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Curie-point pyrolyser of volatile matter generated by element in element determination

A technology of element determination and Curie point, which is applied in the field of instrument analysis, can solve the problems of slow heating rate of tube furnace cracker, peak and tailing of element volatiles, and prolonged measurement time, so as to improve the cracking rate of samples by heating up, The peak shape is sharp and the peak is fast.

Inactive Publication Date: 2014-05-14
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the pyrolysis heating device used in this patent is a tube furnace cracker. Due to the slow heating rate of the tube furnace cracker (the time required for the sample to rise from room temperature to the cracking temperature after heating is greater than 2 seconds), the elements are volatilized The peak tailing of the substance on the measuring instrument is serious, and the detected peak shape is not sharp, which makes the measurement time longer and the accuracy is not good

Method used

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  • Curie-point pyrolyser of volatile matter generated by element in element determination
  • Curie-point pyrolyser of volatile matter generated by element in element determination

Examples

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Effect test

Embodiment 1

[0043] A Curie point pyrolyzer used for generating volatiles from elements during element determination, comprising an induction heating coil 1, a quartz reaction liner 2, a reaction chamber 3, a reaction tube sealing plug and a sample holder integration device 4, and a carrier gas inlet 5 , carrier gas outlet 6, sample crucible 7 (preferably 500°C-800°C), sample crucible support 8, crucible support 9, wherein crucible or foil support support and sealing plug connecting rod; The time required for the inside point material to rise from room temperature to the Curie point temperature after heating is less than 500 milliseconds. The element samples to be measured are directly loaded in the Curie point pyrolysis crucible. When the sample of the element to be measured is indirectly loaded in the Curie point crucible, a layer of high molecular polymer is sprayed on the surface of the crucible sample; the thickness of the crucible wall is 0.08-1 mm. Among them, the high molecula...

Embodiment 2

[0046] A Curie point pyrolyzer used for generating volatiles from elements during element determination, comprising an induction heating coil 1, a quartz reaction liner 2, a reaction chamber 3, a reaction tube sealing plug and a sample holder integration device 4, and a carrier gas inlet 5 , a carrier gas outlet 6, a foil 7, a holder 8 for carrying the sample foil, and a holder 9 for carrying the foil.

[0047] The sample crucible or foil of the present invention is composed of a Curie point material with a Curie point temperature of 980° C., and the time required for the sample to rise from room temperature to the Curie point temperature after being heated by the Curie point material is less than 300 milliseconds.

[0048] The Curie point pyrolyzer used to generate volatiles from elements during element determination according to the present invention, wherein the sample of the element to be measured is directly or indirectly loaded in the Curie point pyrolytically wrapped and...

Embodiment 3

[0051] Analysis of Arsenic Content in Rice

[0052]Use the device described in preferred embodiment one to carry out the determination of arsenic content in rice flour. Accurately weigh 4 mg of rice flour sample into an iron crucible, then put the crucible into a quartz tube, turn on the high-frequency coil power supply for induction heating, at this time the Curie point temperature of the iron crucible is 770°C. The elemental volatiles and organics produced by the pyrolysis are carried by the carrier gas (argon, 300 ml / min) and passed through a three-stage semi-conductor refrigeration condenser device (condensation temperature -20°C) and a quartz wool filter layer. After purification, the rice flour The volatile matter of arsenic in the element is detected by atomic fluorescence (the atomic fluorescence atomizer is connected with a hydrogen generator with a hydrogen generation rate of 450 ml / min, so as to provide a hydrogen source for the normal ignition of the atomizer). ...

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Abstract

The invention discloses a curie-point pyrolyser of a volatile matter generated by an element in element determination. The curie-point pyrolyser adopts a liner tube and a curie-point pyrolysis crucible or curie-point foil filled with samples, with larger volumes than that of a pyrolysis chromatograph part. The pyrolyser comprises a heating coil 1, a quartz reaction liner tube 2, a reaction cavity 3, a reaction tube seal plug and sample support integrated device 4, a carrier gas inlet 5, a carrier gas outlet 6, the sample crucible or foil 7, a support 8 for carrying the sample crucible or foil, and a bracket 9 for carrying the support of the crucible or foil, wherein the bracket 9 for carrying the support of the crucible or foil and a seal plug are connected with a rod. Compared with a conventional tubular furnace pyrolyser, the curie-point pyrolyser has the advantages that heating velocity is high, the time of generating the volatile matter by the element is short, spectrum peak is sharp in element determination, environment temperature is low, operation is safe, and the like, and is beneficial to the accurate element determination.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis, and in particular relates to a Curie point cracker used for elements to generate volatiles during element determination. Background technique [0002] With the rapid development of modern instrument analysis, atomic spectrometer plays an increasingly obvious role in the determination of elements due to its advantages of fast determination, high accuracy and low detection limit. The sample entry system used in atomic spectrometers is currently mainly a pneumatic atomization system. The important disadvantage of the pneumatic atomization method is that the atomization efficiency of the sample is too low, and only about 3-5% of the sample solution containing elements is actually entered into the atomizer (ionizer) of the instrument, so that the sensitivity and detection limit of the instrument are limited. limit. In order to improve the sensitivity of these elements and reduce the de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44
Inventor 段旭川
Owner TIANJIN NORMAL UNIVERSITY
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