Method for simultaneously detecting inorganic tin and organotin compounds through low pressure ion chromatography-inductively coupled plasma-mass spectrometry

A low-pressure ion chromatography and inductive coupling technology, applied in the field of detection and analysis of tin compounds, can solve the problems of high price, unsatisfactory, high analysis cost, etc., achieve low maintenance costs, improve stability, and reduce costs

Inactive Publication Date: 2017-06-20
SICHUAN UNIV
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Problems solved by technology

For example, Yu Zhenhua et al. reported a method for the simultaneous detection of multiple organotins in seafood using high performance liquid chromatography-inductively coupled plasma mass spectrometry (Yu Zhenhua, Jing Miao, Wang Geng, et al., HPLC- Inductively coupled plasma mass spectrometry simultaneously detects various organotins in seafood [J], Analytical Chemistry, Volume 36, Issue 8: 1035-1039), although this method can simultaneously determine trimethyltin chloride ( TMT), dibutyltin chloride (DBT), tributyltin chloride (TBT), diphenyltin chloride (DPhT) and triphenyltin chloride (TPhT), these five organotin compounds, but There are still the following problems to be improved: (1) the method cannot realize the simultaneous analysis of organotin compounds and inorganic tin, and cannot meet the needs of the simultaneous determination of these two types of tin in actual use; (2) the high performance liquid chromatography The price is high, and the supporting chromatographic column is a consumable product, and the price is relatively high, so the analysis cost is extremely high; (3) High-performance liquid chromatography adopts high-pressure operation. In a high-pressure environment, the sealing of the injection valve and other components Prone to problems, so the maintenance cost of the instrument is also relatively high in use; (4) the high-efficiency liquid phase mobile phase that this method adopts is acetonitrile-water-acetic acid mixed solution, contains 65% (v / v) in the mobile phase The content of acetonitrile and the organic solvent is as high as 77% (v / v), and the high organic load will easily lead to the instability of the analysis signal of the inductively coupled plasma mass spectrometry, and the high content of highly toxic acetonitrile is likely to cause harm to the health of the analysis operators

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  • Method for simultaneously detecting inorganic tin and organotin compounds through low pressure ion chromatography-inductively coupled plasma-mass spectrometry
  • Method for simultaneously detecting inorganic tin and organotin compounds through low pressure ion chromatography-inductively coupled plasma-mass spectrometry
  • Method for simultaneously detecting inorganic tin and organotin compounds through low pressure ion chromatography-inductively coupled plasma-mass spectrometry

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Embodiment 1

[0028] In the present embodiment, the standard sample is tested to investigate the linear range and detection limit of the method of the present invention, the steps are as follows:

[0029] 1. Preparation of standard samples

[0030] Preparation of standard stock solution: Weigh monomethyltin chloride (MeT), dibutyltin chloride (DBT), diphenyltin chloride (DPhT), trimethyltin chloride (TMT) and tributyltin chloride Based on tin chloride (TBT), use acetone to dissolve MeT, DBT, DPhT, TMT and TBT respectively, transfer to a volumetric flask and prepare MeT, DBT, DPhT, TMT and TBT with a concentration of 10 mg / L. stock solution.

[0031] Due to Sn 4+ Than Sn 2+ It is more stable, so tetravalent inorganic tin salts are used when preparing inorganic tin standard samples, and water-soluble inorganic tetravalent tin salts are weighed, dissolved in deionized water, transferred to a volumetric flask, and prepared with deionized water to constant volume. 4+ Standard stock solution ...

Embodiment 2

[0051] In this example, the method of the present invention is used to measure the total inorganic tin, MeT, DBT, DPhT, TMT and TBT in the actual leather sample.

[0052] 1. Sample Preparation

[0053] Take 4 pieces of leather samples, and each sample is processed according to the following operations:

[0054] Cut the leather sample into small pieces of 1 cm × 1 cm and mix them evenly. Accurately weigh 0.500 g of the cut sample and place it in the sample tube of the focused microwave synthesis system. Add 10.0 mL of acidic artificial sweat (the preparation method of the artificial sweat) : 0.5g of L-histidine hydrochloride, 5g of sodium chloride, 2.2g of sodium dihydrogen phosphate hydrate, and deionized water to make 1L solution and adjust the pH value to 5.5 with hydrochloric acid solution) at 75°C for 6min, extract The supernatant was then taken for subsequent analysis. The supernatants obtained from the 4 samples after the aforementioned extraction operations are respecti...

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Abstract

The invention provides a method for simultaneously detecting inorganic tin and organotin compounds through low pressure ion chromatography-inductively coupled plasma-mass spectrometry. Analysis devices comprising a low pressure pump, a six-way injection valve, a sample introduction ring, a cation separating column and an inductively coupled plasma mass spectrometer are adopted. The method comprises the following steps: 1, plotting a baseline; 2, platting the spectra of the inorganic tin and the organotin compounds in a sample; 3, plotting the spectra of the inorganic tin and the organotin compounds in a standard sample, and drawing the working curves of the inorganic tin and the organotin compounds; and 4, calculating the concentrations of the inorganic tin and the organotin compounds in the sample. The method can be used to simultaneously detect the concentrations of total inorganic tin, monomethyltin trichloride, dibutyltin dichloride, diphenyltin dichloride, trimethyltin chloride and tributyltin chloride in the sample.

Description

technical field [0001] The invention belongs to the technical field of detection and analysis of tin compounds, in particular to a method for simultaneously measuring inorganic tin and organic tin compounds by low-pressure ion chromatography-inductively coupled plasma mass spectrometry. Background technique [0002] Organotin compounds (organotin compounds, OTCs) are a class of tin-containing organometallic compounds. Because different organotin compounds have various functions such as anticorrosion, sterilization and deodorization, they are widely used in ship antifouling coatings, pesticides and insecticides, tanning, plastic chemicals and other industries. Organotin is an internationally recognized toxic pollutant. A low concentration of organotin compounds can produce great toxicity, and its half-life can reach several years in the absence of oxygen or ultraviolet rays. EU 2009 / 425 / EC limits the total amount of organotin in leather products to ≤0.1%. The textile eco-la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/96G01N30/88
CPCG01N30/88G01N30/96G01N2030/884G01N2030/8868
Inventor 张新申靳皓琛
Owner SICHUAN UNIV
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