CN104028174B - The chemical evapn generating means of multielement and method thereof - Google Patents
The chemical evapn generating means of multielement and method thereof Download PDFInfo
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Abstract
The chemical evapn generating means of multielement provided by the invention and method for generation thereof.This chemical evapn generating means, comprise imbibition portion, liquid storing part, at least one suction pumps, push away liquid pump portion, reducing agent pumping section, gas-liquid separation portion, carrier gas portion and mist output interface, imbibition portion, liquid storing part, push away liquid pump portion, reducing agent pumping section, gas-liquid separation portion, carrier gas portion respectively have multiple passage, identical and the respective passage of the number of channels that various piece has is communicated with correspondingly, and number of channels is identical with the kind quantity need carrying out the element of chemical evapn generation.This invention ensures that when multiple element detects simultaneously, for accuracy and the reliability of often kind of Element detection, and shorten analysis time, decrease analysis cost, improve analysis efficiency.
Description
Technical field
The present invention relates to analytical chemistry field, particularly relate to chemical evapn generating means and the method thereof of multielement.
Background technology
Chemical evapn method for generation utilizes chemical reaction to make determinand form the gaseous compound of volatilization, and belonging to gas sampling technology, is improve sensitivity for analysis and optionally effective way.The method comprises hydride occurring mode, mercury vapour occurring mode and other volatile matter occurring mode.Hydride occurring mode is widely used in the trace element analysis such as As, Sb, Bi, Se, Te, Pb, Sn, Ge.Produce covalently bound molecular gas compound-hydride after these elements and reducing agent react, this hydride has very low boiling point, is gas at normal temperatures.Mercury vapour occurring mode is used for analytical element Hg, and the Hg2+ in solution is reduced into volatile atoms state mercury by reducing agent, the vapour pressure of mercury very high (being about 0.0016MPa when 20 DEG C) when room temperature.Other volatile matter occurring mode is used for analytical element Zn, Cd, Au, Ag, Cu etc., and under the condition having reinforcing agent, these elements and reducing agent react and can produce the very high volatile gaseous compound of luminous efficiency.These three kinds of occurring modes produce chemical reaction character difference during gaseous material, the physical property of gaseous products also has larger difference, therefore the generation efficiency of reaction condition to gaseous material carried out when chemical evapn reacts has a significant impact, only have and react under optimum conditions, the gaseous material that often kind of element ability generation efficiency is the highest.The condition affecting the chemical evapn luminous efficiency of element has determinand solution medium, reducing agent, solution flow rate, carrier gas flux, reaction compartment etc.
Realizing element chemistry steam in currently available technology to react, is completed by unipath reaction system.This reaction system is made up of single path imbibition portion, single path liquid storing part, single path gas-liquid separation portion and interconnective single path pipeline.The different optimum reaction condition needs of often kind of element cannot be met simultaneously, simple optimum organization can only be carried out by the partial reaction condition of the element to limited kinds.Such as, Li Haitao etc. (" trace arsenic, antimony, selenium and mercury in chemical evapn generation-four-way atomic fluorescence spectrometry Simultaneously test water sample ", " assay laboratory ", 28th volume the 4th phase, in April, 2009,9-13 page) report As, Hg, Se, Sb tetra-kinds of elements in applied chemistry steam method for generation and atomic fluorescence coupling Simultaneously test water sample.Within 2012, Ni meets auspicious grade (" trace As, Sb, Bi, Te in chemical evapn generation-four-way atomic fluorescence spectrometry Simultaneously test High Purity Gold ", " assay laboratory ", 50th volume the 7th phase, in July, 2012,58-60 page) report As, Sb, Bi, Te tetra-kinds of elements utilized in chemical evapn method for generation and atomic fluorescence coupling Simultaneously test High Purity Gold.The element chemistry steam method for generation of these two sections of documents has just carried out the optimum organization of phase recency in the reaction system of unipath for the reaction condition of used solution acidity, medium solution, reducing agent, carrier gas flux for wherein corresponding four kinds of elements.In fact, even consider all reaction conditions needing to optimize, because optimum organization itself is a kind of compromise mode, cannot reach for each element use optimum condition corresponding thereto, moreover in actual applications the very large element of reaction condition difference is realized carrying out simultaneously that chemical evapn reacts is extremely difficult, in addition, the needs usually of groping for optimal conditions make repeated attempts, and waste time and energy.
