Decompressed purge-and-trap processing equipment for non-volatile organic compound in water sample and processing method thereof

A non-volatile, purge and trap technology, applied in the field of chromatography, can solve the problems of many intermediate steps, long time required, secondary pollution, etc., and achieve the effect of short cycle, easy automation, and less manual operation

Inactive Publication Date: 2011-01-19
四川省环境监测中心站
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To sum up, for non-volatile organic compounds in water samples, the current common organic reagent pretreatment technology is characterized by the need to use organic reagents, a variety of instruments, reagents and analysis vessels, and many intermediate steps, which are easy to introduce interference. It takes a long time and there is secondary pollution

Method used

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  • Decompressed purge-and-trap processing equipment for non-volatile organic compound in water sample and processing method thereof
  • Decompressed purge-and-trap processing equipment for non-volatile organic compound in water sample and processing method thereof
  • Decompressed purge-and-trap processing equipment for non-volatile organic compound in water sample and processing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take the determination of acenaphthylene content in water by vacuum purge and trap as an example:

[0032] The decompression purging and trapping treatment device for non-volatile organic compounds in water samples is composed of a sample heater 1, a purge bottle 2, a trap 3, a pressure controller 4 and a pump 5 in sequence, and the purge gas 6 passes through the purge The gas inlet 7 is connected to the purge bottle 2 , the purge bottle is connected to the trap 3 through the purge gas outlet 8 , and the trap 3 is connected to the pump 5 through the pressure controller 4 .

[0033] The trap 3 traps the gas and takes it out and puts it into the heater 13 of the trap. The chromatographic carrier gas 14 is connected to the chromatographic inlet 12 in the column thermostat 11 through the transfer line 15 after analyzing the target object through the trap 3 , the chromatographic inlet is connected to the chromatographic detector 9 through the chromatographic column 10 .

[...

Embodiment 2

[0049] Adopt the device of embodiment 1, analyze the method for benzo [a] anthracene, chrysene, benzo [a] pyrene, benzo [b] fluoranthene in a certain water sample:

[0050] 1. Standard solution preparation

[0051] (1) Prepare the mixed standard solutions of the above four polycyclic aromatic hydrocarbons with concentrations of 0.01 μg / L, 0.1 μg / L, 1.0 μg / L, and 10.0 μg / L, wherein the standard concentrations of benzo[b]fluoranthene are respectively 0.02μg / L, 0.2μg / L, 2.0μg / L, 20.0μg / L, see Table 1 for their properties.

[0052] (2) Add 10 mL of water from the above standard into a 20 mL headspace bottle, and seal the headspace bottle.

[0053] 2. Gas connection

[0054] With embodiment 1.

[0055] 3. Purge and trap method

[0056] The sample heating temperature is set to 80°C, the pressure of the whole closed system is controlled at 20kpa through the pump and the pressure controller, the trapping material is polyacrylate (PA) solid-phase microextraction needle with a film ...

Embodiment 3

[0062] Using the device of Example 1, analyze benzo[k]fluoranthene, benzo(g, h, i) perylene, indeno[1,2,3-cd] perylene, dibenzo(a, h) in water samples ) method of anthracene:

[0063] 1. Standard solution preparation

[0064] (1) Prepare mixed standard solutions of the above four polycyclic aromatic hydrocarbons with a concentration of 0.01 μg / L, 0.1 μg / L, 1.0 μg / L, and 10.0 μg / L, in which the standard of benzo(g, h, i) perylene The concentrations are 0.02μg / L, 0.2μg / L, 2.0μg / L, and 20.0μg / L respectively, and their properties are shown in Table 2.

[0065] (2) Add 10 mL of water from the above standard into a 20 mL headspace bottle, and seal the headspace bottle.

[0066] 2. Gas connection

[0067] With embodiment 1.

[0068] 3. Purge and trap method

[0069] Set the sample heating temperature to 90°C, control the pressure of the entire closed system at 5kpa through a pump and a pressure controller, and use polyacrylate (PA) solid-phase microextraction needles with a film...

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Abstract

The invention discloses decompressed purge-and-trap processing equipment for a non-volatile organic compound in a water sample and a processing method thereof. The invention is characterized in that the equipment is formed by sequentially connecting a sample heater (1), a purge bottle (2), a trapper (3), a pressure controller (4) and a pump (5), wherein purge gas (6) is connected with the purge bottle (2) through a purge gas inlet (7); the purge bottle is connected with the trapper (3) through a purge gas outlet (8); the trapper (3) is connected with the pump (5) through the pressure controller (4); the gas trapped by the trapper (3) is taken out and then placed into a heater (13) of the trapper; chromatographic carrier gas (14) is connected with a chromatographic injection port (12) in a column oven (11) through the trapper (3) and a transmission pipeline (15); and the chromatographic injection port is connected with a chromatographic detector (9) through a chromatographic column (10). The processing method comprises the following steps: forming a negative pressure environment around a test sample under the action of the pump, and increasing the vapor pressure of the non-volatile organic compound under the negative pressure environment; purging the bottom of the sample by utilizing inert gas so that the target compound can be trapped by the trapper after being blown out from the sample; and finally, resolving the target compound at high temperature and then carrying out chromatographic analysis.

Description

technical field [0001] The present invention relates to a device for treating non-volatile organic matter in a water sample by vacuum purging and trapping and a treatment method thereof, in particular to a sample treatment method for trapping by vacuum purging and trapping and eluting non-volatile organic matter by thermal analysis method. It belongs to the technical field of chromatographic separation. Background technique [0002] The purge and trap method is a mature sample pretreatment technology. Due to the advantages of less sample volume, high enrichment efficiency, less matrix interference, and easy on-line monitoring, Bellar and Lichtenberg first published the purge and trap method in 1974. Chromatographic determination of volatile organic compounds in water has always been paid attention to by environmental science and analytical chemistry. U.S. EPA601, 602, and many other standard methods have used purge and trap technology to measure various volatile organic co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08
Inventor 张渝程小艳杨坪
Owner 四川省环境监测中心站
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