Pneumatic atomization-chemical vapor generation multifunctional integrated sampling device suitable for ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometer)

Abstract

The utility model discloses a pneumatic atomization-chemical vapor generation multifunctional integrated sampling device suitable for ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometer), which comprises an atomizing chamber, wherein a waste liquid outlet is formed in the bottom of the atomizing chamber; the reaction platform is arranged in the atomizing chamber; the reducing agent sampling pipe is mounted on the atomizing chamber, and the lower end of the reducing agent sampling pipe extends to the reaction platform; an acidified sample inlet and an argon inlet are formed in the atomizer, and the atomizer is mounted on the atomizing chamber; the outlet pipe is mounted on the atomizing chamber, and the lower end of the outlet pipe extends into the atomizing chamber and is positioned above the reaction platform. The device disclosed by the utility model can realize the functions of pneumatic atomization sample injection and chemical vapor generation sample injection by using the same set of device, and is suitable for simultaneous determination of elements which are easy to form chemical vapor such as hydrides and other elements which are not easy to form chemical vapor; the detection sensitivity of elements easy to form chemical vapor can be remarkably improved, and the detection sensitivity of other elements is not reduced.

Description

Technical Field

[0001] The utility model relates to a pneumatic atomization - chemical vapor generation multi - functional integrated sampling device applicable to ICP - OES, belonging to the technical field of spectral detection devices. Background Technique

[0002] Traditional pneumatic atomization sampling is still the most common sampling method for commercial instruments. The solution sample is transformed into aerosol droplets by a pneumatic nebulizer and transmitted into the inductively coupled plasma. This sampling method is simple to operate and has good stability. However, the sample atomization and transmission efficiency are low (about 1% - 5%), and a large amount of matrix impurities will be introduced, reducing the analysis sensitivity.

[0003] Chemical vapor generation sampling directly generates chemical vapors or atomic vapors such as volatile hydrides of heavy metals or transition metal elements (such as Hg) through chemical reactions, effectively separating them from the matrix. It is an efficient sampling method for introducing elements to be measured into spectral instruments for analysis (generally, the gaseous sampling efficiency is considered to be close to 100%), and can meet the quantitative analysis requirements of trace and ultra - trace elements. Analytical methods represented by the "chemical vapor generation - atomic fluorescence spectrophotometry" method have become the conventional means for analyzing elements such as arsenic (As), mercury (Hg), selenium (Se), antimony (Sb), tin (Sn), cadmium (Cd), tellurium (Te), lead (Pb), germanium (Ge), bismuth (Bi), zinc (Zn), etc. in domestic laboratories. However, the applicable range of this method is currently limited to about ten elements that are easy to form hydrides and cold vapor elements.

[0004] The two sampling methods each have their own characteristics, advantages and disadvantages. Combining the two sampling methods can achieve complementary functions. Currently, mainstream instruments are equipped with pneumatic atomization sampling devices, and at the same time, chemical vapor generation sampling devices can also be selected separately; the sampling method can be selected according to needs to analyze and detect different elements. During the actual detection process, the replacement of the two sampling devices will cause the plasma to extinguish, and it is necessary to re - ignite and pre - heat to stabilize before testing another sampling method. In this way, when two sampling methods are required for separate detection, the detection efficiency is greatly reduced. Content of the Utility Model

[0005] The purpose of the utility model is to provide a pneumatic atomization - chemical vapor generation multi - functional integrated sampling device applicable to ICP - OES in view of the problems existing in the prior art. The utility model can use the same set of devices to realize the functions of pneumatic atomization sampling and chemical vapor generation sampling, is applicable to the simultaneous determination of elements that are easy to form chemical vapors such as hydrides and other elements that are not easy to form chemical vapors, and can significantly improve the detection sensitivity of elements that are easy to form chemical vapors without reducing the detection sensitivity of other elements.

