Method for detecting organic tin in water body

A detection method and organotin technology, applied in the field of water pollution detection, can solve the problems of elution and long extraction time, and achieve the effects of saving elution time, reducing operation difficulty and improving environmental friendliness.

Pending Publication Date: 2020-11-17
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the technical problems of long elution and extraction time in the prior art, the present invention provides a new gas chromatography detection method for organotin in water bodies with high sensitivity, extraction, derivation and detection within 15-20 minutes

Method used

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  • Method for detecting organic tin in water body
  • Method for detecting organic tin in water body
  • Method for detecting organic tin in water body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] S1. Sampling - collect water sample 1 from the backwashing drainage of the water plant filter into the sampling bottle, after standing still for 2 hours, filter it through a 0.45μm polyvinylidene fluoride filter membrane, pour it into a brown glass bottle, and put the glass bottle into Store at 0°C.

[0031] S2. Sample preparation—take 50 ml of the sample to be tested in step S1, add 20 mL of methanol solution containing 1% (v / v) hydrochloric acid to the sample, and stir well until the mixture is uniform. After refluxing at a high temperature of 40° C. for 30 minutes, filter through the polyvinylidene fluoride filter membrane described in step S1 again to obtain a pretreated water sample.

[0032] S3. Liquid-liquid extraction and concentration of samples—add 20 mL of pH 2.0 phosphate-citrate buffer solution and 10 mL of tert-butyl ether solution to the pretreated water sample obtained in step S2, add high-purity water to dissolve and dilute to 100mL, then shake the dis...

Embodiment 2

[0044] S1. Sampling—the difference between the process and Example 1 is that the water sample taken is water sample 2, which is different from other water samples in collection time.

[0045] S2. Sample preparation—the process is exactly the same as in Example 1.

[0046] S3. Liquid-liquid extraction and concentration of the sample—the process is exactly the same as in Example 1.

[0047] S4. Ethylation and constant volume of the sample—the process is different from that of Example 1 in that the pH of the ethylation reaction system is controlled to be 6.0.

[0048] S5. Prepare standard solution—the process is exactly the same as that in Example 1.

[0049] S6. Detection by gas chromatography-flame photometry—the process is exactly the same as that in Example 1.

[0050] S7. Determination of standard curve—the process is exactly the same as that in Example 1.

[0051] S8. Characterization of results——the corresponding quantitative peak area of ​​the organotin in the chromato...

Embodiment 3

[0057] S1. Sampling—the difference between the process and Example 1 is that the water sample taken is water sample 3, which is different from other water samples in collection time.

[0058] S2. Sample preparation—the process is exactly the same as in Example 1.

[0059] S3. Liquid-liquid extraction and concentration of the sample—the process is exactly the same as in Example 1.

[0060] S4. Ethylation and constant volume of the sample—the process is exactly the same as in Example 1.

[0061] S5. Prepare standard solution—the process is exactly the same as that in Example 1.

[0062] S6. Detection by gas chromatography-flame photometry—the difference between the process and Example 1 is that the temperature of the injection port is set to 250°C

[0063] S7. Determination of standard curve—the process is exactly the same as that in Example 1.

[0064] S8. Characterization of results——the corresponding quantitative peak area of ​​the organotin in the chromatogram obtained fr...

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Abstract

The invention discloses a method for detecting organic tin in a water body. The method specifically comprises the following steps: carrying out liquid-liquid extraction reflux on a to-be-detected sample solution; adding a certain amount of extract liquor into a phosphate citrate buffer solution, normal hexane and a sodium tetraethylborate solution for derivatization; separating the extract liquorthrough a chromatographic column, and comparing with a standard solution by using a flame photometric method to obtain a standard curve, so as to calculate and detect the organic tin in the water body. According to the method, a liquid-liquid extraction gas chromatography flame photometry detector is adopted to determine the concentration of the organic tin compound in the water, derivatization and extraction are performed at the same time in the step S4; therefore, compared with solid-phase extraction in the background art, complex elution steps are not needed, the elution time is saved, theextraction and derivatization time is shortened, operation is easy and rapid. In addition, the actual sample analysis requirements can be met.

Description

technical field [0001] The invention relates to the technical field of water pollution detection, in particular to a method for detecting organotin in water. Background technique [0002] Organotin compounds are metal endocrine disruptors, mainly used as stabilizers for plastic products and antifouling agents for ship oil pollution. After extensive use in the past, it has caused serious pollution to the environment and ecology. Organotin compounds are a kind of persistent organic pollutants, especially tributyltin (TBT), although the content in drinking water sources such as rivers is low, they will be toxic to the human reproductive system through bioaccumulation in the food chain. The analysis and detection of organotin compounds mainly adopt liquid-liquid extraction, solid-phase extraction, solid-phase microextraction, liquid-phase microextraction or stirring rod adsorption extraction, and then use gas chromatography, high performance liquid chromatography, gas chromatog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68G01N2030/685
Inventor 莫嘉晨林涛张心悦
Owner HOHAI UNIV
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