On-line regeneration experimental method for fillers in organic matter carbon and nitrogen analysis based on elemental analyzer
An elemental analyzer, carbon and nitrogen technology, applied in the direction of chemical analysis by means of combustion, can solve the problems of insufficient combustion of samples, increased accuracy, reduced conversion rate, etc., to achieve perfect functions, improved reduction ability, and improved oxidation ability Effect
Active Publication Date: 2016-05-25
NORTHWEST INST OF ECO ENVIRONMENT & RESOURCES CAS
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Problems solved by technology
During the experiment, as the amount of test samples increases, the consumption of the above-mentioned consumables increases, the redox capacity also decreases, and the conversion rate of the samples decreases, which can only be solved by replacing the consumables; in addition, in order to reduce the consumption of copper in the reduction furnace, during the oxidation process It is necessary to control the amount of oxygen injection (otherwise excess oxygen will enter the reduction furnace to oxidize metal copper), if the oxygen injection amount is insufficient, it will cause insufficient combustion of the sample, increase the accumulation effect and affect the accuracy of the test results
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[0018] specific implementation plan
[0019] Below, in conjunction with accompanying drawing, technical scheme of the present invention is described further:
[0020] Such as figure 1 Schematic diagram of the online regeneration test process for elemental analyzer packing. Mainly include: autosampler 1, oxidation furnace 2, reduction furnace 3, helium pressure regulating valve 4, hydrogen pressure regulating valve 5, carbon dioxide pressure regulating valve 6, oxygen pressure regulating valve 7, electric cold trap 8, chromatographic column 9 , TCD detector 10, gas stable isotope ratio mass spectrometer (MS) 11, three-way valve 12 between carbon dioxide gas pipeline and hydrogen pipeline, leak detection valve (a1) 13, leak detection valve (a2) 14, six-way valve Six contacts of (B): (b1, b2, b3, b4, b5, b6), ten contacts of ten-way valve (C): (c1, c2, c3, c4, c5, c6, c7, c8, c9, c10).
[0021] When the solid sample tightly wrapped by the tin cup enters the 1000°C oxidation f...
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The invention discloses an element-analyzer-based online regeneration test method of a filler for carbon and nitrogen analysis of an organic matter. The method is characterized in that the oxidizing capacity of an oxidizing agent is improved by adopting an online oxygen supplementation way; the reduction capacity of copper can be restored by online supplementing hydrogen to a reduction furnace; the hydrogen which is adsorbed on the surface of the metal copper can be precipitated in a way of introducing carbon dioxide into the reduction furnace, so that a regeneration function of the filler is completed online. By adopting the method, the regeneration function of the filler can be completed online under the situation that the test does not need to be stopped and the filler does not need to be replaced, so that the cost is reduced, the detection efficiency and analysis precision of an instrument can be improved, the repeatability of the filler can be guaranteed, and the method is an economic and effective analysis method which is convenient to popularize.
Description
technical field [0001] The invention relates to an on-line regeneration experimental method for fillers used when an elemental analyzer tests the carbon and nitrogen elements of organic matter in solid samples. Background technique [0002] Elemental analyzer for determining nitrogen and carbon element analysis in soil, sediment, fertilizer or agricultural samples. Its working principle is to put the sample into the combustion reactor from the automatic sampler, and feed pure oxygen into the system to make the sample burn. The final sample is converted into various oxides of carbon and nitrogen and water vapor, and then enters the reduction furnace to be reduced to CO 2 , N 2 And other detectable gases, use chromatographic separation column and TCD detector to complete the detection of carbon and nitrogen content, and use stable isotope mass spectrometer to complete the detection of nitrogen and carbon isotope ratio. [0003] The combustion reactor of the elemental analyze...
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IPC IPC(8): G01N31/12
Inventor 孙维贞余海棠
Owner NORTHWEST INST OF ECO ENVIRONMENT & RESOURCES CAS