CN102662010A

CN102662010A - Method for measuring quinoline content in dispersing agent MF

Info

Publication number: CN102662010A
Application number: CN2012101328211A
Authority: CN
Inventors: 郭彦召; 李萍; 王丽娟; 连保香; 王峰; 郝军峰
Original assignee: ANYANG SHUANGHUAN AUXILIARIES Co Ltd
Current assignee: ANYANG SHUANGHUAN AUXILIARIES Co Ltd
Priority date: 2012-05-03
Filing date: 2012-05-03
Publication date: 2012-09-12

Abstract

The invention relates to an analysis method, and belongs to a method for measuring quinoline content in a dispersing agent MF. The method comprises the following steps: dissolving a weighed sample in water, fully extracting quinoline in the dispersing agent MF by using a quantitative organic solvent which is immiscible with water, standing for demixing, extracting an organic phase for sample injection, detecting by using a gas chromatograph, and calculating the quinoline content in the sample, wherein the organic solvent is benzene or methylbenzene, and methylbenzene preferably; a carrier gas is nitrogen; a chromatographic column is a packed column or a capillary column, and capillary column preferably; an injection mode comprises split injection and splitless injection, and split injection preferably, and a split ratio is 1:15-1:30, and 1:20 preferably; and the detector is a flame ionization detector (FID), an internal standard method or an external standard method is selected, and the external standard method is preferred. The method is easy and convenient to operate, accurate in results, low in detection limit, and favorable for quickly analyzing the quinoline content in the dispersing agent MF, so that a cause is easily found out, measures are taken early, and an aim of preventing harm to a human body is fulfilled.

Description

Quinoline Determination on content method in the Dispersant MF

Technical field

The present invention relates to a kind of analytical approach, belong to quinoline Determination on content method in the Dispersant MF.

Background technology

Dispersant MF is claimed dispersing agent MF again, the formaldehyde condensation products of methyl naphthalene sulfonic acid sodium, CAS number: 9084-06-4, chemical composition: dispersing agent MF (methylene dimethyl sodium dinaphthalenesulfonate).Proterties: Dispersant MF is brown ceramic powder, and is soluble in water, is prone to the moisture absorption, do not fire, and has good diffusivity and thermal stability, do not have miserable passing through property and foamability, and acid and alkali-resistance, hard water and inorganic salts do not have affinity to fibers such as linen-cottons; Protein and polyamide fibre there is affinity; Can use simultaneously with anionic and non-ionics, Dispersant MF belongs to anionic surfactant.Quinoline is a kind of component of producing raw materials used washing oil in the Dispersant MF, and content is approximately 3%～5%, in existing manufacturing technique; Quinoline can be residual to some extent in Dispersant MF; Therefore quinoline contacts meeting has certain harm with skin to human body, detects in the Dispersant MF content of quinoline and seems have particularly importantly, and does not also have mature and reliable at present; Easy to operate, accurate test method as a result.

Summary of the invention

The object of the present invention is to provide a kind of easy to operate, result to measure quinoline Determination on content method in the Dispersant MF accurately.

Quinoline Determination on content method in the Dispersant MF; The sample of weighing is soluble in water, use with the abundant extraction and dispersion agent of the immiscible quantitative organic solvent of water MF in quinoline, standing demix; Extract the organic phase sample introduction; Use gas chromatographic detection,, calculate the content of quinoline in the sample with the contrast of quinoline standard specimen; Used organic solvent is benzene or toluene, preferred toluene, and nitrogen is selected in carrier gas for use; Chromatographic column is selected packed column or capillary column for use, the refin capillary column, and the sample introduction pattern comprises split sampling, split sampling not; Preferred split sampling, split ratio 1:15～1:30, preferred 1:20; Detecting device uses fid detector, selects internal standard method or external standard method for use, preferred external standard method.

Adopt assay method of the present invention, easy and simple to handle, the result is accurate, and detectability is low, helps the express-analysis to quinoline content in the Dispersant MF, so that ascertain the reason, takes measures early, to reach the purpose of avoiding human harm.