In order to solve the defect of said method, realizing more Simultaneous multi element analysis, having and improving to improve accuracy and reliability to the chemical evapn system of reacting.Such as, the applying date is on November 18th, 2011, and publication date is the Chinese invention patent application CN102519922A(application number on June 27th, 2012: 201110369625.1) developed the reducing agent utilizing multiple reducing agent input to control many variable concentrations-media on the basis of existing technology and realized each concentration of element in Simultaneously test sample.This method just meets the difference needs of multielement for reducing agent condition, but do not relate to for current-carrying and solution medium to be measured, solution flow rate, the impact of other conditions many such as carrier gas flux and reaction compartment, and the course of reaction of often kind of element needs to repeat, namely, can only can enter the operation of lower a kind of element after to a kind of element complete operation process, although improve accuracy and the reliability of detection to a certain extent, but really do not realize multielement and produce gaseous material simultaneously, and add analysis time, improve analysis cost, analysis efficiency is lower.
Summary of the invention
The invention reside in solve in prior art and cannot realize multielement and produce the technical problem that gaseous material, detection accuracy and reliability are low, analysis time is long, analysis cost is high, analysis efficiency is low simultaneously.
The invention provides a kind of chemical evapn generating means of multielement, comprise imbibition portion, liquid storing part, at least one suction pumps, push away liquid pump portion, reducing agent pumping section, gas-liquid separation portion, carrier gas portion and mist output interface, imbibition portion, liquid storing part, push away liquid pump portion, reducing agent pumping section, gas-liquid separation portion, carrier gas portion respectively has multiple passage, identical and the respective passage of the number of channels that various piece has is communicated with correspondingly, number of channels is identical with the kind quantity need carrying out the element of chemical evapn generation, each passage of liquid storing part comprises the first triple valve be communicated with successively, liquid storage ring and the second triple valve, the output in imbibition portion, the output pushing away liquid pump portion is communicated with the input of the first triple valve, the output of the second triple valve is communicated with the input in the input of suction pumps and gas-liquid separation portion, reducing agent pumping section is communicated with the input in gas-liquid separation portion, carrier gas portion is communicated with gas-liquid separation portion, gaseous mixture output interface is communicated with the output in gas-liquid separation portion.
In one embodiment, chemical evapn generating means comprises a suction pumps and one-to-many dispenser, and imbibition portion comprises an aspirating needle and one-to-many dispenser, and suction pumps and one-to-many dispenser, aspirating needle are all optionally be communicated with one-to-many dispenser.
In one embodiment, imbibition portion comprises at least two aspirating needles and at least two passages that are connected, and this chemical evapn generating means comprises at least two suction pumps, and each suction pumps corresponds to a passage in imbibition portion.
In one embodiment, suction pumps is single channel syringe pump.
In one embodiment, imbibition portion comprises at least two aspirating needles and at least two passages that are connected, and this chemical evapn generating means comprises a multichannel suction pumps, each passage of multichannel suction pumps and each passage one_to_one corresponding in imbibition portion.
In one embodiment, this multichannel suction pumps is multi-channel peristaltic pump.
In one embodiment, push away liquid pump portion and comprise one and push away liquid pump and multiple passage, the caliber of each passage is different.