[0006] The technical solution provided by the present utility model to solve the above technical problems is: A pneumatic atomization - chemical vapor generation multi - functional integrated sampling device applicable to ICP - OES, comprising:

[0007] An atomization chamber, with a waste liquid outlet provided at the bottom of the atomization chamber;

[0008] A reaction platform, which is arranged inside the atomization chamber;

[0009] A reductant injection tube, which is installed on the atomization chamber, and its lower end extends to the reaction platform;

[0010] An atomizer, which is provided with an acidified sample injection port and an argon gas inlet, and is installed on the atomization chamber;

[0011] An outlet tube, which is installed on the atomization chamber, and its lower end extends into the atomization chamber and is located above the reaction platform.

[0012] A further technical solution is that the atomization chamber is a corrosion - resistant atomization reaction chamber.

[0013] A further technical solution is that the atomization chamber includes an atomization reaction chamber with a cylindrical or hemispherical inner cavity and a conical liquid discharge chamber, and the atomization reaction chamber is threadedly connected to the liquid discharge chamber.

[0014] A further technical solution is that the atomizer, the outlet tube, and the reductant injection tube are all installed on the atomization chamber through threaded interfaces.

[0015] A further technical solution is that the threaded interface is a polytetrafluoroethylene threaded interface.

[0016] A further technical solution is that the atomizer, the outlet tube, and the reductant injection tube are respectively located at the upper left side, the top, and the upper right side of the atomization chamber.

[0017] A further technical solution is that the reaction platform is a reaction circular plate, and four liquid discharge holes are provided on the reaction circular plate.

[0018] A further technical solution is that a stepped structure is provided at the bottom of the inner cavity of the atomization reaction chamber, and the upper end of the liquid discharge chamber presses the reaction circular plate against the lower step surface of the stepped structure.

[0019] A further technical solution is that a sealing ring is provided between the reaction circular plate and the lower step surface of the stepped structure.

[0020] The present utility model has the following beneficial effects:

[0021] 1. It has all the functions of the currently mainstream and classic pneumatic atomization (PN) sampling;

[0022] 2. In the same set of equipment, a new chemical vapor generation (CVG) injection function is added, combining the pneumatic atomization - chemical vapor generation injection functions into one. The advantages are as follows: Without shutting down the instrument or replacing the equipment, it can be seamlessly converted from pneumatic atomization directly to chemical vapor generation devices such as hydride generators, reducing the time for replacing the equipment and repeated preheating and stabilization, and greatly improving the efficiency of testing samples;

[0023] 3. For complex samples that require pneumatic atomization injection to detect the content of most conventional elements and also need to use chemical vapor generation such as hydride generators to detect the content of less sensitive elements with low content such as mercury (Hg), arsenic (As), selenium (Se), antimony (Sb), tin (Sn), tellurium (Te), lead (Pb), germanium (Ge), bismuth (Bi), etc., it is an excellent application scenario;

[0024] 4. When two injection methods are required for a sample, such as when detecting elements such as K(Na) or B in the sample, it is advisable to first use pneumatic atomization injection. After detecting the conventional elements including K(Na) or B, then use chemical vapor generation injection to detect other elements as needed. This can save the time for flushing the residual high - concentration K(Na) or B elements. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the overall structure of the present utility model.

[0026] As shown in the figure: 1 - atomization chamber; 2 - atomizer; 3 - acidified sample injection port; 4 - argon gas inlet; 5 - outlet pipe; 6 - reductant injection pipe; 7 - waste liquid outlet; 8 - reaction platform. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0027] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are some, but not all, of the embodiments of the utility model. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present utility model without creative efforts shall fall within the protection scope of the present utility model.

[0028] In the description of the present utility model, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings. It is only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present utility model. In addition, the terms "first", "second", "third" are only used for descriptive purposes and cannot be construed as indicating or implying relative importance.

[0029] In the description of the present utility model, it should be noted that unless otherwise clearly specified and defined, the terms "installation", "connection", and "coupling" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific circumstances.

[0030] In addition, the technical features involved in different embodiments of the present utility model described below can be combined with each other as long as they do not conflict with each other.

