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Miniaturized electrolyte contact glow discharge emission spectrum device

A technology of glow discharge and emission spectroscopy, applied in the field of atomic emission spectroscopy analysis and testing, can solve the problems of high cost, complicated process, difficult operation, etc., and achieve the effects of low energy consumption, high excitation efficiency, and easy miniaturization

Inactive Publication Date: 2019-03-22
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as these instruments are concerned, the problems are that the equipment is large in size, high in energy consumption, complex in operation, and high in operating costs, and is not suitable for continuous on-line monitoring in the field
The disadvantages of this device are: 1. the cathode capillary is easily damaged under high voltage; 2. when the solution enters the capillary driven by the peristaltic pump, a large pulse flow will be generated, causing the liquid overflowing from the top of the capillary to be discontinuous, making the overflow solution the same as that of graphite. The electrodes are intermittently turned on, which makes the generated glow discharge plasma unstable; ③The electrolyte continuously overflows from the capillary and flows into the liquid storage pool with a constant liquid level below, and the auxiliary graphite electrode connected to the negative electrode is immersed in the liquid storage pool , so that the electrolyte is connected to the negative electrode of the discharge. This process needs to use the constant liquid level in the liquid storage tank to control the stability of the discharge, which is difficult; ④The electrolyte is generally an acidic solution with pH=1, which is easy to corrode the equipment ; ⑤ The continuous overflow of the overflow liquid and the continuous outflow of the waste liquid maintain the high stability of the electrolyte in the liquid storage tank, but a dual-channel peristaltic pump is required, which is costly, complicated, and difficult to operate

Method used

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  • Miniaturized electrolyte contact glow discharge emission spectrum device
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  • Miniaturized electrolyte contact glow discharge emission spectrum device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The DC stabilized power supply 14 adopts LW100J2 DC stabilized power supply, which provides a voltage of 0-1000V and a current of 0-500mA. A 1-1.2 kΩ shunt resistor 15 is connected in series between the platinum needle 10 and the positive pole 16 of the DC stabilized power supply 14 to protect the tip of the platinum needle 10 from damage due to excessive current. The diameter of the platinum needle 10 is 0.2-0.7mm, the length of the quartz tube 11 exposed at the lower end is 0.3-0.6mm, the diameter of the graphite carbon rod 9 is 2-4mm, and the depth of the lower end of the graphite carbon rod 9 inserted into the liquid storage tank 4 is 1mm. -2cm, the reservoir 4 is cylindrical with a diameter of 2-4cm and a height of 3-5cm. Both the support platform 5 and the translation platform 12 are adjustable three-dimensional translation platforms with micron-level precision, so that the distance between the platinum needle 10 and the overflow liquid surface 13 of the liquid st...

Embodiment 2

[0044] The electrolyte is 2g / L Na 2 SO 4 The glow photos taken by the camera when the solution is at 600V are as follows figure 2 As shown, it can be seen that at 600V, the solution is broken down and a bright discharge plasma is generated.

[0045] In order to further illustrate the stability of the glow discharge plasma that the present invention produces, image 3 The signal intensity at NaI589.6nm is shown as a function of time. Depend on image 3 It can be seen that, as time goes by, the signal intensity of the glow discharge plasma remains unchanged, which is a straight line parallel to the time axis. It shows that the signal intensity of the glow discharge plasma generated by the device of the present invention is stable, and the determination of metal elements in the solution can be realized.

[0046] Figure 4 2g / LNa when the voltage is 600V 2 SO 4 blank solution ( Figure 4 (a)) and with 2g / LNa 2 SO 4 The prepared concentration is all 10mg / L of K, Cu, Pb ...

Embodiment 3

[0048] Adopt the present invention to measure Cu, Pb, K element in the solution respectively, use 2g / LNa 2 SO 4 Prepare 1000 mg / L standard stock solutions of Cu, Pb and K respectively. During the measurement, it is gradually diluted into a series of solutions of 5-15 mg / L, and the series of standard Cu, Pb, and K solutions configured above are respectively driven by the peristaltic pump 3 into the liquid storage tank 4, and the overflow liquid of the liquid storage tank 4 is convex. 13 is in contact with the lower end of the platinum needle 10, the DC stabilized power supply 14 is turned on, and a voltage of 600V is applied between the two electrodes. Use the monochromator 22 to split the light, and the photomultiplier tube 24 to amplify and convert the spectral signal on the data processing system 25 to measure the spectral signal online. Each condition is measured 10 times, and the average value of the signal intensity is taken.

[0049] The signal intensity is measured at...

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Abstract

The invention discloses a miniaturized electrolyte contact glow discharge emission spectrum device. The miniaturized electrolyte contact glow discharge emission spectrum device comprises a sample feeding system, a waste liquid discharging system, an excitation source system, a beam splitting system and a detection and analysis system, wherein a convex liquid surface of overflowing liquid generatedby a liquid storage tank in the sample feeding system forms a discharge cathode; a platinum needle in the excitation source system is an anode; glow discharge plasma which is generated when the platinum needle is in contact with the convex liquid surface of the overflowing liquid is located at one side of a lens; a monochromator of the beam splitting system is arranged at the other side of the lens; the monochromator is connected with an electron-multiplier phototube of the detection and analysis system; the electron-multiplier phototube is connected with a data processing system. A glow discharge source with good stability can be obtained through continuous sample feeding and continuous overflowing of the overflowing liquid. An excitation source device provided by the invention is smallin size and low in power and has no gas loss and no high-temperature environment; a vacuum environment and sample feeding parts including an atomizer and the like are not needed, so that miniaturization is convenient to realize; continuous analysis and determination of the wild field can be realized, and the miniaturized electrolyte contact glow discharge emission spectrum device has a wide application prospect in the aspect of metal element detection in the fields of environment, medicine, food safety and the like.

Description

technical field [0001] The invention belongs to the technical field of atomic emission spectrum analysis and testing, in particular to a miniaturized electrolyte contact glow discharge emission spectrum device. Background technique [0002] The monitoring of metal pollutants is one of the important analytical tasks in environmental monitoring. The detection and analysis of such pollutants is mainly through various large-scale atomic spectroscopic analysis instruments such as inductively coupled plasma, inductively coupled plasma mass spectrometry, atomic absorption, atomic Fluorescence etc. As far as these instruments are concerned, the existing problems are that the equipment is large in size, high in energy consumption, complex in operation, and high in operating costs, and is not suitable for continuous on-line monitoring in the field. At present, analysts not only have to complete daily routine analysis tasks, but also undertake field field analysis tasks for emergencie...

Claims

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Application Information

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IPC IPC(8): G01N21/67G01N21/69
CPCG01N21/67G01N21/69
Inventor 俞洁张志超陆泉芳朱淑雯冯菲菲银玲
Owner NORTHWEST NORMAL UNIVERSITY