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Method for measuring purity of 9-fluorenemethanol

A determination method and technology for purity, applied in the field of liquid chromatography analysis, can solve the problems of not involving the purity of 9-fluorene methanol, not involving the determination and determination of 9-fluorene methanol, etc.

Inactive Publication Date: 2008-02-27
BAOSHAN IRON & STEEL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, people have paid considerable attention to the research on the synthesis of 9-fluorenylmethanol, and it has developed rapidly. There are many reports on the data involved, but none of them involve the determination of 9-fluorenylmethanol, such as "Chemical Reagents", 2003 . to determine the purity of

Method used

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  • Method for measuring purity of 9-fluorenemethanol
  • Method for measuring purity of 9-fluorenemethanol
  • Method for measuring purity of 9-fluorenemethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Experimental equipment and chromatographic conditions:

[0051] The Agilent 1100 high-efficiency chromatograph was selected, equipped with an online vacuum degasser, a quaternary gradient pump, a 20 μl manual injector, a multi-wavelength ultraviolet detector, a column oven, and an Agilent 1100 chemical workstation.

[0052] The chromatographic column is Inertsil ODS-3, the filler particle size is 5μm, the column length is 15cm, and the inner diameter is 4.6mm; the flow rate: 1.0ml / min; the column temperature: 30°C; the detection wavelength: 232nm; the injection volume is 10μl.

[0053] Reagents and medicines:

[0054] The standard sample of 9-fluorenemethanol was provided by ACROS Company of Belgium, the product number is A0182055, and the purity is 99.8%. The standard sample was characterized by infrared spectrum, mass spectrum and nuclear magnetic resonance spectrum, and compared with the standard spectrum, the structure was confirmed. Methanol (chromatographic grad...

Embodiment 2

[0061] The chromatographic conditions are the same as in Example 1. Accurately weigh 28.76mg of 9-fluorenemethanol refined product sample and place in 100ml

[0062] In a clean and dry volumetric flask, dilute to the mark with chromatographically pure methanol, degas it with ultrasonic waves for 10 minutes, shake well, and inject the sample. Obtain the area A1=24558.3 ​​of 9-fluorenemethanol in the sample, calculate according to the following formula:

[0063]

[0064] x 1 : the purity of 9-fluorenemethanol in the refined product sample, %

[0065] x 标 : the purity of 9-fluorenemethanol in the known standard sample, %;

[0066] A 1 : the peak area of ​​the 9-fluorenemethanol component in the sample;

[0067] A 2 : the peak area of ​​the 9-fluorenemethanol component in the standard sample;

[0068] m 1 : mass of sample, g;

[0069] m 2 : mass of standard sample, g.

[0070] X 1 = 99 . 8 ...

Embodiment 3

[0075] The mobile phase is methanol: water=20: 80 (v / v), and other chromatographic conditions are the same as in Example 1. Accurately weigh 27.45mg of 9-fluorenemethanol crude product sample, place it in a 100ml clean and dry volumetric flask, and use chromatographic pure Dilute methanol to the mark, degas with ultrasonic wave for 10 minutes, shake well, and inject the sample. Obtain the area A1=18944.0 of 9-fluorenemethanol in the sample, calculate according to the following formula:

[0076]

[0077] x 1 : the purity of 9-fluorenemethanol in the refined product sample, %

[0078] x 标 : the purity of 9-fluorenemethanol in the known standard sample, %;

[0079] A 1 : the peak area of ​​the 9-fluorenemethanol component in the sample;

[0080] A 2 : the peak area of ​​the 9-fluorenemethanol component in the standard sample;

[0081] m 1 : mass of sample, g;

[0082] m 2 : mass of standard sample, g.

[0083] X 1 = ...

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Abstract

The invention discloses a purity measuring method of the 9-Fluorenylmethanol. Firstly it confects the marker of purity and the measured sample, then to detect relative chromatogram chart and the peak area using the HPLC; last to converse to 9-Fluorenylmethanol purity of the sample according to the quantity calculation formula of the external scaling method. The invention is first to use the HPLC and the ultraviolet multi-wave detector and the peak is edge and has high separation degree; the separating time is short; the relative standard deviation is 0.25% and the recovery rate is 98.1%-103.2%. The invention can be used to detect the 9-Fluorenylmethanol purity in production, use, the sale and study field.

Description

technical field [0001] The invention belongs to a liquid chromatography analysis method in the field of analytical chemistry, and more specifically relates to a method for measuring the purity of 9-fluorenemethanol by using a high performance liquid chromatography instrument. Background technique [0002] 9-Fluorenemethanol It is a white needle-like crystal with a melting point of 106-107°C and is insoluble in water. It is an important raw material for preparing functional pigments, dyes, medicines, pesticides, and polymer monomers, and its price is extremely expensive. 9-fluorenylmethanol is also an important intermediate of biochemical raw materials. It reacts with phosgene to generate 9-fluorenylmethyl chloroformate (Fmoc-Cl). Fmoc-Cl is a protective agent for the preparation of amino acids. In its synthesis important and unique. With the continuous development of biological science and technology, the preparation of amino-protecting agent products from 9-fluorenemeth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/26G01N30/86B01J20/281
Inventor 陈叶飞张秀云陈国敏陆惠萍
Owner BAOSHAN IRON & STEEL CO LTD
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