Method for high-performance liquid phase chromatographic analysis on content of 4,5-dinitro-2,7-naphthalenedisulfonic acid serving as an intermediate
A high performance liquid chromatography, naphthalene disulfonic acid technology, applied in the direction of analysis materials, measuring devices, material separation, etc., to achieve the effect of short analysis time and simple method
Inactive Publication Date: 2015-04-29
ZAOZHUANG UNIV +1
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There is no public report on the accurate determination of the content of 4,5-dinitro-2,7-naphthalene disulfonic acid in the prior art
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Embodiment 1
[0048] see Figure 1-5 , in an embodiment of the present invention, a high-performance liquid chromatography analysis method for the content of the intermediate 4,5-dinitro-2,7-naphthalene disulfonic acid, the method comprising the following steps:
[0049] 1. Mobile phase selection and detection wavelength selection:
[0050] 1) Selection of mobile phase
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Abstract
The invention discloses a method for high-performance liquid phase chromatographic analysis on the content of 4,5-dinitro-2,7-naphthalenedisulfonic acid serving as an intermediate. According the method, reversed phase high-performance liquid chromatography is adopted, wherein the high-performance liquid chromatography comprises the following conditions: a chromatographic column is a 5 mu m XDB-C18 column of 150*4.6 mm, and gradient elution is carried out according to the following conditions by using the following compositions according to the volume ratio: 0 min 1% methanol-99% Li2SO4 with the flow rate of 1.0 mL.min<-1>, 8 min 1% methanol-99% Li2SO4 with the flow rate of 1.0 mL.min<-1>, 9 min 10% methanol-90% Li2SO4 with the flow rate of 1.0 mL.min<-1>, and 10 min 15% methanol-85% Li2SO4 with the flow rate of 1.0 mL.min<-1>; and the ultraviolet detection wavelength is 233 nm, and the injection volume is 20 muL. The method for high-performance liquid phase chromatographic analysis on the content of 4,5-dinitro-2,7-naphthalenedisulfonic acid serving as an intermediate disclosed by the invention can be used for accurately determining the content of 4,5-dinitro-2,7-naphthalenedisulfonic acid as well as the contents of the intermediate 4-nitro-2,7-naphthalenedisulfonic acid and 2,7-naphthalenedisulfonic acid, and is applied to the quality control of 4,5-dinitro-2,7-naphthalenedisulfonic acid during industrial production of H acids.
Description
technical field [0001] The invention relates to the field of analytical chemistry, in particular to a high performance liquid chromatography analysis method for the content of an intermediate 4,5-dinitro-2,7-naphthalene disulfonic acid. Background technique [0002] H acid (1-amino-8-naphthol-3,6-disulfonic acid) is an important intermediate in the dye industry, mainly used in the production of acid, direct and reactive dyes, such as acid magenta 6B, acid scarlet G, acid There are more than 90 kinds of black 10B, direct black, reactive brilliant red K-2BP, reactive purple K-3R, reactive dark blue K-R, etc. These dyes are used for dyeing wool spinning and cotton fabrics, and can also be used for the production of medicines. The global annual demand reaches ten More than 50,000 tons. [0003] The traditional H-acid production method uses refined naphthalene as a raw material, and the product is obtained through sulfonation, nitration, reduction and other steps. Among them, mi...
Claims
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Inventor 吴鸿伟刘雪静曹晗张浩男马可可刘晓兰马苗苗刘秀丽卢国艳王莹
Owner ZAOZHUANG UNIV
