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Method and device for generating element steam through spontaneous induction of micro-droplets

A vapor generation and micro-droplet technology, applied in the field of analytical chemical atomic spectroscopy, can solve the problems of affecting the anti-interference effect of the element to be tested, affecting the accurate determination of the element, and increasing the complexity of the device, so as to reduce the test cost, the structure is simple, and the Effects of Reagent Interference

Active Publication Date: 2020-07-10
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the sodium borohydride (potassium) / acid reduction system is easy to form volatile hydrides with a variety of non-metals and transition metals, and the reduction reaction speed is fast, and it is easy to be used in conjunction with various detection methods, but the reduction system also has shortcomings. Location: 1) Susceptible to the interference of transition metal ions in the matrix solution and reaction reagents; 2) (K)NaBH 4 The solution is unstable, and it is troublesome to prepare and use it now; 3) (K)NaBH 4 A large amount of toxic waste liquid is likely to be produced with acid and other substances, which will cause potential pollution to the environment
[0007] Plasma vapor generation also relies on the hydrogen and hydroxyl radicals produced by the decomposition of water molecules in the plasma discharge process to realize the transformation process of elements from solution ions to volatile atoms, molecules, hydrides or oxides, and also avoids the addition of redox The use of chemical reagents, but the design of the plasma discharge device will also significantly affect the anti-interference effect of the elements to be measured by coexisting ions
[0008] In summary, although these conventional chemical vapor generation methods can realize the transformation of analyte elements from solution ions to volatile substances, the redox process must rely on external factors such as chemical redox reagents, electric fields, light, ultrasound, etc. Microwave or plasma drives will not only increase the complexity of the device, but also inevitably bring about interference from external forces, which will affect the accurate determination of elements

Method used

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  • Method and device for generating element steam through spontaneous induction of micro-droplets
  • Method and device for generating element steam through spontaneous induction of micro-droplets
  • Method and device for generating element steam through spontaneous induction of micro-droplets

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Such as figure 1 For the device and process shown, a glass concentric pneumatic nebulizer is selected, the inner diameter of the central tube of the nebulizer is 0.1 mm, the Ar carrier gas pressure is 40 psi, and the pure water flow rate is 100 µL min -1 , with a flow injection loop volume of 100 µL. 1-10 µgL -1 Hg 2+ The standard solution is spontaneously reduced to volatile Hg by micro-droplets 0 , after the cold atomic fluorescence detection, the peak figure is as follows figure 2 Shown in a-d, illustrate that the method of the present invention can be used for Hg 2+ of steam is generated. at 1-10 µg L -1 Hg in range 2+ The peak area signal value and its concentration also showed a good linear relationship (R 2 =0.9997), such as image 3 Shown, illustrating that the method of the present invention can also be used for Hg 2+ quantitative analysis.

Embodiment 2

[0038] Such asfigure 1 For the device and process shown, a glass concentric pneumatic nebulizer is selected, the inner diameter of the central tube of the nebulizer is 0.2 mm, the nebulizing gas pressure is 50 psi, and the flow rate of pure water is 100 µL min -1 , with a flow injection loop volume of 100 µL. 5 μg L -1 As 3+ Vapor generation and atomization to As under the action of hydrogen radicals in micro-droplets 0 , after the cold atomic fluorescence detection, the peak figure is as follows Figure 4 , indicating that the microdroplet spontaneous vapor generation process can also be used for As 3+ determination.

Embodiment 3

[0040] Such as figure 1 For the device and process shown, a quartz concentric pneumatic nebulizer is selected, the inner diameter of the central tube of the nebulizer is 0.2 mm, the nebulizing gas pressure is 50 psi, and the flow rate of pure water is 100 µL min -1 , with a flow injection loop volume of 100 µL. 5 μg L -1 Se 4+ Vapor generation and atomization to Se are achieved under the action of hydrogen radicals in micro-droplets 0 , after the cold atomic fluorescence detection, the peak figure is as follows Figure 5 , indicating that the microdroplet spontaneous vapor generation process can also be used for Se 4+ determination.

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Abstract

The invention discloses a method and a device for generating element steam through spontaneous induction of micro-droplets. The device is composed of a micro-injection pump, a flow injection valve, apneumatic atomizer and a gas-liquid separator. The flow rate of the micro-injection pump is 10-500 [mu]L min<-1>, and the pressure of atomized gas is 10-120 psi. Carrier flow pure water is introducedby a micro-injection pump and then enters a pneumatic atomizer together with a to-be-detected element solution in a sample injection ring of a flow injection valve to form micro-droplets, steam generation of to-be-detected element ions is achieved in the micro-droplet process, and generated gaseous volatile matter enters a detector to be detected after being separated by a gas-liquid separator along with carrier gas. The size of the micro-droplets is 1-20 [mu]m, the types of the to-be-detected elements can be Hg, As, Se, Te or Sb and the like, and the detector can be a cold atom luminoscope ora cold atom absorption instrument. The method and the device for generating element steam through spontaneous induction of micro-droplets do not need to be driven by external forces such as oxidation-reduction reagents, electric fields, illumination, ultrasound, microwaves or plasmas. The device is simple in structure and small in size, and is easily integrated with the existing spectrum instruments.

Description

technical field [0001] The invention relates to the technical field of analytical chemical atomic spectroscopy, in particular to a method and device for generating elemental vapor induced spontaneously by micro-droplets. Background technique [0002] Chemical vapor generation (Chemical Vapor Generation, CVG) is the most commonly used sample introduction technique in the field of atomic light / mass spectrometry. It is a process that converts the target analyte element from the solution ion state to its volatile gaseous atom, molecule or compound through redox reaction. Combining chemical vapor generation technology with atomic light / mass spectrometry instruments such as atomic fluorescence (AFS), atomic absorption (AAS), inductively coupled plasma mass spectrometry (ICP-MS) or optical emission spectroscopy (ICP-OES) can achieve in-solution Sensitive determination of various metal and non-metal elements. [0003] Traditional chemical vapor generation is achieved by the reacti...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N21/31G01N21/64
CPCG01N1/28G01N21/3103G01N21/6404G01N2021/3107
Inventor 何倩张宁馨何会军张劲
Owner OCEAN UNIV OF CHINA