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Method for processing high-boiling-point solvant essence before gas-phase colour-spectrum mass-spectrum combined detection

A gas chromatography mass spectrometry, high boiling point solvent technology, applied in the field of high boiling point solvent essence treatment, can solve the problems of the loss of effective components of the essence, slow adsorption process, unfavorable adsorption, etc., to reduce the loss of effective components, improve the recovery efficiency, shorten the The effect of payback time

Inactive Publication Date: 2007-03-28
HUABAO FLAVOURS & FRAGRANCES CO LTD
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AI Technical Summary

Problems solved by technology

[0004] 1. Using activated carbon to absorb volatile components, the amount absorbed is not much, and the qualitative and quantitative aspects are not accurate enough;
[0005] 2. The adsorption process is slow and takes more than ten hours;
[0006] 3. It needs to be concentrated, which will cause the loss of the active ingredients of the essence during the concentration process
[0008] 1. This method is easy to generate foam during the experiment, overloading the instrument, and easily causing damage to the instrument;
[0009] 2. If there is water in the sample, the blowing out of water vapor is not conducive to the next step of adsorption, which will bring difficulties to the separation of non-polar gas chromatography columns, and water will also have a quenching effect on flame detectors

Method used

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  • Method for processing high-boiling-point solvant essence before gas-phase colour-spectrum mass-spectrum combined detection

Examples

Experimental program
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Effect test

Embodiment 1

[0035] As shown in Figure 1, connect the nitrogen cylinder 1 directly to the pressure reducing valve 2, then connect the gas outlet of the pressure reducing valve 2 to the air inlet of the flowmeter 3, and then connect the gas outlet of the flowmeter 3 with the high boiling point solvent essence to be processed The three-necked flask 4 of the sample is then used to receive the active component gas carried out by the condenser tube 5 equipped with a low-temperature receiving solvent.

[0036] The three-necked flask 4 is put into the water bath 6, and the water temperature of 30° C. to 80° C. is more suitable. Put the condenser tube 5 into the cold trap 7. The condensation temperature of the cold trap 7 should be controlled at -25°C to -15°C. The temperature difference between the high and low temperature of the cold trap 7 should be above 5°C to protect the condensate pump and open the cycle.

[0037] One side bottle mouth 41 of wherein said three-necked flask 4 is connected wi...

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Abstract

The invention discloses a first detection method of a high boiling point solvents fragrance samples before using gas chromatography mass spectrometry prior. Certain steps: weight 10~50g high boiling point solvents fragrance samples and out it into a 30 to 80 degreeC three-mouth flask; puts 600~1500ml / min ventilation velocity of inert gas flow and nitrogen flow and brings out the flavor components effectively, receives solvent absorption in -25~-15 degreeC, receives the self-enrichment samples by direct injection GC-MS detection. The invention method can analyze the essence of effective qualitative and quantitative composition accurately and improve the recovery efficiency, shorten recovery time, reduce the loss of effective ingredients, eliminate impurity effectively in the course of processing.

Description

technical field [0001] The invention relates to gas chromatography-mass spectrometry detection of essence, in particular to a method for processing high-boiling-point solvent essence before detection. Background technique [0002] Since high-boiling-point solvents such as oils will pollute the gas chromatography column and even be scrapped, high-boiling-point solvent flavors cannot directly enter GC / MS (gas chromatography and mass spectrometry) for sample analysis, so pre-processing is required before entering GC / MS. deal with. The existing pretreatment methods for high-boiling point solvent flavor samples before gas chromatography-mass spectrometry detection mainly use dynamic headspace method and purge and trap method. However, there are deficiencies in both preprocessing methods, among which: [0003] The dynamic headspace method has the following disadvantages: [0004] 1. Using activated carbon to absorb volatile components, the amount absorbed is not much, and the q...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N1/40
Inventor 高久磊陈浩张福军
Owner HUABAO FLAVOURS & FRAGRANCES CO LTD
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