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A kind of method for detecting the purity of dimethyl isophthalate-5-sodium sulfonate by liquid chromatography

A technology of dimethyl isophthalate and liquid chromatography, applied in the field of instrument analysis, can solve the problems of not being able to further reflect the inherent quality of the product, failing to provide guidance for improving the quality, difficult to vaporize, etc., to achieve the best separation effect, Small error, time-consuming effect

Active Publication Date: 2016-10-05
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

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  • A kind of method for detecting the purity of dimethyl isophthalate-5-sodium sulfonate by liquid chromatography
  • A kind of method for detecting the purity of dimethyl isophthalate-5-sodium sulfonate by liquid chromatography
  • A kind of method for detecting the purity of dimethyl isophthalate-5-sodium sulfonate by liquid chromatography

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Experimental program
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Effect test

Embodiment 1

[0030] A method of liquid chromatography detection dimethyl isophthalate-5-sodium sulfonate purity:

[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 l...

Embodiment 2

[0054] A method of liquid chromatography detection dimethyl isophthalate-5-sodium sulfonate purity:

[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. Filt...

Embodiment 3

[0075] A method of liquid chromatography detection dimethyl isophthalate-5-sodium sulfonate purity:

[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 f...

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Abstract

The invention discloses a method for detecting the purity of dimethyl isophthalate-5-sodium sulfonate by liquid chromatography, using FL2200 liquid chromatography, N2000 chromatographic workstation, and the specification of chromatographic column Kromstar C18 is 4.6×150mm 5 μm The volume ratio of mobile phase a and mobile phase b is 80-90:10-20; detection wavelength: 220nm; flow rate: 0.8mL / min; injection volume: 20 μ L; column temperature: 30 ℃; use detection method of the present invention , the detection time is less than 10 minutes; the analysis accuracy can reach 0.01ng; the reproducibility is good, the relative error is 0.2%; the operation is simple and the analysis is fully automated; the quality of dimethyl isophthalate 5 sulfonate is achieved. purpose of effective control.

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 Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N30/89G01N30/96G01N2030/027
Inventor 王青青王亮郭学阳翟浩桐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郭祥荣杨荣华杨明晖孙春辉刘梅
Owner WEIFANG WORLD CHEM
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