[0031] As Figure 1 shown, a pneumatic nebulization - chemical vapor generation multi - functional integrated sampling device applicable to ICP - OES provided by the present utility model includes: an atomization chamber 1, and an atomizer 2, an outlet pipe 5, a reductant inlet pipe 6, and a waste liquid outlet 7 are respectively arranged on the upper left side, top, upper right side, and bottom of the atomization chamber 1;

[0032] A reaction platform 8 is arranged in the atomization chamber 1; the lower end of the reductant inlet pipe 6 extends to the reaction platform 8; the lower end of the outlet pipe 5 extends into the atomization chamber 1 and is located above the reaction platform 8; an acidified sample inlet 3 and an argon inlet 4 are arranged on the atomizer 2.

[0033] When the present utility model is specifically used, the upper end of the outlet pipe 5 is connected to the ICP - OES torch tube; at the beginning, under the action of the carrier gas entering from the argon inlet 4, the atomizer 2 sprays the sample solution at the acidified sample inlet 3 from an extremely fine nozzle, and the finer droplets are mixed with the carrier gas to form an aerosol, which enters the atomization chamber 1. The coarser droplets are sprayed onto the reaction platform 8. At the same time, after the coarser droplets sprayed from the pneumatic atomizer 2 directly or contact the outer wall of the lower end of the outlet pipe 5, they flow along the pipe wall to the central position of the reaction platform 8;

[0034] Then, a potassium borohydride or sodium borohydride solution is sent through the reductant inlet pipe 6 by a single - channel peristaltic pump, mixed and reacted with the sample solution on the reaction platform 8 to generate chemical vapors such as volatile hydrides and hydrogen gas, which together with the sample aerosol pass through the outlet pipe 5 of the atomization chamber 1 and enter the ICP torch tube for excitation. The reaction waste liquid flows from the reaction platform 8 along the side wall of the atomization chamber 1 into the waste liquid outlet 7 and is discharged by the action of the peristaltic pump.

[0035] In this embodiment, the atomization chamber 1 is a corrosion - resistant atomization reaction chamber made of acid - and alkali - resistant, hydrofluoric - acid - resistant corrosion - resistant plastic or other corrosion - resistant materials; the atomization chamber 1 includes upper and lower parts. The upper half is an atomization reaction chamber with a cylindrical or hemispherical inner cavity, and the lower half is a conical liquid - discharging chamber. The atomization reaction chamber is thread - connected to the liquid - discharging chamber for easy disassembly.

[0036] In this example, asFigure 1 As shown, the atomizer 2, the reductant inlet tube 6, and the outlet 5 are installed on the atomization chamber 1 through a threaded interface 9.

[0037] In this example, as Figure 1 shown, the specific structure of the reaction platform 8 is: the reaction platform 8 is a reaction disc, and four drain holes are provided on the reaction disc. The shape of the drain holes is as Figure 1 shown, and they are evenly distributed on the reaction disc; the center of the reaction disc is slightly lower than the edge by 1 mm.

[0038] In this embodiment, for the convenience of installation, a stepped structure is provided at the bottom of the inner cavity of the atomization reaction chamber, and the reaction disc is arranged between the atomization reaction chamber and the drain chamber. That is, when the atomization reaction chamber and the drain chamber are threadedly connected, the upper end surface of the drain chamber presses the reaction disc against the lower step surface of the stepped structure. When disassembling, only the drain chamber needs to be removed, and the reaction disc can also be removed.

[0039] To improve the sealing effect, a preferred implementation is that a sealing ring is provided between the reaction disc and the lower step surface of the stepped structure.

[0040] As Figure 1 shown, the pneumatic atomization and vapor generation injection functions of this embodiment can be switched or used simultaneously.

[0041] (1) Use of the pneumatic atomization injection device: Close the reductant inlet tube 6 or inject a blank reagent to achieve the same function as traditional pneumatic atomization injection.

