CN205844171U - A kind of device formed for element evaporation thing - Google Patents
A kind of device formed for element evaporation thing Download PDFInfo
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- CN205844171U CN205844171U CN201620746395.4U CN201620746395U CN205844171U CN 205844171 U CN205844171 U CN 205844171U CN 201620746395 U CN201620746395 U CN 201620746395U CN 205844171 U CN205844171 U CN 205844171U
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- liquid separator
- peristaltic pump
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Abstract
The utility model discloses a kind of device formed for element evaporation thing, this device includes the ingress pipe of dithiocarbonic acid (salt) solution, peristaltic pump, tee T, gas-liquid separator, carrier gas inlet, carrier gas outlet and the discharging of waste liquid pipe of the sample solution ingress pipe containing element, amino-contained；Wherein threeway is connected with peristaltic pump, gas-liquid separator respectively, and gas-liquid separator is provided with carrier gas gateway and separates the discharging of waste liquid pipe of volatile gas.Its method is by the solution of the dithiocarbonic acid (or its salt) of amino-contained and Element Solution on-line mixing to be measured, mixed solution carries out gas-liquid separation immediately, makes volatile element complex enter into elemental analyser and carries out detecting or the preparation of chemical vapor deposition films for element.
Description
Technical field
This utility model belongs to instrument analysis technology field, relates to a kind of device formed for element evaporation thing.
Background technology
At present, the hydride generation sampling system used in atomic spectrograph, major part is to use sodium borohydride (potassium)
That makees hydride generation goes back original reagent, by the hydrogen in sodium borohydride (potassium), the element reduction in sample solution is become gaseous hydro
After thing, element is measured in atomic spectrograph.The Conventional pneumatic mist in atomic spectrum is compared due to hydride sample introduction efficiency
Changing sample introduction, (Conventional pneumatic nebulization sampling only has 3-5%, measures sensitivity relatively low, and hydride sample introduction higher sample introduction efficiency
Efficiency is close to 100%), thus on measuring, there is higher sensitivity and the feature of lower detection limit.Applied is to use
Sodium borohydride (potassium) and be easily formed nine elements (arsenic, antimony, bismuth, germanium, stannum, lead, selenium, tellurium, hydrargyrum) of hydride traditionally and form this
The hydride of a little elements and be measured by atomic spectrograph.
In recent years, along with deepening continuously of scientific and technical personnel's research, some are engaged in the staff of analysis, in succession find, have
Close other element and also with sodium borohydride (potassium), hydrogenation can occur, and successively deliver many research papers.Such as Guo is little big
The zinc and the cadmium that are found that in acidic aqueous solution at normal temperatures equal to nineteen ninety-five can be reduced into volatile by sodium borohydride solution
Hydride, and use this hydrogenation generation sample to enter system, atomic fluorescence determines the zinc in actual sample and cadmium
Assay.Aderval.SLuna and P.Pohl has reported for work some elements such as lower 2000 and calendar year 2001 respectively
Gold, silver, copper, manganese, titanium etc. can also form hydride with sodium borohydride (potassium) reaction at normal temperatures.But the side of above-mentioned document report
Method, there is formation hydride efficiency comparison be low, residual phenomena than more serious defect so that the method is subject in actual use
To hindering.
Using sodium borohydride chemical evapn generation another one deficiency is that sodium borohydride price comparison is expensive, and unstable.
Its solid reagent length standing time can resolve into block sodium metaborate, and solution standing time is long can decompose.It is generally required to it is existing
With now joining.It addition, sodium borohydride to make reducing agent for measuring element number or limited.Such as, for survey zinc cobalt time
Wait its sensitivity the lowest, rare earth can not be surveyed.
Summary of the invention
The purpose of this utility model is that the shortcoming overcoming prior art is with not enough, it is provided that a kind of brand-new waving for element
The device that stimulating food is formed.
The technical solution of the utility model is as follows:
A kind of device formed for element evaporation thing, it is characterised in that this device includes that the sample solution containing element imports
Pipe 1, the ingress pipe 2 of dithiocarbonic acid (salt) solution of amino-contained, peristaltic pump 3, tee T 4, gas-liquid separator 5, carrier gas inlet
6, carrier gas outlet 7 and discharging of waste liquid pipe 8；Wherein threeway 4 is while being connected with peristaltic pump 3, another side and gas-liquid separator 5 phase
Even, gas-liquid separator 5 lower end is provided with carrier gas inlet 6, and upper end is provided with carrier gas outlet 7, is provided with discharging of waste liquid pipe in gas-liquid separator
8。
The forming method of element evaporation thing, is the solution of the dithiocarbonic acid (salt) of amino-contained and Element Solution to be measured to be existed
Line mixes, and mixed solution carries out gas-liquid separation mensuration immediately, makes volatile element complex enter into elemental analyser and enters
Row detection or the preparation of the chemical vapor deposition films for element.