The present invention also provides a kind of chemical evapn method for generation of multielement, adopts above-mentioned chemical evapn generating means, comprises the steps:
(1) liquid to be measured is mixed with medium solution respectively, in order to be mixed with multiple mixed solution;
(2) adjust the first triple valve and the second triple valve, make imbibition portion, liquid storing part is communicated with suction pumps, start suction pumps, above-mentioned multiple mixed solution is sucked via imbibition portion in the corresponding liquid storage ring of liquid storing part;
(3) again adjust the first triple valve and the second triple valve, make to push away liquid pump portion, liquid storing part is communicated with gas-liquid separation unit, start and push away liquid pump portion, the mixed solution in each liquid storage ring is pushed in the respective channel in gas-liquid separation portion with required flow rate;
(4) start reducing agent pumping section, each reductant solution is passed in the respective channel in gas-liquid separation portion;
(5) each mixed solution and each reductant solution fully react and produce gas in the passage in gas-liquid separation portion, open carrier gas portion, pass in the respective channel of gas-liquid separation by carrier gas with required flow;
(6) gas produced through each passage in gas-liquid separation portion that carrier gas is taken out of is collected at gaseous mixture output interface.
In one embodiment, in step (2), imbibition portion comprises an aspirating needle and one-to-many dispenser, aspirating needle is inserted after in a kind of mixed solution and start suction pumps, above-mentioned mixed solution is sucked in a liquid storage ring of liquid storing part, successively aspirating needle to be inserted in different mixed solutions and to be optionally communicated with one-to-many dispenser by aspirating needle, making suction pumps draw mixed solution successively in the corresponding liquid storage ring of liquid storing part.
In one embodiment, in step (2), imbibition portion comprises at least two aspirating needles and at least two passages that are connected, is inserted by each aspirating needle after in each mixed solution and starts suction pumps, draws mixed solution in the corresponding liquid storage ring of liquid storing part simultaneously or successively.
In one embodiment, for the liquid to be measured containing As element, medium solution in step (1) contains 5 ~ 20%v/v hydrochloric acid and 0.5 ~ 2%w/v thiocarbamide, the flow velocity of mixed solution is in step (3) 3 ~ 5mL/min, reductant solution in step (4) contains 1 ~ 2%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 350mL/min.
In one embodiment, for the liquid to be measured containing Hg element, medium solution in step (1) contains 5 ~ 20%v/v nitric acid, the flow velocity of mixed solution is in step (3) 4 ~ 6mL/min, reductant solution in step (4) contains 0.01 ~ 1%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 400mL/min.
In one embodiment, for the liquid to be measured containing Pb element, medium solution in step (1) contains 1 ~ 2%v/v hydrochloric acid, the flow velocity of mixed solution is in step (3) 2 ~ 4mL/min, reductant solution in step (4) contains 1.5 ~ 3%w/v potassium borohydride, 0.5 ~ 1%w/v NaOH and 1 ~ 2%w/v potassium ferricyanide, and the carrier gas flux in step (5) is 300mL/min.
In one embodiment, for the liquid to be measured containing Ge element, medium solution in step (1) contains 5 ~ 30%v/v phosphoric acid, the flow velocity of mixed solution is in step (3) 3 ~ 4mL/min, reductant solution in step (4) contains 1 ~ 2%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 350mL/min.
In one embodiment, for the liquid to be measured containing Cd element, medium solution in step (1) contains 1 ~ 2%v/v hydrochloric acid, 0.5 ~ 1.5 μ g/mLCo
2+, 0.5 ~ 2%w/v thiocarbamide, the flow velocity of mixed solution is in step (3) 2 ~ 4mL/min, reductant solution in step (4) contains 1 ~ 3%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 330mL/min.
Chemical evapn generating means provided by the invention and method for generation thereof, can simultaneously for multielement, meet the different requirements of often kind of element for many reaction conditions such as current-carrying and determinand solution medium, reducing agent, solution flow rate, reaction compartments, not only ensure the accuracy for often kind of Element detection and reliability, and the multielement analysis time can be shortened, decrease analysis cost, improve analysis efficiency.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the chemical evapn generating means of multielement in the present invention.
