CN108426873A - A kind of detection method and dedicated unit of hydride - Google Patents
A kind of detection method and dedicated unit of hydride Download PDFInfo
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- CN108426873A CN108426873A CN201810192313.XA CN201810192313A CN108426873A CN 108426873 A CN108426873 A CN 108426873A CN 201810192313 A CN201810192313 A CN 201810192313A CN 108426873 A CN108426873 A CN 108426873A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The present invention relates to the detection technique of hydride, more particularly to the detection method and dedicated unit of a kind of hydride.Including gas-liquid sample feeding pipe, gas-liquid separation unit, gas center pipe, atomization gas air inlet pipe and level balance unit, wherein gas-liquid separation unit is connected to the bottom of level balance unit, the top of the gas-liquid separation unit is connected to gas-liquid sample feeding pipe and gas central tube, the end of the gas center pipe is placed in the nozzle of the atomization gas air inlet pipe, and the side of the level balance unit is equipped with leakage fluid dram.The direct measurement of the elements such as Ge, As, Se, Te, Sb, Sn and Hg can be achieved.This method uses hydride atomiser system, simplify experiment flow, improve method sensitivity, reduce detection danger, realize quick, simple, efficient, the accurate test hydride elements of ICP OES, ICP OES and research and application associated with hydride direct injected system are opened, test industry has boundless application value.Simultaneously also higher reference value is provided for On Analysis of Chemical Species of Elements.
Description
Technical field
The present invention relates to the detection technique of hydride, more particularly to the detection method and dedicated unit of a kind of hydride.
Background technology
In recent years, with the development of spectrum test analytical technology, ICP-OES is widely used, and conventional func is
Incisively and vividly through performance, it because its test speed is fast, easy to operate, data stabilization is accurate etc., increasingly draws attention, especially
It is the exploitation of its expanded function, causes the concern of Analysts.The hydride element such as As, Se is always that ICP-OES is surveyed at present
The problem of examination is mainly shown as that these constituent contents are extremely low, is less than instrument detection limit, tests low strength, and there is also relatively strong
Interference element, influence the Accurate Determining of these elements, these ionization potentials are higher, it is more difficult to ionize, sensitivity is relatively low, detection
It limits higher.
And then it is badly in need of a kind of effectively removing that interference, separation be quickly fast, hydride of high sensitivity, lowering apparatus detection limit
Detection method and dedicated unit.
Invention content
Present invention aims at provide a kind of detection method and dedicated unit of hydride.
To achieve the above object, the invention adopts a technical scheme as：
A kind of ICP-OES hydride atomization system, including gas-liquid sample feeding pipe (1), gas-liquid separation unit (3), gas center
Manage (4), atomization gas air inlet pipe (5) and level balance unit (10), wherein gas-liquid separation unit (3) and level balance unit (10)
Bottom connection, the top of the gas-liquid separation unit (3) is connected to gas-liquid sample feeding pipe (1) and gas central tube (4), the gas
The end of body central tube (4) is placed at the spout (6) of the atomization gas air inlet pipe (5), the level balance unit (10)
Side is equipped with leakage fluid dram.
The diversion pipe (2) being connected to the gas-liquid sample feeding pipe (1) is equipped in the gas-liquid separation unit (3).
The diversion pipe (2) tilts down and is unenclosed construction above.
The gas-liquid separation unit (3) is connected to the bottom of level balance unit (10) by connecting pipeline (9).
The top of the level balance unit (10) is closed ball (7).
The top of the gas-liquid separation unit (3) is pyramidal structure, and the pyramidal structure connects with the gas center pipe (4)
It is logical.
The gas center pipe (4) is inserted in the atomization gas air inlet pipe (5) and end is placed in the atomization gas air inlet
At the spout (6) for managing (5).
The leakage fluid dram of level balance unit (10) side is connect with drain pipe (8).
