Palm mono-fiber micro-tube, capillary gas chromatographic column, and preparation and application thereof

A technology of gas chromatography column and capillary column, which is applied in the field of capillary gas chromatography column and its preparation and application, palm single fiber microtube, can solve the problems that there are no research reports on gas chromatography separation medium of biomass materials, and achieve high column efficiency, particle size The effect of uniform diameter distribution and rich functional groups

Active Publication Date: 2018-12-07
LUOYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no research report on the use of biomass materials as gas chromatography separation media

Method used

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  • Palm mono-fiber micro-tube, capillary gas chromatographic column, and preparation and application thereof
  • Palm mono-fiber micro-tube, capillary gas chromatographic column, and preparation and application thereof
  • Palm mono-fiber micro-tube, capillary gas chromatographic column, and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] (1) peel off the palm fiber from the palm tree, rinse with deionized water to remove impurities, dry at 80°C for 12 hours, cut 50 grams of cleaned and dried palm fiber into 2-3cm long; then place the palm fiber at a concentration of In 5mol / L NaOH solution, react at 150°C for 16h, then cool to 25°C;

[0073] (2) Ultrasonic treatment of the mixed system after cooling in step (1) for 4h with ultrasonic power of 50KW, then use ionized water to wash 4 times to neutrality to obtain palm single fiber microtubes (SPFMs), see figure 1 , the surface of the prepared palm monofilament microtubules is rough and contains abundant pores, the particle size distribution is uniform, the functional groups are rich, and there are many pores, the surface has wrinkles, the diameter is 3-5 μm, and the pore size is about 1 μm;

[0074] (3) Quartz capillary column (10m×0.25mm i.d.) was treated with NaOH solution with a concentration of 1mol / L and HCl solution with a concentration of 0.1mol / L ...

Embodiment 2

[0079] (1) peel off the palm fiber from the palm tree, rinse with deionized water to remove impurities, dry at 80°C for 12 hours, cut 50 grams of cleaned and dried palm fiber into 1-2cm long; then place the palm fiber at a concentration of In 4mol / L NaOH solution, react at 180°C for 12h, then cool to 30°C;

[0080] (2) Ultrasonic treatment of the mixed system after cooling in step (1) with ultrasonic power of 60KW for 3h, and then use ionized water to wash 3 times to neutrality to obtain palm monofilament microtubules (SPFMs);

[0081] (3) Quartz capillary column (10m×0.25mm i.d.) was sequentially treated with NaOH solution with a concentration of 1mol / L and HCl solution with a concentration of 0.1mol / L for 35min, then cleaned to neutral, and dried at 220°C under a nitrogen atmosphere 8h, obtain the pretreated capillary column;

[0082] (4) Mix 110 μL tetraethylorthosilicate (TEOS), 220 μL polydimethylsiloxane, hydroxyl-blocked short (HO-TOS), 10 μL polymethylhydrogensiloxane...

Embodiment 3

[0086] (1) peel off the palm fiber from the palm tree, rinse with deionized water to remove impurities, dry at 80°C for 12 hours, cut 50 grams of cleaned and dried palm fiber into 3-5cm long; then place the palm fiber at a concentration of In 6mol / L NaOH solution, react at 130°C for 18h, then cool to 20°C;

[0087] (2) The mixed system after cooling in the step (1) is ultrasonically treated with ultrasonic power of 45KW for 5h, then adopts ionized water to wash 5 times to neutrality, obtains palm monofilament microtubules (SPFMs);

[0088] (3) Quartz capillary column (10m×0.25mm i.d.) was sequentially treated with NaOH solution with a concentration of 1mol / L and HCl solution with a concentration of 0.1mol / L for 40min, then cleaned to neutral, and dried at 180°C under a nitrogen atmosphere 12h, obtain the pretreated capillary column;

[0089] (4) Mix 110 μL tetraethylorthosilicate (TEOS), 220 μL polydimethylsiloxane, hydroxyl-blocked short (HO-TOS), 10 μL polymethylhydrogensil...

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Abstract

The invention belongs to the field of chromatographic analysis and particularly relates to a palm mono-fiber micro-tube, a capillary gas chromatographic column, and preparation and application thereof. In the invention, with palm fiber being a raw material, the palm mono-fiber micro-tube is produced through hydro-thermal synthesis; the palm mono-fiber micro-tube is uniform in particle size distribution, contains abundant functional groups, has large quantity of pores and has wrinkles on surface, and is 3-5 [mu]m in diameter and about 1 [mu]m in pore size. With tetraethyl orthosilicate being aprecursor, hydrogen-containing silicone oil being an end-capping agent, hydroxyl silicone oil being a crosslinker, trifluoroacetic acid being a catalyst and the palm mono-fiber micro-tube being a stationary phase, hydrolysis and a condensation chemical reaction are carried out to make the capillary gas chromatographic column, which has high column efficiency being better than that of a common commercial column, HP-5. The capillary gas chromatographic column can effectively separate a complex blend sample and isomers composed of compounds in different molecular structures with wide polarity. The product shows excellent selectivity and sensitivity in measurement on isomer impurity purities in a practical sample.

Description

technical field [0001] The invention belongs to the field of chromatographic analysis, and in particular relates to a palm monofilament microtube, a capillary gas chromatography column and its preparation and application. Background technique [0002] Gas chromatography (GC) is one of several common methods for qualitative and quantitative analysis of complex mixtures of organic compounds. The key to chromatographic separation is to choose the appropriate stationary phase. In order to effectively separate complex samples or isomers, gas chromatography stationary phases need to have rich functional groups or special morphology. The current chromatographic stationary phases are all chemically synthesized organic / inorganic compounds. The composition of these materials is relatively complex, the synthesis process is cumbersome, the cost is high, and at the same time, it will cause environmental pollution. [0003] Biomass, as a promising renewable resource, has shown many adv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C3/02D21C3/04D21H17/05
CPCD21C3/02D21C3/04D21H17/05
Inventor 刘献明孙涛毋乃腾周战刘贵龙
Owner LUOYANG NORMAL UNIV
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