Fig. 2 is the flow chart of the chemical evapn method for generation of multielement in the present invention.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail, should be understood that given embodiment only plays illustrational object, be not intended to limit the scope of the invention.
The invention provides the chemical evapn generating means of multielement, comprising: imbibition portion 11, liquid storing part 12, at least one suction pumps 13, push away liquid pump portion 14, reducing agent pumping section 20, gas-liquid separation portion 30, carrier gas portion 40 and mist output interface 50.Wherein, imbibition portion 11, liquid storing part 12, push away liquid pump portion 14, reducing agent pumping section 20, gas-liquid separation portion 30, carrier gas portion 40 respectively have multiple passage (at least two passages), identical and the respective passage of the number of channels that various piece has is communicated with correspondingly, and number of channels is identical with the kind quantity need carrying out the element of chemical evapn generation.Specifically, each passage of liquid storing part 12 comprises the first triple valve 121, liquid storage ring 122 and the second triple valve 123 that are communicated with successively.The output in imbibition portion 11, the output pushing away liquid pump portion 14 are communicated with the input of the first triple valve 121, the output of the second triple valve 123 is communicated with the input of at least one suction pumps 13 and the input in gas-liquid separation portion 30, reducing agent pumping section 20 is communicated with the input in gas-liquid separation portion 30, carrier gas portion 40 is communicated with gas-liquid separation portion 30, and gaseous mixture output interface 50 is communicated with the output in gas-liquid separation portion 30.
In one embodiment, imbibition portion 11 comprises an aspirating needle and one-to-many dispenser.Chemical evapn generating means comprises a suction pumps 13 and one-to-many dispenser, and suction pumps 13 is a single channel pump (being such as single channel injection pumping section).Aspirating needle and one-to-many dispenser, suction pumps 13 are all optionally be communicated with one-to-many dispenser, suction pumps 13 in order to imbitition successively in the respective channel of liquid storing part 12.In another embodiment, imbibition portion 11 comprises the multiple aspirating needle and multiple passage that are connected.This chemical evapn generating means comprises multiple suction pumps 13, and each suction pumps 13 corresponds to a passage in imbibition portion, in order to simultaneously or successively imbitition in the respective channel of liquid storing part 12.In another embodiment again, imbibition portion 11 comprises the multiple aspirating needle and multiple passage that are connected.This chemical evapn generating means comprises a suction pumps 13, this suction pumps 13 is a multi-channel pump (being such as multi-channel peristaltic pump), each passage of multichannel suction pumps and each passage one_to_one corresponding in imbibition portion 11, in order to simultaneously or successively imbitition in the respective channel of liquid storing part 12.
Push away liquid pump portion 14 to comprise one and push away liquid pump and multiple passage, the caliber of each passage is different, in order to adjust the flow velocity of liquid in each passage.
Carrier gas portion 40 can in order to provide identical or different carrier gas flux.
The present invention also provides the chemical evapn method for generation of multielement, comprises the steps:
(1) liquid to be measured is mixed with medium solution respectively, in order to be mixed with multiple mixed solution;
(2) adjust the first triple valve 121 and the second triple valve 123, make imbibition portion 11, liquid storing part 12 is communicated with suction pumps 13, start suction pumps 13, above-mentioned multiple mixed solution is sucked in the corresponding liquid storage ring 122 of liquid storing part 12 via imbibition portion 11;
(3) the first triple valve 121 and the second triple valve 123 is again adjusted, make to push away liquid pump portion 14, liquid storing part 12 is communicated with gas-liquid separation unit 30, start and push away liquid pump portion 14, the mixed solution in each liquid storage ring 122 is pushed in the respective channel in gas-liquid separation portion 30 with required flow rate;
(4) start reducing agent pumping section 20, each reductant solution is passed in the respective channel in gas-liquid separation portion 30;
(5) each mixed solution and each reductant solution fully react and produce gas in the passage in gas-liquid separation portion 30, open carrier gas portion 40, carrier gas are passed into required flow in the respective channel of gas-liquid separation 30;
(6) collect at gaseous mixture output interface 50 gas that each passage in gas-liquid separation portion 30 taken out of through carrier gas produces.