A method of hydride being detected using the device, product enters gas after sample to be separated is reacted with reducing agent
Liquid sample feeding pipe, then through introducing gas center pipe under negative pressure force effect, hydride gas is extracted, then realize to hydrogen through atomization gas effect
Compound gas is completely separated, and will then be introduced into ICP-OES quarter bends, and the liquid portion isolated is discharged by sewer pipe.
Specifically：Sample is that sample is reacted into gas-liquid sample feeding pipe with reducing agent, the preliminary separation for realizing gas and liquid,
Gas-liquid separation unit is introduced, and under the action of diversion pipe, realize that liquid is downward, the gases such as hydride of generation are upward, realize
The final separation of gas-liquid, the gases such as hydride are introduced through gas center pipe, atomization gas through atomization gas air inlet, and atomization gas is simultaneously final
Hydride etc. is realized gas separation through spout and is introduced, waste liquid part and unicom pipeline and level balance unit unicom, and
Under blind end effect, level balance, waste liquid part is maintained to be discharged by sewer pipe, realized under constant-pressure conditions, hydride draws mist
Change device, is finally connected with fog chamber, is eventually directed into ICP-OES quarter bends.
Advantage for present invention：
The method of the present invention and device can realize the direct measurement of the elements such as Ge, As, Se, Te, Sb, Sn and Hg.Use this hair
Bright hydride atomiser system, simplifies experiment flow, improves method sensitivity, reduces detection danger, realizes ICP-OES
Quickly, simply, efficiently, accurate test hydride element, open and studied associated with ICP-OES and hydride direct injected system
With application, test industry has boundless application value.Simultaneously also higher reference price is provided for On Analysis of Chemical Species of Elements
Value, and can be applied to the analysis fields such as geology, ocean, environment, medicine, quality inspection, material, alloy, nuclear industry and be used as to hydrogenation
The direct approach of object element determination.
Description of the drawings
Fig. 1 is block diagram provided in an embodiment of the present invention；In figure：1 is gas-liquid sample feeding pipe, and 2 be diversion pipe, and 3 be gas
Liquid separative element, 4 be gas center pipe, and 5 be atomization gas air inlet pipe, and 6 be spout, and 7 be closed sphere, and 8 be sewer pipe, and 9 be company
Siphunculus road, 10 be level balance unit.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, right in the following with reference to the drawings and specific embodiments
The present invention is described in detail.
Detection method utilizes the hydride atomization system, and sample is reacted with reducing agent, generates hydride, gives up
Liquid generates hydride and passes through gas center by gas-liquid separation unit, unicom pipeline, level balance unit and sewer pipe discharge
Pipe sprays under atomization gas effect by spout, and passes through ICP-OES central tubes, is eventually introduced ICP-OES, complete As, Se,
The elements such as Te and Hg it is quick, accurate, test simultaneously.
Detection process sample of the present invention is reacted into gas-liquid sample feeding pipe with reducing agent, preliminary point for realizing gas and liquid
From, introducing gas-liquid separation unit, and under the action of diversion pipe, realize that liquid is downward, the gases such as hydride of generation are upward, real
The final separation of existing gas-liquid, the gases such as hydride are introduced through gas center pipe, atomization gas through atomization gas air inlet, atomization gas and most
Hydride etc. is realized gas separation through spout eventually and is introduced, waste liquid part and unicom pipeline and level balance unit unicom, and
Under blind end effect, level balance, waste liquid part is maintained to be discharged by sewer pipe, realized under constant-pressure conditions, hydride is drawn
Atomizer is finally connected with fog chamber, is eventually directed into ICP-OES quarter bends.The elements such as Ge, As, Se, Te, Sb, Sn and Hg can be achieved
Direct measurement.This method uses hydride atomiser system, simplifies experiment flow, improves method sensitivity, reduce
Detection danger realizes quick, simple, efficient, the accurate test hydride elements of ICP-OES, it is straight with hydride to open ICP-OES
Research associated with sampling system and application are connect, test industry has boundless application value.Also it is simultaneously element valence point
Analysis provides higher reference value.
