Method for determining linear alkylbenzene sulfonate (LAS) in textile dyeing and finishing auxiliaries by ion-pair liquid chromatography

A technology of alkylbenzene sulfonate and liquid chromatography, applied in the field of linear alkylbenzene sulfonate detection, can solve the research reports and method standards for the analysis and detection of LAS residues, poor LAS chromatographic retention and resolution , large interference and other issues

Active Publication Date: 2014-04-16
南京海关工业产品检测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing research reports on the detection of LAS residues, most of the studies are on the detection of residual LAS in the water environment, and all use high-performance liquid chromatography (HPLC) separation, diode array detector (or ultraviolet detector) Detection, the liquid phase conditions were not optimized during HPLC detection, the chromatographic retention and resolution of LAS were poor, and the interference of LAS was greatly affected by ultraviolet light detection
At present, there are no research reports and method standards for the analysis and detection of LAS residues in textile dyeing and finishing auxiliaries

Method used

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  • Method for determining linear alkylbenzene sulfonate (LAS) in textile dyeing and finishing auxiliaries by ion-pair liquid chromatography
  • Method for determining linear alkylbenzene sulfonate (LAS) in textile dyeing and finishing auxiliaries by ion-pair liquid chromatography
  • Method for determining linear alkylbenzene sulfonate (LAS) in textile dyeing and finishing auxiliaries by ion-pair liquid chromatography

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Experimental program
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Effect test

Embodiment 1

[0090] Embodiment 1: actual textile dyeing and finishing auxiliaries sample detection

[0091] (1) Actual samples

[0092] The sample is a textile dyeing and finishing auxiliaries produced by a well-known domestic dyeing and finishing auxiliaries company and sold in the market, and the theoretical value of the amount of LAS added in the process of configuring these dyeing and finishing auxiliaries is provided. There are 9 kinds of textile dyeing and finishing auxiliaries, which can be used in various textile dyeing and finishing processes such as spinning, sizing, dyeing, printing, and finishing.

[0093] (2) Detection steps

[0094] 1) Preparation of sample solution: Weigh about 1g (accurate to 0.0001g) of textile dyeing and finishing auxiliaries, put it in a 50mL volumetric flask, and dilute to volume with methanol+water (50+50, v / v). Placed in an ultrasonic generator, ultrasonic treatment at room temperature for about 30 minutes.

[0095] 2) Solid-phase extraction (SPE) ...

Embodiment 2

[0110] Embodiment 2: standard addition recovery rate test

[0111] (1) Test samples

[0112] LAS was not detected in the sample of the same-bath degreasing agent produced by a well-known domestic dyeing and finishing auxiliaries company and sold in the market. Add LAS standard solutions of three concentration levels such as 25mg / kg, 100mg / kg, and 1000mg / kg to the negative sample, and the sample after adding the standard is determined according to the method of the present invention. Five parallel samples were made for each spiked level sample.

[0113] (2) Detection steps

[0114] 1) Preparation of sample solution: Weigh about 1g (accurate to 0.0001g) of textile dyeing and finishing auxiliaries, put it in a 50mL volumetric flask, and dilute to volume with methanol+water (50+50, v / v). Placed in an ultrasonic generator, ultrasonic treatment at room temperature for about 30 minutes.

[0115] 2) Solid-phase extraction (SPE) purification: first activate the SAX column with 5mL ...

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Abstract

The invention discloses a method for determining linear alkylbenzene sulfonate (LAS) in textile dyeing and finishing auxiliaries by ion-pair liquid chromatography, belonging to the analysis and detection fields of LAS residue in the textile dyeing and finishing auxiliaries. The method comprises the steps of firstly, sample solution preparation, namely, dissolving a sample with a strong polar solvent under the assistance of ultrasonic waves; secondly, solid-phase extraction and purification; and thirdly, separating by the ion-pair liquid chromatography and detecting by a fluorescence detector. The LAS is used as a standard, the chromatographic retention times of LAS in a comparative sample solution and a standard solution are compared, the special fingerprint spectrum is qualitatively analyzed and the sum of the peak areas of four main components of the LAS is quantified by an external standard method. The method for determining the linear alkylbenzene sulfonate (LAS) in textile dyeing and finishing auxiliaries by the ion-pair liquid chromatography is high in detection sensitivity, strong in anti-jamming capability and accurate in qualitative and quantitative analysis.

Description

technical field [0001] The invention relates to the technical field of linear alkylbenzene sulfonate detection, more specifically to a method for measuring various textile dyeing and finishing auxiliaries by ultrasonic-assisted extraction, solid-phase extraction purification, ion-pair liquid chromatography separation, and fluorescence detector. Method for linear alkylbenzene sulfonates. Background technique [0002] Textile dyeing and finishing auxiliaries can be divided into anionic, cationic, nonionic and amphoteric. Among them, anionic surfactants—linear alkylbenzene sulfonate (LAS) surfactants are widely used, and LAS has become a daily anionic Synonym for surfactant. LAS, usually composed of linear sodium alkylbenzene sulfonate with a carbon chain length of 10 to 13 (see the chemical structure figure 1 ), the hydrophobic group is an alkylphenyl group, and the hydrophilic group is a sulfonic acid group. 80% of textile printing and dyeing auxiliaries are surfactants. L...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 丁友超曹锡忠汤娟钱凯蔡建和
Owner 南京海关工业产品检测中心
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