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Gas-liquid contact extraction method and device

A technology of gas-liquid contact and extraction method, applied in sampling device, measuring device, sampling and other directions, can solve the problem of large distribution coefficient, and achieve the effect of improving the contact rate and improving the extraction efficiency

Active Publication Date: 2016-12-07
SHIMADZU SEISAKUSHO CO LTD +1
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  • 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] Passed the previous P&T method and used figure 1 The gas-liquid contact extraction method of the present invention, which includes the system of the gas-liquid contact extraction device of the present invention and the automatic liquid sample supply device, analyzes the sample water containing 2-MIB and Geosimin. Shows an experimental example of the comparison of the amount of material migration to the gas phase between 2-MIB and Geosimin.

[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. It shows the theoretical mass transfer amount and the respective extraction efficiency of 2-MIB and Geosimin moving from the liquid phase to the gas phase at a concentration of 5 ppt (5 pg / mL). In the conventional P&T method, the sample water volume was 20 ml. In the method of the present invention, the water was passed at a flow rate of 2 ml / min for 20 minutes, so the total ...

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 purge gas flow rate and the sample water flow rate are changed to compare the extraction efficiency of 2-MIB and Geosimin. The extraction efficiency conditions of 2-MIB and Geosimin based on purge gas flow and sample water flow are:

[0163] A: Sample water flow: 4ml / min, purge gas flow: 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 was 60°C. The result is expressed in image 3 . It is found that the condition for obtaining high extraction efficiency for both components is B in the figure.

[0167]

[0168] (1) Sample water extraction conditions

[0169] 1) Extraction temperature of sample water: 60...

Embodiment 3

[0194] Based on figure 1 The 2-MIB and Geosimin analysis reproducibility of the system including the gas-liquid contact extraction device and the automatic liquid sample supply device of the present invention were tested. 2-MIB and Geosimin have been known as musty-causing substances in tap water. However, according to the Tap Water Law in April 2005, as a water quality standard item, a low standard value of 0.01μg / L (10ppt) was set. As the lower limit of quantification, an extremely low value of 1 / 10 of 0.001μg / L (1ppt) is required. The olfactory threshold is described in the "Guidelines for Olfactory Measurements" issued by the Ministry of the Environment.

[0195] A repeated reproducibility test with the concentration of 1 ppt of each of 2-MIB and Geosimin was performed. The result is expressed in Figure 4 , Figure 5 , Image 6 . In addition, the CV (%) of the peak area values ​​of 2-MIB and Geosimin in the three measurements was calculated. The good results shown in Tabl...

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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 in liquid (hereinafter referred to as "GC") or gas chromatograph mass analyzer (hereinafter also referred to as "GC / MS"). It is "analyzed species".) In the analysis, the method and device for effective gas-liquid extraction of the analyzed species. Background technique [0002] In the analysis by GC or GCMS, as the analysis method using the gas-liquid extraction operation, there are purge and trap (hereinafter referred to as "P&T") method and headspace (hereinafter referred to as "HS" Situation.) Law. These are the analytical methods described in the Water Supply Law under the jurisdiction of the Ministry of Health, Labour and Welfare. [0003] (1) P&T law and its problems [0004] The P&T method is a method of forcibly extracting the analytical species dissolved in the solution into the gas phase by passing a gas with low solubility into the solution, and temporarily holding the extracted analytical spec...

Claims

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Application Information

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Patent Type & Authority Patents(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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