Embodiment 1
As shown in Figure 1, in ICP-OES hydride atomization systems, including gas-liquid sample feeding pipe 1, gas-liquid separation unit 3, gas
Heart pipe 4, atomization gas air inlet pipe 5 and level balance unit 10, the wherein bottom of gas-liquid separation unit 3 and level balance unit 10 connect
Logical, the top of gas-liquid separation unit 3 is connected to gas-liquid sample feeding pipe 1 and gas central tube 4, and the end of gas center pipe 4 is placed in
At the spout 6 of atomization gas air inlet pipe 5, the side of level balance unit 10 is equipped with leakage fluid dram, and leakage fluid dram is connect with drain pipe 8.
Further, the diversion pipe 2 being connected to gas-liquid sample feeding pipe 1 is equipped in gas-liquid separation unit 3.Diversion pipe 2 dips down
Tiltedly and it is unenclosed construction above.Gas-liquid mixture after reaction flows through gas-liquid sample feeding pipe 1, after diversion pipe 2, on gas
It rises, the waste liquid of generation is mixed by diversion pipe 2 with the liquid of gas-liquid separation unit 3.
Further, gas-liquid separation unit 3 is connected to the bottom of level balance unit 10 by connecting pipeline 9, gas-liquid point
It is connected to level balance unit 10 by connecting pipeline 9 from waste liquid in unit 3, waste liquid flows into level balance by connecting pipeline 9
Unit 10.
Further, the top of level balance unit 10 is closed ball 7, and the liquid level in level balance unit 10 is being closed
Under the action of sphere 7, pressure balance is realized, waste liquid is overflowed and is discharged by sewer pipe 8, realize gas-liquid separation unit 3 and liquid
The pressure balance of face balance unit 10.
The top of gas-liquid separation unit 3 is pyramidal structure, and pyramidal structure is connected to gas center pipe 4, and gas center pipe 4 is inserted
In atomization gas air inlet pipe 5 and end is placed at the spout 6 of atomization gas air inlet pipe 5.
Detection method：
Detected sample is reacted into gas-liquid sample feeding pipe 1 with reducing agent, and the preliminary separation for realizing gas and liquid introduces gas
Liquid separative element 3, and under the action of diversion pipe 2, realize that liquid is downward, the gases such as hydride of generation are under negative pressure force effect
Upwards, stablize extraction hydride gas, realize the final separation of gas-liquid.The gases such as hydride are through gas center pipe 4, atomization gas warp
Atomization gas air inlet pipe 5 introduces, and atomization gas finally draws hydride etc. through spout 6, forms uniform hydride gas mixture.
Waste liquid part and connecting pipe 9 and 10 unicom of level balance unit, and under the action of closed ball 7, level balance is maintained, it gives up
Liquid part is discharged by sewer pipe 8, is realized under constant-pressure conditions, and hydride draws atomizer, is finally connected with fog chamber, is eventually introduced
To ICP-OES quarter bends, realize hydride gas sample introduction, it can be achieved that the elements such as Ge, As, Se, Te, Sb, Sn or Hg direct measurement.
Embodiment 2
The measurement of As, Sb, Sn element in soil
1. accurately weighing 100mg pedotheques in 15ml polytetrafluoroethylliner liners；
2. add 2.5ml HF and 0.5ml HCl, in being cleared up in advance 2 hours on 150 DEG C of electric hot plates, pressure release of uncapping；
3. the sample after pre- resolution, closed, it is placed in anti-corrosion efficient sample-dissolving tank；
4. it is cleared up 12 hours in 180 DEG C in anti-corrosion Electric heat oven, it is cooling；
5. taking out liner, add 1ml HCl sour to dry to the greatest extent in being caught up on 150 DEG C of electric hot plates；
6. add 1ml HCl and 2ml 18.2M Ω pure water, 150 DEG C of airtight digestions 12 hours；
7. liner is taken out in cooling, 10% thiocarbamide 1ml, dilution constant volume to 5g (about 50 times of extension rate) is added.
