Heat purge and trap instrument and heat purge and trap method

A thermal purging and trapping tube technology, applied in the field of purging and trapping, can solve the problems of long time, impurity component interference measurement, unfavorable environmental protection and health of operators, etc.

Inactive Publication Date: 2013-03-20
BEIJING RES INST OF URANIUM GEOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have their own advantages and disadvantages, but a large amount of organic solvents such as dichloromethane and n-hexane are required in the operation process, which is not conducive to environmental protection and the health of operators, and it is easy to introduce impurity components to interfere with the determination.
The extracted solution needs to be concentrated by nitrogen blowing to improve the detection sensitivity, and the concentration process takes a long time, and components with lower boiling points are easily lost

Method used

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  • Heat purge and trap instrument and heat purge and trap method
  • Heat purge and trap instrument and heat purge and trap method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A thermal purging and trapping apparatus of the present invention comprises a heating furnace 4, a sample furnace 3, a high-purity nitrogen cylinder 1, a transmission pipe 5, a trapping pipe 8 and a refrigeration cold hydrazine 7.

[0026] The sample furnace 3 is made of general-purpose No. 304 stainless steel. The furnace body is cylindrical, with a bottom at one end and a flange opening at the other end. There are 4 fixing bolts evenly around the flange, and the outer diameter of the furnace is 48mm. , wall thickness 4mm; the cover of the sample furnace is also processed by general-purpose 304 stainless steel. The furnace cover has two holes with diameters of 3mm and 6mm respectively. They are fixed by fixing bolts, and there is a high-temperature-resistant gasket between the furnace cover and the furnace body.

[0027] The sample furnace 3 is placed in a heating furnace 4 . The heating furnace 4 is preferably two types: one is a cylindrical resistance wire heating f...

Embodiment 2

[0032] A kind of thermal purging and trapping method utilizing thermal purging and trapping apparatus of the present invention, comprises the following steps successively:

[0033] Step 1, placing the sample to be tested in the sample furnace 3;

[0034] Step 2, the adsorption material is Tenax TA with 80 mesh particles;

[0035] Step 3, using the aluminum block heating furnace 4 to heat the sample furnace 3 at a heating temperature of 180°C;

[0036] Step 4: Turn on the high-purity nitrogen gas and refrigeration cold hydrazine 7, the flow rate of high-purity nitrogen is 80mL / min, the capture time lasts for 30 minutes, and the refrigeration cold hydrazine is kept at -1°C. Transfer Tube Heat: Off.

[0037] The recoveries of the various components were determined in conjunction with automated thermal desorption-GC / MS. C 8～16 The recovery rate of alkanes and m-xylene is greater than 95%, C 17～22 The recovery of alkanes and 2,4-dinitrotoluene was >92%. The sensitivity is bet...

Embodiment 3

[0039] A kind of thermal purging and trapping method utilizing thermal purging and trapping apparatus of the present invention, comprises the following steps successively:

[0040] Step 1, placing the sample to be tested in the sample furnace 3;

[0041] Step 2, the adsorption material is Tenax TA with 80 mesh particles;

[0042] Step 3, using the aluminum block heating furnace 4 to heat the sample furnace 3 at a heating temperature of 320°C;

[0043] Step 4: Turn on the high-purity nitrogen gas and the refrigeration cold hydrazine 7, the high-purity nitrogen flow rate is 30mL / min, the capture time lasts for 30 minutes, and the refrigeration cold hydrazine 7 maintains 6°C. Transfer tube heating: ON, heating temperature is 100°C.

[0044] The recoveries of the various components were determined in conjunction with automated thermal desorption-GC / MS. C 8～16 The recovery rate of alkanes and m-xylene is greater than 98%, C 17～22 The recovery of alkanes and 2,4-dinitrotoluene ...

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Abstract

The invention relates to a heat purge and trap instrument, comprising a heating furnace, a sample furnace, a high-purity nitrogen gas cylinder, a transmission pipe sealably connected with the air outlet of the sample furnace, a trapping pipe sealably connected with the other end of the transmission pipe and a cooling cold trap with the trapping pipe sleeved therein. The invention also relates to a heat purge and trap method. The method successively comprises the following steps of 1. putting a to-be-tested sample in the sample furnace; 2. adsorbing materials with 80-mesh granular Tenax TA; 3. heating the sample furnace to a temperature of 180 DEG C-600 DEG C; 4. opening the high-purity nitrogen gas cylinder and the cooling cold trap, wherein the flow rate of the high-purity nitrogen gas is 20 mL / 80 min; the collecting time lasts for 30-60 minutes; and the cooling cold trap is kept at a temperature of -1.0 DEG C-15.0 DEG C. The heat purge and trap instrument and the heat purge and trap method are in no need of organic reagents and post-enrichment processes, and are suitable for the determination of volatile organic components in solid samples such as rocks, soils, coals and the like. Combined with GC / MS, the sensitivity for detecting alkane organic components is superior to 0.1 ng / g.

Description

technical field [0001] The present invention relates to a thermal purging and trapping instrument, in particular to a thermal purging and trapping instrument suitable for the determination of volatile organic components in rock, soil, coal and other solid samples; the present invention also relates to a thermal purging and trapping instrument Sweep capture method. Background technique [0002] According to the EPA method (Method 5035), organic components with a boiling point lower than 200°C in solid samples are trapped through a closed purge and trap system. The trapping principle is to adjust the acidity of the sample with a buffer solution of a certain pH value. Under the high-purity gas, the organic components are purged into the trap, and the quantitative and qualitative determinations are carried out by GC or GC / MS after thermal desorption. Since a buffer solution is used in the method, the purging and trapping temperature is limited; in addition, water vapor will con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08
Inventor 李伯平郭冬发崔建勇刘桂方董晨
Owner BEIJING RES INST OF URANIUM GEOLOGY
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