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A method for recovering and reusing the reduction tube of an elemental analyzer

The technology of an elemental analyzer and a recovery method is applied in the field of recovery and reuse of the reduction tube of the elemental analyzer, which can solve the problems of high instrument operation cost, high recovery cost, large consumption, etc., so as to reduce the instrument operation cost and improve the recovery rate. ability, the effect of improving accuracy

Active Publication Date: 2021-06-22
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are two major problems in the elemental analyzer: one is that the reducing agent linear copper consumes quickly and consumes a large amount, and the black copper oxide generated after being oxidized is sintered to form a copper oxide column, which is difficult to remove from the quartz tube, making the reducing tube The whole is scrapped, and the operating cost of the instrument is very high; the second is that under the condition of rapid dynamic combustion, the nitrogen analysis results of samples with high nitrogen content with structures such as nitrogen-containing heterocycles and nitro groups are often low
It can solve the existing situation that the element analyzer is occupied during the reduction of granular copper in the element analyzer, which affects the normal use of the element analyzer
[0007] However, the regeneration method of the reduction tube in several elemental analyzers disclosed in the prior art is cumbersome and needs to rely on other large-scale instruments. The popularity of the method is low, and the recovery cost is high, which violates the original intention of recovery.

Method used

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  • A method for recovering and reusing the reduction tube of an elemental analyzer

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Experimental program
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Effect test

Embodiment 1

[0035] Put a failed reduction tube in a 500mL plastic measuring cylinder, rinse the reduction tube slowly with 3.1mol / L dilute sulfuric acid, and continue to rinse until the invalid linear copper can be separated from the quartz tube, and the rinse time is about 30 minutes;

[0036] Pour out the invalid linear copper from the quartz tube, scrub the quartz tube with alkaline water, and rinse it with pure water several times to obtain a clean quartz tube;

[0037] After immersing the invalid linear copper in dilute sulfuric acid for 6 hours, fully react the sintered copper oxide, take out the unreacted pure copper, wash it with water for several times, dry it in vacuum at 80°C for 1 hour, and recover the linear copper. The recovery rate of linear copper is (47.88±2.78)%.

[0038] The surface of the new linear copper and the recovered linear copper was observed with a scanning electron microscope, and the results were as follows: figure 1 shown, from figure 1 In (a) and (b), it...

Embodiment 2

[0044] After the recovery and reduction tube prepared in Example 1 was assembled into the instrument, after the instrument was heated up, the blank sample was taken, and the standard sample was taken, the element content of metronidazole was measured. The test results are shown in Table 2.

[0045] Table 2 Determination results of metronidazole element content when using recovery reduction tube

[0046] project C(w%) H(w%) N(w%) first measurement 42.00 5.36 24.56 Second determination 42.01 5.32 24.55 third determination 41.96 5.34 24.58 theoretical value 42.07 5.26 24.54

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Abstract

The invention relates to the field of elemental analysis, and discloses a method for recovering and reusing the reducing tube of an elemental analyzer. The method uses dilute sulfuric acid to rinse and soak the reducing tube containing invalid linear copper, and oxidizes the oxidized linear copper surface. Copper reacts away, leaving unoxidized pure copper, which is recovered to obtain linear copper. The method is low in cost, simple in operation, does not need to rely on other large-scale instruments, has high popularity, and can effectively reduce instrument operating costs. And the specific surface area of ​​the linear copper recovered by this method is much larger than that of the new linear copper, the reduction ability is enhanced, and the determination result of nitrogen element is accurate when measuring samples with high nitrogen content such as nitro groups and nitrogen-containing heterocycles. higher.

Description

technical field [0001] The invention relates to the field of elemental analysis, in particular to a recovery and reuse method for a reduction tube of an elemental analyzer. Background technique [0002] Elemental analysis is an important quantitative analysis method, which is often used as an important supplement to qualitative analysis methods such as NMR, mass spectrometry, spectroscopy, and chromatography, and provides information on the elemental composition and content of the tested sample. Therefore, elemental analyzers have been widely used in many fields such as chemistry, chemical industry, pharmaceuticals, materials, energy, food, environment, and agriculture. At present, many important academic journals have required elemental analysis data as an important indicator of purity, which shows its importance. [0003] The working principle of the CHN mode of the elemental analyzer is as follows: in the combustion tube, the sample is burned and decomposed under the act...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23G1/10C23G3/00G01N31/12
CPCC23G1/103C23G3/00G01N31/12
Inventor 蒋艳余明新
Owner ZHEJIANG UNIV