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Analysis sample injection apparatus and method for making element form volatile by using organic matter cracking

A technology of sampling device and cracking device, which is applied in the field of instrument analysis and can solve the problems of increasing the cost of analysis and testing, affecting accuracy, environmental pollution, etc.

Inactive Publication Date: 2015-03-25
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004]At present, when atomic spectrometry is used to determine elements, whether atomized or gaseous sampling is used, the sample to be tested needs to be digested in most cases ( pretreatment), which makes the whole analysis and test process take a long time (sample pretreatment time usually accounts for 50-75% of the whole analysis time), and at the same time, the detection limit of the solution is affected due to the use of chemical reagents in the pretreatment, Increasing the blank value will affect the accuracy of the determination
Furthermore, sample pretreatment causes environmental pollution and increases the cost of analysis and testing

Method used

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  • Analysis sample injection apparatus and method for making element form volatile by using organic matter cracking
  • Analysis sample injection apparatus and method for making element form volatile by using organic matter cracking
  • Analysis sample injection apparatus and method for making element form volatile by using organic matter cracking

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0138] Embodiment 1: Arsenic content analysis in rice

[0139] In a 20 ml quartz test tube, accurately add 10 mg of rice sample, then put a rubber stopper with inlet and outlet of carrier gas (argon, flow rate 300 ml / min) on it and plug the test tube mouth tightly. The carrier gas outlet pipe carrying elemental volatiles is connected in series with a U-shaped condenser (to remove water and organic volatiles) and a plastic tube with quartz wool (to remove particulate matter). The purified carrier gas and atomic fluorescence atoms At this time, the atomic fluorescence atomizer is also connected with a hydrogen generator (hydrogen generation rate: 450 ml / min), so as to provide a hydrogen source for the normal ignition of the atomizer. And the carrier gas inlet is connected with the atomic fluorescence carrier gas supply pipe. When the device is connected and running stably, immediately insert the test tube into the thermostatic furnace that has been heated to 550°C in advanc...

Embodiment 2

[0140] Embodiment 2: the analysis of cadmium in spinach

[0141] The full set of apparatus and parameters of the preferred embodiment 2 were used to determine the cadmium content in spinach. In a quartz crucible (10 ml), accurately add 20 mg of spinach sample, because the vegetable itself is an organic matrix sample, so do not add any additional organic matter. Then put the crucible into the constant temperature furnace that has been heated to 550°C in advance under the supply of carrier gas, and start the instrument at the same time to start the atomic fluorescence measurement. By comparing with another spinach surface sample GBW10015 to make an appearance standard curve, the measurement result is 88ppb. However, the normal nitric acid-perchloric acid method was used to digest the sample, and the cadmium in the sample was measured by hydride to generate adispersive atomic fluorescence. The result was 83ppb, which shows that this method is in good agreement with the tradit...

Embodiment 3

[0142] Embodiment 3: the analysis of lead in fish gill

[0143] The full set of apparatus and parameters of the preferred example 4 were used to determine the cadmium content in fish gills. In a 10 ml quartz crucible, accurately add 10 mg of the fish gill sample, because the sample itself is an organic matrix sample, so do not add any more organic matter. Then put the crucible through the integrated device of the crucible support bracket and rubber sealing plug under the carrier gas, and quickly put it into the constant temperature furnace that has been heated to 600 ℃ in advance, and start the instrument at the same time to start the atomic fluorescence measurement. (Argon gas flow rate is 500 ml / min, hydrogen generator flow rate is 400 ml / min). Measure the content of lead in fish gills according to the standard addition method, and the assay result is 60ppb. However, the normal nitric acid-perchloric acid method was used to digest the sample and the lead content in the...

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Abstract

A method and injection device making use of organic cracking to cause an element to form a volatile for analysis; the injection device comprises a cracking device for heating of a sample, a condensation device for condensing the water and volatile organic material generated during sample heating, and optionally, a dust removal device for removing fine particulate matter; the method comprises the following steps: adding organics to a sample and mixing well; heating the mixture in a carrier gas of an inert gas, causing the hydrogen generated during organic cracking and the sample element to be tested to form an elemental volatile; separating and removing the water vapor in the elemental volatile, the organic volatile, and the fine particulate matter, then sending to the atomic spectrometer for measurement; without sample dissolution, the method directly measures solids and semi-solids, as well as trace elements in a liquid sample, especially trace elements in organic matrix samples such as foods; the method features rapid analysis, high accuracy, low cost of analysis, and no environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis, and in particular relates to an elemental analysis sampling device and method which utilizes the cracking and dehydrogenation of organic matter to form elements into volatiles. 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 application of atomic spectrometer (AFS, AAS, ICP-OES, ICP-MS, etc.) to determine the elements in the sample, the first step is the entry of the sample (or sample introduction, sample introduction). That is, through the sample entering the system, the element to be measured in the sample solution is introduced into the atomization (or ionization) device of the spectrometer, where the element is atomized or ionized, and an absorption or emission sp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/25G01N21/64
CPCH01J49/00G01N21/25G01N1/00G01N31/12G01N1/44
Inventor 段旭川卜范龙
Owner TIANJIN NORMAL UNIVERSITY
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