Embodiment

Specify below and realize implementation of the present invention:

The sample of weighing is soluble in water, use with the abundant extraction and dispersion agent of the immiscible quantitative organic solvent of water MF in quinoline, standing demix extracts the organic phase sample introduction, uses gas chromatographic detection, calculates the content of quinoline in the sample.

Concrete steps are following:

1, takes by weighing quantity of sample, be mixed with the certain density WS; 2, add certain amount of organic solvent; 3, concuss extraction certain hour, standing demix; 4, extract the upper organic phase sample introduction,,, calculate the concentration of quinoline in the organic phase through internal standard method or external standard method, and then calculate the content of quinoline in the sample with the contrast of quinoline standard specimen through the peak area of quinoline in the gas chromatographic detection organic phase.The concentration of the WS is 1%～20% (massfraction) in the step 1; Used organic solvent is a benzene in the step 2, and toluene geometric ratio anharmonic ratio water is little, with the immiscible organic solvent of water; The step 3 concussion time is 1～5min, and the standing demix time is 0.5～3h; The liquid phase chromatogram condition that relates in the step 4: nitrogen is selected in carrier gas for use, presses 0.1Mpa before the post, and chromatographic column is selected packed column or capillary column for use, the refin capillary column; If use capillary column, the sample introduction pattern comprises split sampling, and split sampling is not shunted/split sampling not; If using split sampling pattern, split ratio is 1:15～1:30, preferred 1:20; Detecting device uses fid detector, selects internal standard method or external standard method for use, preferred external standard method.

Used raw material among the following embodiment, reaction reagents etc. if no special instructions, are all buied from market, and related reaction conditions and method particularly point out like nothing, are conventional reaction conditions and method.

Embodiment: through the content of quinoline in the external standard method Dispersant MF, accurately take by weighing the chromatographically pure quinoline of different quality, be mixed with 25mL toluene standard specimen solution, with the peak area and the retention time of gas Chromatographic Determination quinoline; GC conditions: carrier gas is a nitrogen, presses 0.1Mpa before the post, and bypass flow 25mL/min detects with FID; 260 ℃ of injector temperature, 160 ℃ of post oven temperature, degree, 260 ℃ of detector temperatures, sample size 1 μ L; Do ordinate with peak area, do horizontal ordinate with quinoline concentration, (x is a quinoline concentration to make typical curve y=11.752x-345; The μ g/mL of unit, y are peak area), retention time 3.2min.

Take by weighing the 1g Dispersant MF and add 25ml water; Fully the dissolving back adds 25ml toluene, and concuss 3min left standstill 1 hour; Extract upper organic phase clear liquid sample introduction; Using gas chromatographic detection quinoline peak area is 495, and the concentration of calculating quinoline in the solution according to typical curve is 71 μ g/mL, and the content of quinoline is 1126ppm in the sample.

According to assay method of the present invention, have the countless versions combination, can not enumerate one by one in an embodiment, as long as belong to flesh and blood of the present invention, all belong to protection scope of the present invention with interior prescription and process combination, repeat no more here.

Claims

1. quinoline Determination on content method in the Dispersant MF; The sample of weighing is soluble in water, use with the abundant extraction and dispersion agent of the immiscible quantitative organic solvent of water MF in quinoline, standing demix; Extract the organic phase sample introduction; Use gas chromatographic detection,, calculate the content of quinoline in the sample with the contrast of quinoline standard specimen; It is characterized in that: used organic solvent is benzene or toluene, preferred toluene, and nitrogen is selected in carrier gas for use; Chromatographic column is selected packed column or capillary column for use, the refin capillary column, and the sample introduction pattern comprises split sampling, split sampling not; Preferred split sampling, split ratio 1:15～1:30, preferred 1:20; Detecting device uses fid detector, selects internal standard method or external standard method for use, preferred external standard method.