The dithiocarbonic acid (salt) of above-mentioned amino-contained is: diethyldithiocar bamic acid, diethyl-dithio amino
The salt that formic acid is formed with alkali metal, alkaline-earth metal and ammonia.Wherein alkali metal is lithium, sodium, potassium；Alkaline-earth metal is magnesium and calcium.
The dithiocarbonic acid (salt) of above-mentioned amino-contained is preferably sodium diethyldithiocarbamate, Methyl disulfide generation
Carbamic acid sodium or APDC (potassium, sodium).
Part major element, section transitions element, precious metal element and the rare earth unit that in this utility model, element to be measured refers to
Element, wherein major element refers to: calcium, magnesium, strontium, barium, gallium, aluminum, indium, thallium, germanium, stannum, lead, arsenic, antimony, bismuth selenium tellurium；Transition unit
Element refers to: scandium, titanium, vanadium, chromium, manganese, ferrum, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, cadmium, hafnium, tantalum, tungsten, rhenium, hydrargyrum；Noble metal unit
Element is ruthenium, rhodium, palladium, silver, osmium, iridium, platinum, gold；Rare earth element refer to lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium,
Erbium, thulium, ytterbium, lutecium, uranium, thorium and plutonium.
In above-mentioned element preferred element refer to indium, thallium, germanium, stannum, lead, arsenic, antimony, bismuth, ruthenium, rhodium, palladium, silver, osmium, iridium,
Platinum, gold, scandium, titanium, vanadium, chromium, manganese, ferrum, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, cadmium, hafnium, tantalum, tungsten and hydrargyrum.
Two solution concentrations in this utility model are 0.005-35%(w/w respectively) dithiocarbonic acid (salt) of amino-contained
The Element Solution on-line mixing to be measured of solution and acidity 0.005-10.0 M.
In this utility model, the dithiocarbonic acid (salt) of amino-contained is in preferred mass concentration mixed with Element Solution
Being 0.005-15%, dithiocarbonic acid (salt) mass concentration of preferred amino-contained is 0.03-10%, the two of preferred amino-contained
Bamic acid (salt) mass concentration is 3-8%.
In this utility model the most to be mixed after the acidity of solution be preferably 0.01-0.4 mol/L；Treat the most online
The acidity of mixed solution is 0.05-3.0M;The acidity of the solution after preferred line is to be mixed is 0.05-0.15M.
An exemplary embodiments of the present utility model comprises the steps:
(1) sodium diethyldithiocarbamate (or the pyrrole using peristaltic pump continuous drawing mass concentration to be respectively 3-8%
Cough up alkane aminodithioformic acid ammonia) solution and acidity be 0.05-0.3M containing element sample solution；(2) make two strands of solution one
Converge reaction in miniature three-way pipe, in gas-liquid separator, carry out gas-liquid separation immediately after；(3) isolated gas is imported into
Atomic spectrograph is measured.
First typical device (see Figure of description 1) of the present utility model, imports including the sample solution containing element
Pipe, the ingress pipe of dithiocarbonic acid (salt) solution of amino-contained, peristaltic pump, tee T, gas-liquid separator, carrier gas inlet, carrier gas
Outlet and discharging of waste liquid pipe；Converge in tee T after two solution of peristaltic pump pumps and react, then with gas-liquid separator
Being connected, gas-liquid separator is provided with carrier gas inlet, and carrier gas outlet, separates the waste liquid of volatile gas by peristaltic pump through discharging of waste liquid
Bank of tubes goes out.
It is applicable to second typical device (see Figure of description 2) of the present utility model, molten including the sample containing element
Liquid ingress pipe 1, the ingress pipe 2 of dithiocarbonic acid (salt) solution, peristaltic pump 3, tee T 4, Atomic Absorption or the inductance of amino-contained
Nebulizer 9, Atomic Absorption or the inductively coupled plasma of the nebulization sampling of coupled plasma optical emission spectrum (or mass spectrum)
Emission spectrum (or mass spectrum) fog chamber (rotary spray chamber or Scott fog chamber) 5, carrier gas inlet, carrier gas outlet and discharging of waste liquid
Pipe；Mixed by two strands of solution after threeway after two solution of peristaltic pump pumps, subsequently into nebulizer, enter after atomizer spray
Fog chamber, gas-liquid separator be provided with carrier gas inlet and carrier gas outlet, separate volatile gas waste liquid by peristaltic pump through discharging of waste liquid
Bank of tubes goes out.
