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High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface

A high-performance liquid chromatography and atomic absorption technology, applied in the field of interface design of analytical chemistry combined instruments, can solve problems such as reducing chromatographic separation efficiency, and achieve the effect of solving peak broadening

Inactive Publication Date: 2009-07-01
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to achieve high efficiency of on-line digestion, an on-line digestion pipeline up to 5 meters is generally used, but due to the serious post-column broadening caused by the long pipeline, the efficiency of chromatographic separation is greatly reduced

Method used

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  • High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface
  • High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Such as figure 1 As shown, the present invention mainly includes: a thin inner diameter tee 2, a thin quartz tube 4, an ultraviolet lamp 5, a cross 6, a reaction tube 9, a large inner diameter tee 12 and a connecting pipe. The connection method is: the thin inner diameter tee 2 is connected with the thin quartz tube 4, the cross 6, the reaction tube 9 and the large inner diameter tee 12 in turn. The thin inner diameter tee 2 branch pipes connect the HPLC effluent inlet 1 and K 2 S 2 o 3 (1.5%) (as an oxidizing agent, other persulfates can also be used) solution delivery pipe 3 . The two thin quartz tubes 4 (inner diameter: 0.5mm, length: 20cm) are connected by a connecting pipeline 14, and are close to the outer wall of the ultraviolet lamp tube 5 (ultraviolet lamp power: 5W). Four-way connection hydrochloric acid solution (30%) (acid solution, reacts with reducing agent to generate active hydrogen, reduces arsenic to hydride) transfer pipe 7 and KBH 4 (1.5%) (redu...

Embodiment 2

[0020] Connection mode is the same as embodiment 1,

[0021] Two thin quartz tubes 4, inner diameter: 1.5mm, length: 40cm;

[0022] UV lamp power: 15W;

[0023] Reaction tube 9: inner diameter 0.5mm, length 60cm;

[0024] Fine inner diameter tee 2: inner diameter 1.2mm;

[0025] Four-way 6: inner diameter 1.5mm;

[0026] Large inner diameter tee 12: inner diameter 2.5mm;

[0027] K 2 S 2 o 3 Solution pump flow: 0.5ml / min;

[0028] Hydrochloric acid solution pump flow rate: 0.5ml / min;

[0029] KBH 4 Solution pump flow rate: 0.5ml / min.

[0030] The analytes were separated by high performance liquid chromatography and passed through the fine inner diameter tee 2 and K 2 S 2 o 3 The solution is mixed into the ultraviolet digestion part (thin quartz tube 4, which is digested under the action of ultraviolet light to produce small molecules that are easy to hydride. The digested product is mixed with hydrochloric acid solution and KBH 4The solutions are mixed to form hy...

Embodiment 3

[0032] Connection mode is the same as embodiment 1,

[0033] Two thin quartz tubes 4, inner diameter: 2mm, length: 10cm;

[0034] UV lamp power: 8W;

[0035] Reaction tube 9: 2mm, length 40cm;

[0036] Fine inner diameter tee 2: inner diameter 1mm;

[0037] Four-way 6: inner diameter 2mm;

[0038] Large inner diameter tee 12: inner diameter 2mm;

[0039] K 2 S 2 o 3 Solution pumping flow: 2ml / min;

[0040] Hydrochloric acid solution pump flow rate: 2.5ml / min;

[0041] KBH 4 Solution pump flow: 2.5ml / min.

[0042] The analytes were separated by high performance liquid chromatography and passed through the fine inner diameter tee 2 and K 2 S 2 o 3 The solution is mixed into the ultraviolet digestion part (thin quartz tube 4, which is digested under the action of ultraviolet light to produce small molecules that are easy to hydride. The digested product is mixed with hydrochloric acid solution and KBH 4 The solutions are mixed to form hydrides, which enter the gas-l...

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Abstract

The high-performance liquid chromatography-hydride atomic absorption / fluorescence spectroscopy instrument interface relates to the technical field of analytical chemistry coupled instrument interface design. It is characterized in that it contains successively connected thin inner diameter tee, thin quartz tube, cross, reaction tube, and large inner diameter tee; the first branch pipe of the thin inner diameter tee is connected to the inlet of the high performance liquid chromatography effluent, and the second branch is connected to the oxidant Transmission tube, the third branch is connected to one end of the thin quartz tube, and the thin quartz tube is next to an ultraviolet lamp tube; the other end of the thin quartz tube is connected to the first branch of the four-way pipe, and the second branch of the four-way pipe is connected to the acid solution transmission pipe. The three branches are connected to the reducing agent transmission pipe, the fourth branch is connected to one end of the reaction tube, the other end of the reaction tube is connected to the first branch of the large inner diameter tee, the second branch of the large inner diameter tee is connected to the carrier gas transmission pipe, and the third branch is connected to Delivery tube to gas-liquid separator. This interface not only realizes the online digestion of complex organic arsenic, mercury, antimony, selenium and other compounds, but also solves the problem of peak broadening.

Description

Technical field: [0001] The invention relates to the technical field of interface design for analytical chemistry combined instruments, in particular to the interface design for combined use of chromatography and electrothermal atomic absorption / atomic fluorescence instruments. Background technique: [0002] The toxicity, bioavailability, and mobility of elements are largely determined by their existing forms. Speciation analysis can provide more information than total element concentration analysis. It can not only reflect the content of the analyte, but also reflect The existence state of the analyte is of great significance to the research of environmental science and life science, and has attracted enough attention. The object of speciation analysis is usually biological or environmental samples. Generally speaking, the sample matrix is ​​relatively complex, and the content of elements to be measured is trace level. In addition, each form must be qualitatively and quanti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N35/00G01N30/74G01N21/31G01N21/64
Inventor 张新荣朱振利赵蕊韦超邢志刘华琳
Owner TSINGHUA UNIV
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