In an embodiment of step (2), imbibition portion 11 comprises an aspirating needle and one-to-many dispenser, aspirating needle is inserted after in a kind of mixed solution and start suction pumps 13, above-mentioned mixed solution is sucked in the liquid storage ring of liquid storing part 12, successively aspirating needle to be inserted in different mixed solutions and to be optionally communicated with one-to-many dispenser by aspirating needle, making suction pumps 13 draw mixed solution successively in the corresponding liquid storage ring of liquid storing part 12.
In another embodiment of step (2), imbibition portion 11 comprises at least two aspirating needles and at least two passages that are connected, each aspirating needle is inserted after in each mixed solution and start suction pumps 13, draw mixed solution in the corresponding liquid storage ring of liquid storing part 12 simultaneously or successively.
In step (3), the optimum response speed of each mixed solution of the selection gist of flow velocity.
In step (4), the selection gist of reductant solution for the character of reactive element.
After step (6), method provided by the invention by by gaseous mixture output interface 50, with Instrument crosslinkings such as AFS, electrothermal quartz tube atomization Atomic Absorption Spectrometer, inductively coupled plasma atomic emission spectrometer, icp mses.
Chemical evapn generating means provided by the invention and method for generation thereof, can simultaneously for multielement, meet the different requirements of often kind of element for many reaction conditions such as current-carrying and determinand solution medium, reducing agent, solution flow rate, reaction compartments, not only ensure the accuracy for often kind of Element detection and reliability, and the multielement analysis time can be shortened, decrease analysis cost, improve analysis efficiency.
Embodiment:
For the liquid to be measured containing As, Hg, Pb, Ge, Cd five kinds of elements, chemical evapn method for generation of the present invention is described, each parts of wherein used chemical evapn generating means are all Five-channel.The reaction condition of corresponding five kinds of elements is set to as follows, and measures with AFS coupling.
Reaction condition for As element:
Medium solution contains 5% ~ 20%(v/v) hydrochloric acid and 0.5% ~ 2% (w/v) thiocarbamide;
The propelling movement flow velocity of the mixed solution of liquid to be measured and medium solution is 3 ~ 5mL/min;
Reductant solution contains 1% ~ 2% (w/v) potassium borohydride and 0.5% ~ 1% (w/v) NaOH;
Carrier gas flux is 350mL/min.
Reaction condition for Hg element:
Medium solution contains 5% ~ 20%(v/v) nitric acid;
The propelling movement flow velocity of the mixed solution of liquid to be measured and medium solution is 4 ~ 6mL/min;
Reductant solution contains 0.01% ~ 1% (w/v) potassium borohydride and 0.5% ~ 1% (w/v) NaOH;
Carrier gas flux is 400mL/min.
Reaction condition for Pb element:
Medium solution contains 1% ~ 2%(v/v) hydrochloric acid;
The flow velocity of the mixed solution of liquid to be measured and medium solution is 2 ~ 4mL/min;
Reductant solution contains 1.5% ~ 3% (w/v) potassium borohydride, 0.5% ~ 1% (w/v) NaOH, 1% ~ 2% (w/v) potassium ferricyanide;
Carrier gas flux is 300mL/min.
Reaction condition for Ge element:
Medium solution contains 5% ~ 30%(v/v) phosphoric acid;
The flow velocity of the mixed solution of liquid to be measured and medium solution is 3 ~ 4mL/min;
Reductant solution contains 1% ~ 2% (w/v) potassium borohydride and 0.5% ~ 1% (w/v) NaOH;
Carrier gas flux is 350mL/min.
