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A method for determining the effective content of akd emulsion by ionic liquid-assisted headspace gas chromatography

A headspace gas chromatography and ionic liquid technology, which is applied in the field of analysis and detection, can solve the problems such as the absence of quantitative detection of the effective content of AKD emulsion, low efficiency and time-consuming, and achieve the effects of shortening detection time, improving experimental efficiency and convenient operation.

Active Publication Date: 2020-04-28
SOUTH CHINA UNIV OF TECH
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Not only time-consuming and inefficient, but also cause certain errors in the quantitative detection of AKD
Therefore, there is currently no standard method for quantitatively detecting the effective content of AKD emulsion

Method used

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  • A method for determining the effective content of akd emulsion by ionic liquid-assisted headspace gas chromatography
  • A method for determining the effective content of akd emulsion by ionic liquid-assisted headspace gas chromatography
  • A method for determining the effective content of akd emulsion by ionic liquid-assisted headspace gas chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This embodiment measures the effective content of 5 kinds of commercially available AKD emulsions, and the specific determination steps are as follows:

[0028] (1) Establish a standard curve: add 150 μL of sodium bicarbonate solution with a concentration of 0.05 mol / L to the headspace vial, and after capping, use a syringe to calibrate the concentration to 1.067 mol / L, and the volume is 1.9 μL and 4.6 μL , 9.3 μL, 14 μL, and 19 μL of hydrochloric acid solutions were injected into the headspace bottle respectively, and the operating conditions of the headspace sampler and the gas chromatograph were set (the operating conditions of the headspace sampler were: equilibrium temperature 100 ° C, sample equilibrium time 10 min, The auxiliary gas pressure is 80Kpa, the carrier gas balance time in the headspace bottle is 12s, the pipeline inflation time is 12s, the pipeline balance time is 3s, and the loop balance time is 12s; gas chromatography operating conditions: column temp...

Embodiment 2

[0039] The AKD emulsion of known content (the laboratory is made, the mass ratio of AKD wax sheet and starch is 1:5) is added in the unknown AKD emulsion sample, detects again according to the method for embodiment 1, addition amount and experimental value are as follows: Table 2.

[0040] Table 2 Recovery experimental results

[0041]

[0042]

[0043] As can be seen from the results in Table 2, the detection method of the present invention is objective and accurate (relative error<2.3%) and has high precision.

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Abstract

The invention belongs to the technical field of analysis and detection and discloses a method for determining the effective content of an AKD emulsion by ionic liquid assisted headspace gas chromatography. The method comprises preparing a sodium bicarbonate solution with a known concentration in a headspace bottle, respectively injecting different amounts of hydrochloric acid solutions into the headspace bottle, carrying out headspace gas chromatography, drawing a standard curve according to the relationship of a chromatographic peak area signal value and a hydrochloric acid solution use amount, accurately weighing an AKD emulsion sample and an ionic liquid, putting the AKD emulsion sample and ionic liquid into the headspace bottle, carrying out headspace gas chromatography under the sameoperation conditions, recording gas chromatography signal values of carbon dioxide and substituting the gas chromatography signal values into the standard curve to obtain the effective AKD content ofthe sample. The method has high precision, is easy to operate, produces a detection result in short time, greatly improves experimental efficiency and is very suitable for detection of the effective content of the AKD emulsion.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a method for determining the effective content of AKD emulsion by ionic liquid-assisted headspace gas chromatography. Background technique [0002] Alkyl ketene dimer (AKD) is a typical reactive sizing agent, which is widely used in medium-alkaline papermaking, and improves its application properties, such as strength and printing performance, by giving paper more hydrophobic properties . Commercially available AKD emulsions usually use cationic starch for emulsification stabilization. In synthetic control and papermaking applications, the effective content of AKD emulsion is a very important parameter to measure its quality. [0003] Traditionally, the effective content of AKD emulsion can be quantitatively detected by iodometric method. In this method, the emulsion matrix is ​​vacuum-dried after air-drying or low-temperature evaporation to complete...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/66G01N30/06G01N30/86
CPCG01N30/06G01N30/66G01N30/8634
Inventor 闫宁柴欣生
Owner SOUTH CHINA UNIV OF TECH
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