Accompanying drawing illustrates:
Fig. 1 is to be applicable to the installation drawing that element evaporation thing is formed；
Fig. 2 is the installation drawing being applicable to the formation of element evaporation thing with nebulizer；
1, the ingress pipe of dithiocarbonic acid (salt) solution of sample solution ingress pipe 2, amino-contained
3, peristaltic pump 4, tee T gas-liquid 5, separator
6, carrier gas inlet 7, carrier gas outlet 8, discharging of waste liquid pipe
9, nebulizer.
Detailed description of the invention
In order to explain enforcement of the present utility model more fully, it is provided that following of the present utility model prepare embodiment.This
A little embodiments are only to explain rather than limit scope of the present utility model.
Embodiment 1
(1) respectively preparation containing element gold, silver sample solution (constituent content is 500ppb, nitric acid acidity 0.4 M) and
Sodium diethyldithiocarbamate (cupferron, the DDTC) solution of 2.0%, then uses peristaltic pump respectively with 3 ml/min
Flow velocity extract above-mentioned two solution, make two solution react after converging in a tee T.
(2) the element evaporation thing produced and reacted solution are separated in a gas-liquid separator；
(3) reactant liquor flowed out from threeway outlet is flowed into a gas-liquid separator immediately, here by bubbling or
The mode of spraying, isolated element evaporation thing (DDTC and the complex of element).It is former that this volatile matter is imported into atomic spectrograph
Sonization or ionizer carry out spectrum or mass spectroscopy.Measured Element sensitivity is that under identical conditions, solution does not contains DDTC
Time 25-40 times.The sensitivity tool of visible mensuration improves a lot.Figure of description 1. is shown in diagram in detail
Embodiment 2
(1) sample solution containing elemental nickel and cobalt (constituent content is 500ppb, nitric acid acidity 0.15M) and 2.0% is made
Sodium tetramethylenedithiocarbamate (APDC) solution, then uses peristaltic pump to extract with the flow velocity of 4 ml/min respectively
State two solution, make two solution react after converging in a tee T.
(2) the element evaporation thing produced and reacted solution are separated in a gas-liquid separator；
(3) survey during isolated volatile gases hydride is imported into an inductively coupled plasma atomic emission spectrum
Fixed.Measured Element sensitivity be under identical conditions solution without 26 times under the conditions of APDC.Use the nickel that the method obtains
Cobalt detection line is respectively 1ng/ml.Figure of description 1. is shown in diagram in detail
Embodiment 3
In 25 milliliters of test tubes, equipped with 2 milliliters containing element zinc and cadmium sample solution (constituent content is 500ppb,
Nitric acid acidity 0.25M), open carrier gas and make solution bubbling, now rapidly join the sodium diethyldithiocarbamate of 3%
(DDTC) solution, starts atomic fluorescence of zero dispersion photometer simultaneously and is measured.The detection limit obtaining zinc cadmium is respectively 0.01 He
0.005ppb. and when being not added with DDTC, zinc cadmium does not has any signal to occur.
Embodiment 4
(1) sample solution containing element palladium and ruthenium (constituent content is 200ppb, nitric acid acidity 0.4M) and 4.0% is made
Sodium tetramethylenedithiocarbamate (APDC) solution, then uses peristaltic pump to extract with the flow velocity of 4 ml/min respectively
State two solution, make two solution react after converging in a tee T.
(2) the element evaporation thing produced and reacted solution are separated in a gas-liquid separator；
(3) measure during isolated volatile gases hydride is imported into a flame atomic absorption spectrophotometer.Measured
Element sensitivity be under identical conditions solution without 20 and 17 times under the conditions of APDC.Use palladium and the ruthenium inspection of the method acquisition
Outlet is respectively 2ng/ml.Figure of description 2 is shown in diagram in detail.
Embodiment 5
(1) sample solution containing elements La and hydrargyrum (constituent content is 200ppb, nitric acid acidity 0.15M) and 4.0% is made
Sodium tetramethylenedithiocarbamate (APDC) solution, then uses peristaltic pump to extract with the flow velocity of 3 ml/min respectively
State two solution, make two solution react after converging in a tee T.