Reaction condition for Cd element:
Medium solution contains 1% ~ 2%(v/v) hydrochloric acid, 0.5 ~ 1.5 μ g/mLCo
2+, 0.5% ~ 2% (w/v) thiocarbamide;
The flow velocity of the mixed solution of liquid to be measured and medium solution is 2 ~ 4mL/min;
Reductant solution contains 1% ~ 3% (w/v) potassium borohydride and 0.5% ~ 1% (w/v) NaOH;
Carrier gas flux is 330mL/min.
In embodiment, chemical evapn method for generation comprises the following steps:
Liquid to be measured containing As, Hg, Pb, Ge, Cd five kinds of elements is mixed with above-mentioned medium solution respectively, to be mixed with multiple mixed solution.Adjust the first triple valve 121 and the second triple valve 123, make imbibition portion 11, liquid storing part 12 is communicated with suction pumps 13, imbibition portion 11 inserts in above-mentioned mixed solution respectively.Suction pumps 13, sucks each for 1.0mL mixed solution in each liquid storage ring 122 of liquid storing part 12 via imbibition portion 11.
Adjust the first triple valve 121 and the second triple valve 123, make to push away liquid pump portion 14, liquid storing part 12 is communicated with gas-liquid separation unit 30, start and push away liquid pump portion 14, the above-mentioned each mixed solution in liquid storage ring 122 is pushed in the respective channel in gas-liquid separation portion 30 with above-mentioned flow.
Start reducing agent pumping section 20, above-mentioned each reductant solution is passed in the respective channel in gas-liquid separation portion 30.
Mixed solution and reductant solution fully react and produce gas in the passage in gas-liquid separation portion 30, open carrier gas portion 40, carrier gas is passed into above-mentioned flow velocity in the respective channel of gas-liquid separation 30, in order to export reaction gas to AFS via gaseous mixture output interface 50.The measurement result of embodiment refers to table 1.
Table 1
Comparative example:
For the liquid to be measured containing As, Hg, Pb, Ge, Cd five kinds of elements, the reaction condition of liquid to be measured is set to as follows, and measures with AFS coupling.
Chemical evapn method for generation in comparative example comprises the following steps:
Liquid to be measured containing As, Hg, Pb, Ge, Cd five kinds of elements is mixed with the medium solution containing 5% hydrochloric acid and 1% thiocarbamide.The above-mentioned mixed solution of 1.0mL is pushed in gas-liquid separation portion with the flow velocity of 2 ~ 4mL/min.Reductant solution containing 2% potassium borohydride and 0.5% NaOH is passed in gas-liquid separation portion.After fully reacting and produce gas, carrier gas is passed in gas-liquid separation with the flow of 300mL/min, in order to export reaction gas to AFS.The measurement result of comparative example refers to table 2.
Table 2
The size of the measured signal that the tested element that sensitivity represents unit concentration (or absolute magnitude) produces.In embodiment, five groups of sensitivity number are all higher than the numerical value of comparative example medium sensitivity.
To compare with comparative example measurement result through embodiment and draw, multielement measures under a kind of reaction condition, can only meet a kind of reaction requirement of element to a certain extent, can carry out Accurate Determining, then can not ensure the degree of accuracy measured for other element, even cannot measure.The present invention in operation, process for often kind of element is spatially actual is mutually isolated, make the mutual minimum interference between each path, thus the different requirements of often kind of element for many reaction conditions such as solution medium, reducing agent, solution flow rate, reaction compartments can be met, ensure that the accuracy for often kind of Element detection and reliability well, and shorten analysis time, decrease analysis cost, improve analysis efficiency.
