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Active-carbon-fiber type solid-phase adsorption method for gas-phase chromatogram

A technology of activated carbon fiber and gas chromatography, which is applied in the field of analytical chemistry, can solve the problems of short service life, complicated production, long equilibration time, etc., and achieve the effects of long service life, convenient manufacture and high sensitivity

Inactive Publication Date: 2005-01-26
SHANGHAI JIAOTONG UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] (1) The organic solid phase extraction agent is not resistant to high temperature, has short service life, slow mass transfer, relatively long equilibration time, and small enrichment amount
[0004] (2) The polarity of the extractant is different, resulting in insufficient broad-spectrum collection of unknown analytes
[0005] (3) Complex production and high cost
In addition, they only use acid to activate the carbon-based adsorbent, which will cause serious local dissolution grooves of different depths in the fiber (the dissolved substance is an inorganic oxide binder), which will cause the adsorbate to desorb incompletely or peak out. Tailing, and cause "greater selective adsorption of compounds with larger molecular weight and less polarity", which is not as broad-spectrum adsorption performance as activated carbon

Method used

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  • Active-carbon-fiber type solid-phase adsorption method for gas-phase chromatogram
  • Active-carbon-fiber type solid-phase adsorption method for gas-phase chromatogram

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Knead 15% of pitch, 70% of coke powder and 15% of kaolin at 200°C, press them at 350°C, and then put them in a tube furnace under N 2 Under the atmosphere, after carbonization at 1000°C, pass in water vapor for 20 minutes, and after cooling, activated carbon fibers will be obtained, which will be made into the required size and assembled into a solid-phase micro-adsorption device. The methanol in the mousse was analyzed, and the results are shown in Table 1. Using commercially available polyacrylate SPEM, only the huge solvent peak in the mousse and no methanol peak appeared, and the methanol peak in 1ml headspace was also hidden by the impurity peak. In contrast, ACF showed a good Selectivity, it reduces the impurity peaks by tens to hundreds of times, and concentrates the methanol peak.

[0017] Table 1 Determination results of methanol in mousse by ACF-SPMA method

[0018] Manufacturer's name

Embodiment 2

[0020] On the quartz wire with φ = 125 μm, apply phenolic resin with a weight ratio of 40% and a polymerization degree of 50% by dipping method. After each immersion, dry the quartz wire with a hot hair dryer and fully polymerize the resin layer. Repeat this process. The resin layer is gradually thickened to 75 μm. Make this fiber in quartz tube furnace, under coal gas atmosphere, install after carbonization, activation as the operation of embodiment 1, obtain coating type ACF, and compare with the SPMA of the body type ACF in embodiment 1, in gas chromatography Benzene was analyzed above, and the results were as follows figure 1 shown.

[0021] From figure 1 The comparison of the adsorption efficiency of the two ACF fibers shows that the two fibers basically reach equilibrium within 30 seconds, but the adsorption capacity of the body-shaped fiber is 3.3 times that of the coated fiber. Moreover, the quartz wire of the coated fiber is easy to break during operation, and the ...

Embodiment 3

[0023] With 12% phenolic resin (polymerization degree as embodiment 2), 65% graphite powder and 23% montmorillonite powder as raw material, according to embodiment 1, make SPMA device, and measure the benzene industrial waste water with gas chromatography The perchlorethylene, and compared with GB (straight pumping headspace method). The results are shown in Table 2 and Table 3. This fiber has been used more than 300 times, and the adsorption performance has not changed significantly.

[0024] Table 2 Determination results of PCE wastewater samples by SPME method and GB method

[0025] Concentration (mg / L)

SPME method

GB method

0.5

10295

5290

1

23377

13167

2

53333

23906

3

70561

37432

4

85123

44976

Sample to be tested

65931

33168

Sample to be tested +0.5

75197

38095

[0026] SPME method: Y=3024.5+21673*X (R=0.988)

[0027] GB method (direct injecti...

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Abstract

An active carbon fibrous solid phase microadsorption method used in gas-phase chromatographic is to use active carbon fiber ACF with fine adsorption to substitute organic coating solid phase extraction fiber, use natural or synthetic high polymer of asphalt or bakelite assistant with inorganic fillers to make the original fiber then to get porous active carbon fiber with strong adsorption ability and enough strength via high temperature carbonization and activation under the protection of inert or reductive gas. Said porous active carbon fiber as the inner chip of gas chromatograph GC sampler makes direct adsorption collection and GC sampling to the materials to be analysed and finish sampler and analysis after description in GC gas chamber, having got the aim of GC sampler zero solvation with better heat resistance than organic solid extraction fibers in solid micro-extraction.

Description

Technical field: [0001] The invention relates to an activated carbon fiber type solid-phase micro-adsorption method for gas chromatography, specifically a sample pretreatment method that can be used in combination with a gas chromatograph and can simultaneously perform sampling and injection, and is used for quantitative or semi- The method for quantitatively analyzing volatile and semivolatile substances in gas, water samples and solid samples belongs to the technical field of analytical chemistry. Background technique: [0002] Solid phase microextraction (SPME) method is a new type of sample pretreatment and sample injection technology in the current chromatographic technology. Its core is the solid phase extraction fiber installed inside the injector. The fiber is made by mixing different polarities A relatively heat-stable polymer extractant (such as polydimethylsiloxane or polyacrylate) is coated on the outside of the quartz wire. Because the technology has the advant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/08B01J20/20B01J20/30C01B32/336
Inventor 贾金平冯雪王亚林何翊
Owner SHANGHAI JIAOTONG UNIV
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