(2) by produce element evaporation thing and reacted solution through inductively coupled plasma atomic emission spectrum
(ICP-AES) separate in a Scott fog chamber after nebulizer (25PSI pressure) spraying；
(3) measure during isolated volatile gases hydride is imported into a flame atomic absorption spectrophotometer.Measured
Element sensitivity be under identical conditions solution without 20 and 17 times under the conditions of APDC.Use lanthanum and and the hydrargyrum of the method acquisition
Detection line is respectively 5 and 7 ng/ml.Figure of description 2 is shown in diagram in detail.
Embodiment 6
(1) preparation contains element arsenic and the sample solution (constituent content is 500ppb, nitric acid acidity 0.20 M) of scandium respectively
Sodium diethyldithiocarbamate (cupferron, DDTC) solution with 2.0%, then uses peristaltic pump respectively with 3 ml/min
The flow velocity of clock extracts above-mentioned two solution, makes two solution react after converging in a tee T.
(2) the element evaporation thing produced and reacted solution are separated in a gas-liquid separator；
(3) reactant liquor flowed out from threeway outlet is flowed into a gas-liquid separator immediately, here by bubbling or
The mode of spraying, isolated element evaporation thing (DDTC and the complex of element).It is former that this volatile matter is imported into atomic spectrograph
Sonization or ionizer carry out spectrum or mass spectroscopy.Measured Element sensitivity is that under identical conditions, solution does not contains DDTC
Time 25-40 times.The sensitivity tool of visible mensuration improves a lot.Figure of description 1 is shown in diagram in detail.
Embodiment 7
A kind of device formed for element evaporation thing, it is characterised in that this device includes that the sample solution containing element imports
Pipe 1, the ingress pipe 2 of dithiocarbonic acid (salt) solution of amino-contained, peristaltic pump 3, tee T 4, gas-liquid separator 5, carrier gas inlet
6, carrier gas outlet 7 and discharging of waste liquid pipe 8；Wherein converge in tee T after two solution of peristaltic pump pumps and react, the most just
Being threeway 4 while being connected with peristaltic pump 3, another side is connected with gas-liquid separator 5, and gas-liquid separator 5 lower end is provided with carrier gas inlet
6, upper end is provided with carrier gas outlet 7, is provided with discharging of waste liquid pipe 8 in gas-liquid separator.Separate the waste liquid of volatile gas by peristaltic pump
Band influencing meridian discharging of waste liquid bank of tubes goes out.
After the preferred embodiment described in detail, it is familiar with this skilled worker and is clearly understood that, without departing from above-mentioned
Can carry out various change and amendment under claim and spirit, all implement above according to technical spirit of the present utility model
Any simple modification, equivalent variations and the modification that example is made, belongs to the scope of technical solutions of the utility model.
Claims (1)
1. the device formed for element evaporation thing, it is characterised in that this device includes the sample solution ingress pipe containing element
(1), the ingress pipe (2) of dithiocarbonic acid (salt) solution of amino-contained, peristaltic pump (3), tee T (4), gas-liquid separator (5),
Carrier gas inlet (6), carrier gas outlet (7) and discharging of waste liquid pipe (8)；Wherein threeway (4) while being connected with peristaltic pump (3), another side
Being connected with gas-liquid separator (5), gas-liquid separator (5) lower end is provided with carrier gas inlet (6), and upper end is provided with carrier gas outlet (7), gas-liquid
Discharging of waste liquid pipe (8) it is provided with in separator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620746395.4U CN205844171U (en) | 2016-07-15 | 2016-07-15 | A kind of device formed for element evaporation thing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620746395.4U CN205844171U (en) | 2016-07-15 | 2016-07-15 | A kind of device formed for element evaporation thing |
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| CN205844171U true CN205844171U (en) | 2016-12-28 |
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| CN201620746395.4U Expired - Fee Related CN205844171U (en) | 2016-07-15 | 2016-07-15 | A kind of device formed for element evaporation thing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106226252A (en) * | 2016-07-15 | 2016-12-14 | 天津师范大学 | The forming method of a kind of element evaporation thing and device |
| CN108426873A (en) * | 2018-03-09 | 2018-08-21 | 中国科学院海洋研究所 | A kind of detection method and dedicated unit of hydride |
-
2016
- 2016-07-15 CN CN201620746395.4U patent/CN205844171U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106226252A (en) * | 2016-07-15 | 2016-12-14 | 天津师范大学 | The forming method of a kind of element evaporation thing and device |
| CN108426873A (en) * | 2018-03-09 | 2018-08-21 | 中国科学院海洋研究所 | A kind of detection method and dedicated unit of hydride |
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161228 Termination date: 20190715 |
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| CF01 | Termination of patent right due to non-payment of annual fee |