Claims (15)
1. the chemical evapn generating means of a multielement, it is characterized in that, comprise imbibition portion, liquid storing part, at least one suction pumps, push away liquid pump portion, reducing agent pumping section, gas-liquid separation portion, carrier gas portion and mist output interface, imbibition portion, liquid storing part, push away liquid pump portion, reducing agent pumping section, gas-liquid separation portion, carrier gas portion respectively has multiple passage, identical and the respective passage of the number of channels that various piece has is communicated with correspondingly, number of channels is identical with the kind quantity need carrying out the element of chemical evapn generation, each passage of liquid storing part comprises the first triple valve be communicated with successively, liquid storage ring and the second triple valve, the output in imbibition portion, the output pushing away liquid pump portion is communicated with the input of the first triple valve, the output of the second triple valve is communicated with the input in the input of suction pumps and gas-liquid separation portion, reducing agent pumping section is communicated with the input in gas-liquid separation portion, carrier gas portion is communicated with gas-liquid separation portion, mist output interface is communicated with the output in gas-liquid separation portion.
2. chemical evapn generating means according to claim 1, it is characterized in that, chemical evapn generating means comprises a suction pumps and one-to-many dispenser, imbibition portion comprises an aspirating needle and one-to-many dispenser, and suction pumps and one-to-many dispenser, aspirating needle are all optionally be communicated with one-to-many dispenser.
3. chemical evapn generating means according to claim 1, it is characterized in that, imbibition portion comprises at least two aspirating needles and at least two passages that are connected, and this chemical evapn generating means comprises at least two suction pumps, and each suction pumps corresponds to a passage in imbibition portion.
4. chemical evapn generating means according to claim 2, is characterized in that, suction pumps is single channel syringe pump.
5. chemical evapn generating means according to claim 1, it is characterized in that, imbibition portion comprises at least two aspirating needles and at least two passages that are connected, this chemical evapn generating means comprises a multichannel suction pumps, each passage of multichannel suction pumps and each passage one_to_one corresponding in imbibition portion.
6. chemical evapn generating means according to claim 5, is characterized in that, this multichannel suction pumps is multi-channel peristaltic pump.
7. chemical evapn generating means according to claim 1, is characterized in that, pushes away liquid pump portion and comprises one and push away liquid pump and multiple passage, and the caliber of each passage is different.
8. a chemical evapn method for generation for multielement, adopts chemical evapn generating means as described in claim 1,2,4 or 7, it is characterized in that, comprise the steps:
(1) liquid to be measured is mixed with medium solution respectively, in order to be mixed with multiple mixed solution;
(2) adjust the first triple valve and the second triple valve, make imbibition portion, liquid storing part is communicated with suction pumps, start suction pumps, above-mentioned multiple mixed solution is sucked via imbibition portion in the corresponding liquid storage ring of liquid storing part;
(3) again adjust the first triple valve and the second triple valve, make to push away liquid pump portion, liquid storing part is communicated with gas-liquid separation unit, start and push away liquid pump portion, the mixed solution in each liquid storage ring is pushed in the respective channel in gas-liquid separation portion with required flow rate;
(4) start reducing agent pumping section, each reductant solution is passed in the respective channel in gas-liquid separation portion;
(5) each mixed solution and each reductant solution fully react and produce gas in the passage in gas-liquid separation portion, open carrier gas portion, pass in the respective channel of gas-liquid separation by carrier gas with required flow;
(6) gas produced through each passage in gas-liquid separation portion that carrier gas is taken out of is collected at mist output interface.
9. chemical evapn method for generation as claimed in claim 8, it is characterized in that, in step (2), imbibition portion comprises an aspirating needle and one-to-many dispenser, aspirating needle is inserted after in a kind of mixed solution and start suction pumps, above-mentioned mixed solution is sucked in a liquid storage ring of liquid storing part, successively aspirating needle to be inserted in different mixed solutions and to be optionally communicated with one-to-many dispenser by aspirating needle, making suction pumps draw mixed solution successively in the corresponding liquid storage ring of liquid storing part.
10. chemical evapn method for generation according to claim 8, it is characterized in that, in step (2), imbibition portion comprises at least two aspirating needles and at least two passages that are connected, each aspirating needle is inserted after in each mixed solution and start suction pumps, draw mixed solution in the corresponding liquid storage ring of liquid storing part simultaneously or successively.
