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Vapor-liquid contact extraction method and device

A technology of gas-liquid contact and extraction method, which is applied in the direction of sampling device, measuring device, sampling, etc., can solve the problem of large distribution coefficient and achieve the effect of increasing the contact rate and improving the extraction efficiency

Active Publication Date: 2014-07-23
SHIMADZU SEISAKUSHO CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0022] 2) The generation of problems caused by the increase of the purge flow rate
However, with the conventional P&T method and HS method, it is difficult to perform GC or GC / MS analysis of analyte species with "large partition coefficient in gas-liquid equilibrium", "highly water-soluble", and "low olfactory threshold".

Method used

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Effect test

Embodiment 1

[0127] Through the previous P&T method and using the figure 1 In the shown gas-liquid contact extraction method of the present invention comprising the gas-liquid contact extraction device of the present invention and the automatic liquid sample supply device, the sample water containing 2-MIB and Geosimin is analyzed. An experimental example of a comparison of the amount of species transferred to the gas phase between 2-MIB and Geosimin is shown.

[0128] [Table 2]

[0129]

[0130]

[0131] Table 2 is related to the conventional P&T method and the gas-liquid contact extraction method of the present invention, showing the theoretical mass transfer amount and respective extraction efficiency of 2-MIB and Geosimin moving from the liquid phase with a concentration of 5 ppt (5 pg / mL) to the gas phase. The amount of sample water in the conventional P&T method was 20ml. In the method of the present invention, the water was passed for 20 minutes at a flow rate of 2ml / min, so ...

Embodiment 2

[0162] For the gas-liquid contact extraction method of the present invention using the automatic liquid sample supply device of the present invention, the flow rate of the purge gas and the flow rate of the sample water were changed, and the extraction efficiencies of 2-MIB and Geosimin were compared. The extraction efficiency conditions of different 2-MIB and Geosimin based on purge gas flow rate and sample water flow rate are:

[0163] A: Sample water flow rate: 4ml / min, purge gas flow rate: 160ml / min, extraction time: 10 minutes

[0164] B: Sample water flow rate: 2ml / min, purge gas flow rate: 80ml / min, extraction time: 20 minutes

[0165] C: Sample water flow rate: 1ml / min, purge gas flow rate: 40ml / min, extraction time: 40 minutes,

[0166] The extraction temperature is 60°C. The result is expressed in image 3 . It was found that the condition for obtaining high extraction efficiency of both components is B in the figure.

[0167]

[0168] (1) Sample water extract...

Embodiment 3

[0194] for based on figure 1 The analysis reproducibility of 2-MIB and Geosimin of the system including the gas-liquid contact extraction device and the automatic liquid sample supply device of the present invention was tested. 2-MIB and Geosimin are known as musty odor-causing substances in tap water. However, according to the revision of the Tap Water Act in April 2005, a low standard value of 0.01 μg / L (10ppt) was set as a water quality standard item. An extremely low value of 0.001 μg / L (1 ppt), which is 1 / 10 thereof, is required as the lower limit of quantification. The olfactory threshold is described in the "Guidelines for Olfactometry" of the Ministry of the Environment.

[0195] Repeated reproducibility tests were performed at concentrations of 1 ppt for 2-MIB and Geosimin. The result is expressed in Figure 4 , Figure 5 , Figure 6 . In addition, the CV (%) of the peak area values ​​of 2-MIB and Geosimin at the time of three measurements was calculated. Favor...

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Abstract

The present invention provides a method and device for quickly extracting analytical species present in a liquid phase when using vapor-liquid contact extraction for analyzing species having "a large partition coefficient in the vapor-liquid equilibrium," "a high water solubility," or "a low olfactory threshold; " and further provides a method and device for introducing the analytical species as a sample in GC or the like without user assistance over prolonged and continuous periods of time. This method and device perform vapor-liquid contact of a sample liquid and purge gas using a vapor-liquid contact extraction unit for continuously introducing the sample liquid from above and the purge gas from below, and extract the analytical species from the test sample liquid. The purge gas is prevented from flowing out from a liquid reservoir provided to a discharge pipe connected to a bottom part of the vapor-liquid contact extraction unit while the liquid sample is discharged via the reservoir.

Description

technical field [0001] The present invention relates to dissolved substances (hereinafter referred to as In the analysis of "analyte species".), a method and device for effectively performing gas-liquid extraction of the analyte species. Background technique [0002] In the analysis by GC or GCMS, there are purge and trap (hereinafter referred to as "P&T") method and headspace (hereinafter referred to as "HS") as analysis methods using gas-liquid extraction operation. situation.) Act. These are analysis techniques recorded in the Water Service Law governed by the Ministry of Health, Labor and Welfare. [0003] (1) P&T method and its problems [0004] The P&T method is a method in which the analyte species dissolved in the solution are forcibly extracted to the gas phase by passing a gas with low solubility into the solution, and the extracted analyte species are temporarily held in the adsorbent, thereby concentrating the analyte species. Thereafter, the adsorbent is rap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/10G01N1/00G01N30/06
CPCG01N1/4055G01N30/06G01N2030/065
Inventor 福本真治山内博志青野晃下村学武井义之见村正铃木明古野正浩
Owner SHIMADZU SEISAKUSHO CO LTD
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