[0042] (2) Use of the chemical vapor generation injection device: The acidified sample solution is pumped in by a peristaltic pump. Under the action of argon pressure, the sample solution generates an atomization effect like a traditional concentric atomizer (or other pneumatic atomizer), and a sample aerosol is formed at the outlet of the atomizer and enters the atomization chamber; the alkaline solution of potassium borohydride or sodium borohydride is pumped into the reaction platform 8 in the atomization chamber. In the atomization chamber 1, the hydride-forming elements in the sample aerosol and the unatomized sample droplets are mixed with the alkaline reductant solution on the platform, and a reaction occurs rapidly to generate gaseous hydrides. In the atomization chamber 1, the tiny aerosol particles and gaseous hydrides are transported into the ICP-OES torch tube through the upper port of the outlet of the atomization reaction chamber, and the relatively large aerosol particles and waste liquid are discharged through the lower outlet of the atomization chamber.

[0043] Therefore, through this pneumatic atomization - chemical vapor generation device, the purpose of simultaneously determining the hydride and non-hydride forming elements in the same sample solution is achieved, and the sensitivity of mercury (Hg) and chemical vapor elements such as arsenic (As), selenium (Se), antimony (Sb), tin (Sn), cadmium (Cd), tellurium (Te), lead (Pb), germanium (Ge), bismuth (Bi), zinc (Zn), etc. that are prone to form hydrides can be significantly improved.

[0044] As described above, there is no restriction in any form on the present utility model. Although the present utility model has been disclosed through the above embodiments, it is not intended to limit the present utility model. Any person skilled in the art can make some changes or modifications to form equivalent embodiments of equivalent changes by using the disclosed technical content within the scope of the technical solution of the present utility model. However, as long as it does not depart from the content of the technical solution of the present utility model, any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present utility model still fall within the scope of the technical solution of the present utility model.

Claims

1. A multifunctional integrated sampling device suitable for ICP-OES pneumatic atomization-chemical vapor generation, characterized in that: include: An atomization chamber (1), wherein a waste liquid outlet (7) is provided at the bottom of the atomization chamber (1); A reaction platform (8), wherein the reaction platform (8) is arranged in the atomization chamber (1); A reducing agent injection tube (6), the reducing agent injection tube (6) is installed on the atomization chamber (1), and the lower end of the reducing agent injection tube (6) extends to the reaction platform (8); An atomizer (2), wherein the atomizer (2) is provided with an acidified sample inlet (3) and an argon gas inlet (4), and is installed on the atomization chamber (1); An outlet pipe (5), the outlet pipe (5) is installed on the atomization chamber (1), and the lower end of the outlet pipe (5) extends into the atomization chamber (1) and is located above the reaction platform (8).

2. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 1, characterized in that: The atomization chamber (1) is a corrosion-resistant atomization reaction chamber.

3. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 1, characterized in that: The atomization chamber (1) comprises an atomization reaction chamber with a cylindrical or hemispherical inner cavity and a conical liquid discharge chamber, and the atomization reaction chamber is threadedly connected to the liquid discharge chamber.

4. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 1, characterized in that: The atomizer (2), the outlet pipe (5), and the reducing agent injection pipe (6) are all installed on the atomization chamber (1) via a threaded interface (9).

5. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 4, characterized in that: The threaded interface (9) is a polytetrafluoroethylene threaded interface.

6. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 4, characterized in that: The atomizer (2), the outlet pipe (5), and the reducing agent injection pipe (6) are respectively located on the upper left side, the top, and the upper right side of the atomization chamber (1).

7. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 3, characterized in that: The reaction platform (8) is a reaction circular plate, and four drainage holes are arranged on the reaction circular plate.

8. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 7, characterized in that: The bottom of the inner cavity of the atomization reaction chamber is provided with a step structure, and the upper end of the drainage chamber presses the reaction circular plate against the lower step surface of the step structure.

9. The multifunctional integrated sampling device for ICP-OES pneumatic atomization-chemical vapor generation according to claim 8, characterized in that: A sealing ring is arranged between the reaction circular plate and the lower step surface of the step structure.

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