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Method for detecting m-benzene dimethyl isophthalate-5-sodium sulfonate purity by liquid chromatography

A technology of dimethyl isophthalate and liquid chromatography, which is applied in the field of instrumental analysis, can solve the problems of not being able to further reflect the internal quality of the product, not being able to play a guiding role in quality improvement, and difficult to vaporize, so as to achieve the best separation effect, The effect of small error and long time consumption

Active Publication Date: 2015-06-24
WEIFANG WORLD CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Because dimethyl isophthalate-5-sodium sulfonate has a high boiling point and is difficult to vaporize, the purpose of detecting its purity cannot be realized by using commonly used gas chromatography, and the current dimethyl isophthalate-5-sodium sulfonate Detection, generally through conventional chemical titration methods such as acid value and saponification value, is used for quality control, but it cannot further reflect the internal quality of the product, and cannot play a guiding role in quality improvement

Method used

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  • Method for detecting m-benzene dimethyl isophthalate-5-sodium sulfonate purity by liquid chromatography
  • Method for detecting m-benzene dimethyl isophthalate-5-sodium sulfonate purity by liquid chromatography
  • Method for detecting m-benzene dimethyl isophthalate-5-sodium sulfonate purity by liquid chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Instruments used:

[0032] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0033] (2) Column Kromstar C18 4.6×150mm 5μm

[0034] (3) Constant temperature column box: Ripley RPL-C2000

[0035] (4) Ultrasonic degassing device

[0036] 2. Detection conditions:

[0037] (1) Mobile phase:

[0038] a. Water (containing 0.05% tetrabutylammonium chloride by volume);

[0039] b. Methanol;

[0040] Mobile phase ratio V a :V b =40:60

[0041] (2) Detection wavelength: 220nm

[0042] (3) Flow rate: 0.8mL / min

[0043] (4) Injection volume: 20μL

[0044] (5) Column temperature: 30°C

[0045] 3. Sample processing:

[0046] Accurately weigh 0.01g of dimethyl isophthalate-5-sodium sulfonate, dissolve it with distilled water, set the volume in a 100mL volumetric flask after cooling, filter through an aqueous membrane, and degas for later use.

[0047] 4. Filter the prepared mobile phase through a 0.45 μm membrane first, then degas it...

Embodiment 2

[0055] 1. Instruments used:

[0056] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0057](2) Column Kromstar C18 4.6×150mm 5μm

[0058] (3) Constant temperature column box: Ripley RPL-C2000

[0059] (4) Ultrasonic degassing device

[0060] 2. Detection conditions:

[0061] (1) Mobile phase: a. Water (containing 0.05% tetrabutylammonium chloride by volume); b. Acetonitrile; Mobile phase ratio V a :V b =80:20

[0062] (2) Detection wavelength: 220nm

[0063] (3) Flow rate: 0.8mL / min

[0064] (4) Injection volume: 20μL

[0065] (5) Column temperature: 30°C

[0066] 3. Sample processing:

[0067] Accurately weigh 0.01g of dimethyl isophthalate-5-sodium sulfonate, dissolve it with distilled water, set the volume in a 100mL volumetric flask after cooling, filter through an aqueous membrane, and degas for later use.

[0068] 4. Filter the prepared mobile phase through a 0.45 μm membrane first, then degas it by ultrasonic for 15 minut...

Embodiment 3

[0076] 1. Instruments used:

[0077] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0078] (2) Column Kromstar C18 4.6×150mm 5μm

[0079] (3) Constant temperature column box: Ripley RPL-C2000

[0080] (4) Ultrasonic degassing device

[0081] 2. Detection conditions:

[0082] (1) Mobile phase: a. 50mmol / L sodium dihydrogen phosphate solution (containing 0.05% tetrabutylammonium chloride by volume); b. methanol (chromatographically pure); mobile phase ratio V a :V b =40:60

[0083] (2) Detection wavelength: 220nm

[0084] (3) Flow rate: 0.8mL / min

[0085] (4) Injection volume: 20μL

[0086] (5) Column temperature: 30°C

[0087] 3. Sample processing:

[0088] Accurately weigh 0.01g of dimethyl isophthalate-5-sodium sulfonate, dissolve it with mobile phase a by slightly heating, after cooling, set the volume in a 100mL volumetric flask, filter through an aqueous membrane, and degas for later use.

[0089] 4. Filter the prepared mob...

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Abstract

The invention discloses a method for detecting m-benzene dimethyl isophthalate-5-sodium sulfonate purity by liquid chromatography. The method incudes using FL2200 liquid chromatograph, an N2000 chromatographic workstation and chromatographic column Kromstar C18 in 4.6X150 mm and 5 micrometers, the volume ratio of mobile phase a and mobile phase b is 80-90 to 10-20, detection wavelength is 220 nm, flow velocity is 0.8 mL / min, sample injection volume is 20 microliters, and columnar temperature is at 30 degrees Centigrade. By the method, detection time is shorter than 10 minutes, analysis accuracy is up to 0.01 ng, reproducibility is good, relative error is 0.2%, operation is simple, analysis is fully automatic, and quality of m-benzene dimethyl isophthalate-5-sodium sulfonate is effectively controlled.

Description

technical field [0001] The invention relates to a method for detecting the purity of dimethyl isophthalate-5-sodium sulfonate by using liquid chromatography, and belongs to the field of instrument analysis. Background technique [0002] Dimethyl isophthalate-5-sodium sulfonate (commonly known as three monomers, English abbreviation SIPM) is a new type of anionic surfactant with excellent performance. It is used in polyester (polyethylene terephthalate, PET fiber) ) plays an important role in dyeing modification. In the PET production process, adding SIPM as the third monomer can produce cationic dye-dyeable polyester fiber (CDP). As an important differential modifier for the production of modified polyester products (CDP / ECDP, etc.), it solves the problem of poor hygroscopicity, difficult dyeing, and easy dyeing of conventional polyester determined by the molecular structure of polyester after being added to chips (PET). There are many defects such as static electricity, ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N30/89G01N30/96G01N2030/027
Inventor 王青青王亮郭学阳庄玲孙立贞陈晓娟丁志娟赵小云熊激光王兆玲徐大鹏朱浩慧
Owner WEIFANG WORLD CHEM
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