It is reacted with 1% potassium borohydride that reducing agent pipe introduces by sample feeding pipe, generates hydrogen, hydrogen is given birth to As, Sb and Sn
At hydride, introduced in gas-liquid separation unit 3 by 1.In gas-liquid separation unit 3, hydride by gas inlet tube (4) and
Spout (6), and it is introduced into ICP-OES, realize that the Accurate Determining of middle As, Sb and Sn in matrix, table 1 are that hydride measures soil mark
Test data in sample.
1 test data result table macroelement test result of table
The method of the present invention hydride sampling system is easy to operate, has amount of samples few, securely and reliably, pollution-free, batch
Operation.It the sample of target, is restored by reducing agent, is reacted with boron hydride, generate hydride, introduced ICP-OES, realize
The Accurate Determining of the hydride element such as As, Se solves the problems, such as that atomic fluorescence spectrophotometer testing efficiency is low, as a result accurate
Really, instrument detection lower limit is reduced, while there is very strong application value in ocean, geology and environmental analysis.
Claims (9)
1. a kind of ICP-OES hydride atomization system, which is characterized in that including gas-liquid sample feeding pipe (1), gas-liquid separation unit (3),
Gas center pipe (4), atomization gas air inlet pipe (5) and level balance unit (10), wherein gas-liquid separation unit (3) and level balance
The bottom of unit (10) is connected to, and top and the gas-liquid sample feeding pipe (1) and gas central tube (4) of the gas-liquid separation unit (3) connect
Logical, the end of the gas center pipe (4) is placed at the spout (6) of the atomization gas air inlet pipe (5), the level balance list
The side of first (10) is equipped with leakage fluid dram.
2. ICP-OES hydride atomization system according to claim 1, which is characterized in that set in gas-liquid separation unit (3)
There is the diversion pipe (2) being connected to the gas-liquid sample feeding pipe (1).
3. ICP-OES hydride atomization system according to claim 2, which is characterized in that the diversion pipe (2) dips down
Tiltedly and it is unenclosed construction above.
4. ICP-OES hydride atomization system according to claim 1, which is characterized in that the gas-liquid separation unit (3)
It is connected to by connecting pipeline (9) with the bottom of level balance unit (10).
5. ICP-OES hydride atomization system according to claim 1, which is characterized in that the level balance unit
(10) top is closed ball (7).
6. ICP-OES hydride atomization system according to claim 1, which is characterized in that the gas-liquid separation unit (3)
Top be pyramidal structure, the pyramidal structure is connected to the gas center pipe (4).
7. ICP-OES hydride atomization system according to claim 1, which is characterized in that the gas center pipe (4) is inserted
In the atomization gas air inlet pipe (5) and end is placed at the spout (6) of the atomization gas air inlet pipe (5).
8. ICP-OES hydride atomization system according to claim 1, which is characterized in that the level balance unit
(10) leakage fluid dram with drain pipe (8) of side are connect.
9. a kind of method detecting hydride using the device described in claim 1, it is characterised in that：Sample to be separated with
Product enters gas-liquid sample feeding pipe after reducing agent reaction, then through introducing gas center pipe under negative pressure force effect, extracts hydride gas,
It is realized again through atomization gas effect and hydride gas is completely separated, will then be introduced into ICP-OES quarter bends, the liquid isolated
Part is discharged by sewer pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810192313.XA CN108426873A (en) | 2018-03-09 | 2018-03-09 | A kind of detection method and dedicated unit of hydride |
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|---|---|---|---|
| CN201810192313.XA CN108426873A (en) | 2018-03-09 | 2018-03-09 | A kind of detection method and dedicated unit of hydride |
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