11. chemical evapn method for generation as claimed in claim 8, it is characterized in that, for the liquid to be measured containing As element, medium solution in step (1) contains 5 ~ 20%v/v hydrochloric acid and 0.5 ~ 2%w/v thiocarbamide, the flow velocity of the mixed solution in step (3) is 3 ~ 5mL/min, reductant solution in step (4) contains 1 ~ 2%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 350mL/min.
12. chemical evapn method for generation as claimed in claim 8, it is characterized in that, for the liquid to be measured containing Hg element, medium solution in step (1) contains 5 ~ 20%v/v nitric acid, the flow velocity of the mixed solution in step (3) is 4 ~ 6mL/min, reductant solution in step (4) contains 0.01 ~ 1%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 400mL/min.
13. chemical evapn method for generation as claimed in claim 8, it is characterized in that, for the liquid to be measured containing Pb element, medium solution in step (1) contains 1 ~ 2%v/v hydrochloric acid, the flow velocity of the mixed solution in step (3) is 2 ~ 4mL/min, reductant solution in step (4) contains 1.5 ~ 3%w/v potassium borohydride, 0.5 ~ 1%w/v NaOH and 1 ~ 2%w/v potassium ferricyanide, and the carrier gas flux in step (5) is 300mL/min.
14. chemical evapn method for generation as claimed in claim 8, it is characterized in that, for the liquid to be measured containing Ge element, medium solution in step (1) contains 5 ~ 30%v/v phosphoric acid, the flow velocity of the mixed solution in step (3) is 3 ~ 4mL/min, reductant solution in step (4) contains 1 ~ 2%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 350mL/min.
15. chemical evapn method for generation as claimed in claim 8, is characterized in that, for the liquid to be measured containing Cd element, the medium solution in step (1) contains 1 ~ 2%v/v hydrochloric acid, 0.5 ~ 1.5 μ g/mLCo
2+, 0.5 ~ 2%w/v thiocarbamide, the flow velocity of the mixed solution in step (3) is 2 ~ 4mL/min, reductant solution in step (4) contains 1 ~ 3%w/v potassium borohydride and 0.5 ~ 1%w/v NaOH, and the carrier gas flux in step (5) is 330mL/min.
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| CN201310068033.5A Active CN104028174B (en) | 2013-03-04 | 2013-03-04 | The chemical evapn generating means of multielement and method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810349A (en) * | 2005-01-26 | 2006-08-02 | 北京吉天仪器有限公司 | Gas-liquid separator |
| CN2876767Y (en) * | 2006-01-06 | 2007-03-07 | 徐培实 | Vapour absorption type spectrophotometer |
| CN101609046A (en) * | 2009-07-23 | 2009-12-23 | 江苏天瑞仪器股份有限公司 | A kind of sample introduction and hydride generation process and system that is used for atomic fluorescence spectrometer |
| CN202110138U (en) * | 2011-07-04 | 2012-01-11 | 西北有色地质研究院 | Solid sample feeding and atomic fluorescence combined device |
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| JPS6011141A (en) * | 1983-06-30 | 1985-01-21 | Shimadzu Corp | Hydride generating apparatus |
| JP4095360B2 (en) * | 2002-07-10 | 2008-06-04 | Ｔｄｋ株式会社 | Elemental analysis method and elemental analysis apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810349A (en) * | 2005-01-26 | 2006-08-02 | 北京吉天仪器有限公司 | Gas-liquid separator |
| CN2876767Y (en) * | 2006-01-06 | 2007-03-07 | 徐培实 | Vapour absorption type spectrophotometer |
| CN101609046A (en) * | 2009-07-23 | 2009-12-23 | 江苏天瑞仪器股份有限公司 | A kind of sample introduction and hydride generation process and system that is used for atomic fluorescence spectrometer |
| CN202110138U (en) * | 2011-07-04 | 2012-01-11 | 西北有色地质研究院 | Solid sample feeding and atomic fluorescence combined device |
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