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On-line solid-phase extraction gaschromatographic mass spectrometry detection method for organotin in water body

A technology of gas chromatography-mass spectrometry and a detection method, which is applied in the field of online solid-phase extraction gas chromatography-mass spectrometry detection of organic tin in water, can solve the problems of large amount of eluent, time-consuming, etc., and achieve simple operation, accurate results, and impressive results. Satisfactory recovery and reproducibility results

Inactive Publication Date: 2019-11-05
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These traditional methods above usually require additional back extraction, which is time-consuming and requires a large amount of eluent

Method used

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  • On-line solid-phase extraction gaschromatographic mass spectrometry detection method for organotin in water body
  • On-line solid-phase extraction gaschromatographic mass spectrometry detection method for organotin in water body
  • On-line solid-phase extraction gaschromatographic mass spectrometry detection method for organotin in water body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Sampling

[0039] Commercially available purified water of a certain brand was filtered through a polyvinylidene fluoride microporous membrane with a pore size of 0.45 μm, and stored in a refrigerator at 0-4°C until testing.

[0040] (2) sample preparation

[0041] Measure 50mL of the sample to be tested, add 2.72g of sodium acetate trihydrate, after dissolving, add 10mL of a mixed solution of acetic acid and methanol (1:1, v / v), mix well, and adjust the pH to 5 with sodium hydroxide solution to obtain Water samples after pretreatment.

[0042] (3) On-line solid phase extraction purification-derivatization

[0043] like figure 1 As shown, through the peristaltic pump, the concentration of the above pretreated water sample and complexing agent was 4×10 -3 The mol / L sodium diethyldithiocarbamate solution is pumped into the reaction tank to fully react to form complexes. The injection speed of the pretreated water sample is 3mL / min, and the complexing agent sodium ...

Embodiment 2

[0071] Organotin detection in a river water in the source of Qianjiang River

[0072] (1) Sampling

[0073] Put the collected river water from Qianjiangyuan into a 1L brown narrow-mouth glass bottle with a silica gel seal, then transport it back to the laboratory in a portable refrigerator, and filter it through a polyvinylidene fluoride microporous membrane with a pore size of 0.45 μm. , placed in 0 ~ 4 ℃ refrigerated storage, to be tested.

[0074] (2) sample preparation

[0075] The difference between the sample preparation process and Example 1 is that the pH is adjusted to 5.5 with sodium hydroxide solution, and the rest are identical.

[0076] (3) On-line solid phase extraction purification-derivatization

[0077] The difference between the online solid-phase extraction purification-derivatization process and that of Example 1 is that the derivation time is 3 minutes, and the rest are identical.

[0078] (4) Concentrated to volume

[0079] Concentration to volume is...

Embodiment 3

[0098] Organotin detection in a certain seawater in Hangzhou Bay

[0099] (1) Sampling

[0100] The collected seawater in Hangzhou Bay was put into a 1L brown narrow-mouth glass bottle with a silica gel seal, and then transported back to the laboratory in a portable refrigerator, and filtered through a polyvinylidene fluoride microporous membrane with a pore size of 0.45 μm. Store in refrigerated storage at 0-4°C until testing.

[0101] (2) sample preparation

[0102] The difference between the sample preparation process and Example 1 is that the pH is adjusted to 5.2 with sodium hydroxide solution, and the rest are identical.

[0103] (3) On-line solid phase extraction purification-derivatization

[0104] The difference between the on-line solid phase extraction purification-derivatization process and that of Example 1 is that the derivation time is 2.5 min, and the rest are identical.

[0105] (4) Concentrated to volume

[0106] Concentrating to volume is different from...

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Abstract

The invention discloses an on-line solid-phase extraction gaschromatographic mass spectrometry detection method for organotin in a water body. The method comprises the following steps of (1) sampling;(2) sample preparation; (3) on-line solid-phase extraction purification-derivation; (4) concentration and making up to a volume; (5) gas chromatgraphy-mass spectrometrometry detection; (6) drawing ofa standard curve; (7) determination of a sample. The detection method has the advantages that the operation is simple, the sample pretreatment can be rapidly completed, a multiwalled carbon nanotubecolumn is adopted for the first time to achieve online enrichment, purification and derivation, only 25-30 minutes are needed in the whole on-line solid-phase extraction purification-derivation process, the multiwalled carbon nanotube column can be repeatedly used, the use period is 6 months, results are accurate, detection limits of nine kinds of organotin are 1-2.5 ng / L, the recovery rate is 82-116%, the relative standard deviation (n=5) is 3.7-8.5%, the method has higher sensitivity and satisfactory recovery rate and reproducibility, and the method can be used for determination of the content of the organotin in the water.

Description

technical field [0001] The invention relates to the technical field of water pollution detection, in particular to an online solid-phase extraction gas chromatography-mass spectrometry detection method for organotin in water. Background technique [0002] As an important class of environmental hormones, organotin is widely distributed in various media such as the atmosphere, water, soil, sediment, and organisms. It has androgenic effects, interferes with the endocrine system, and causes abnormal reproduction, development, and behavior. Used as PVC stabilizer, hull antifouling material, wood preservative, insecticide, fungicide, among which tributyltin, triphenyltin and their degradation products have been listed as "priority pollutant blacklist" by many countries in the world . Although organotin pollution has attracted global attention, it can persist due to its long half-life. The Water Framework Directive (WFD, 2000 / 60 / EC, 2008 / 105 / EC) sets the EQS for unfiltered water ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/54G01N30/88
CPCG01N30/02G01N30/06G01N30/54G01N30/72G01N30/88G01N2030/025G01N2030/062G01N2030/884
Inventor 胡红美李铁军金衍健孙秀梅张博应忠真
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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