz ampoule
Or earthenware.
8. according to one of the claim 1-7 analytical equipments, it is characterised in that the excitation source (16) is that arsenic element is hollow
Cathode modulation；The fluorescence detector (17) is fiber spectrometer or photomultiplier.
9. according to one of the claim 1-8 analytical equipments, it is characterised in that the sample passes through 0.45 micron membrane filter mistake
Filter, addition 3.0 mole hydrochlorides acidifying, each sampling volume 0.50mL.
10. analytical equipment according to claim 4, it is characterised in that the reaction ring (7) is PTFE material flexible pipes, internal diameter
1mm, external diameter 1.6mm, length 50cm, it is wound up as diameter 5cm ring-types.
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| CN201710970898.9A CN107561050A (en) | 2017-10-18 | 2017-10-18 | Portable low-temp plasma automic fluorescence surveys arsenic analytical equipment |
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| CN201710970898.9A CN107561050A (en) | 2017-10-18 | 2017-10-18 | Portable low-temp plasma automic fluorescence surveys arsenic analytical equipment |
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Cited By (3)
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| CN108732162A (en) * | 2018-05-29 | 2018-11-02 | 四川理工学院 | The device for fast detecting and detection method of arsenic concentration in a kind of water |
| CN109187496A (en) * | 2018-10-16 | 2019-01-11 | 四川大学 | A kind of Atomic Emission Spectral Analysis device based on electric heating evaporation and point discharge |
| WO2020087893A1 (en) * | 2018-10-29 | 2020-05-07 | 重庆民泰新农业科技发展集团有限公司 | Atomic fluorescence spectrometry method and device employing water as carrier fluid |
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