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A kind of quantitative method utilizing hplc method to detect cyanamide

A technology of cyanamide and dicyandiamide, which is applied in the quantitative field of cyanamide detection by HPLC, can solve the problems of scarcity of fluorescence detectors, large human error, high price, etc., and achieve high accuracy and precision , The method is simple and easy to implement

Active Publication Date: 2016-07-20
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, although the chemical analysis method and the potentiometric titration method are relatively simple, they take a long time and have large human errors.
In addition, the detection method of cyanamide reported in the literature is to use a fluorescence detector to detect after pre-column derivatization. This method is time-consuming, and the fluorescence detector is relatively rare and expensive.

Method used

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  • A kind of quantitative method utilizing hplc method to detect cyanamide
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  • A kind of quantitative method utilizing hplc method to detect cyanamide

Examples

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Effect test

Embodiment 1

[0031] There is a batch of 100 kilograms of cyanamide aqueous solution within a certain concentration range, and it is necessary to detect the concentration of cyanamide.

[0032] The high-performance liquid chromatography conditions adopted are: the chromatographic column is InertsilODS-SP, the column length is 150 mm, and the column inner diameter is 5 μm; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 240 nm; the column temperature is 30 ° C; The phase was 5% methanol in water; the flow rate was 0.5 ml / min.

[0033] A kind of quantitative method utilizing HPLC method to detect cyanamide, adopts high-performance liquid chromatograph to detect, internal standard method quantitative analysis, concrete steps comprise:

[0034] (1) prepare cyanamide standard stock solution

[0035] Accurately weigh 1000mg of cyanamide standard substance (purity 98%) in a 500ml volumetric flask, and use 5% methanol aqueous solution to make ...

Embodiment 2

[0057] There is an existing batch of 300 kg of cyanamide aqueous solution with unknown concentration, and the concentration of cyanamide needs to be detected.

[0058] The high-performance liquid chromatography conditions adopted are: the chromatographic column is InertsilODS-SP, the column length is 150 mm, and the column inner diameter is 5 μm; the detector is a variable wavelength ultraviolet absorption detector; the detection wavelength is 240 nm; the column temperature is 20 ° C; The phase was 5% methanol in water; the flow rate was 0.3 ml / min.

[0059] A kind of quantitative method utilizing HPLC method to detect cyanamide, adopts high-performance liquid chromatograph to detect, internal standard method quantitative analysis, concrete steps comprise:

[0060] (1) prepare monodicyandiamide standard stock solution

[0061] Step is with embodiment 1

[0062] (2) prepare cyanamide standard solution

[0063] Step is with embodiment 1

[0064] (3) Standard curve drawing

...

Embodiment 3

[0081] There is an existing batch of 500 kg of cyanamide with unknown content, and the content of cyanamide needs to be tested.

[0082] The high-performance liquid chromatography conditions adopted are: the chromatographic column is InertsilODS-SP, the column length is 150 mm, and the column inner diameter is 5 μm; the detector is a variable wavelength ultraviolet absorption detector; the detection wavelength is 240 nm; the column temperature is 25 ° C; The phase was 5% methanol in water; the flow rate was 0.4 ml / min.

[0083] A kind of quantitative method utilizing HPLC method to detect cyanamide, adopts high-performance liquid chromatograph to detect, internal standard method quantitative analysis, concrete steps comprise:

[0084] (1) prepare monodicyandiamide standard stock solution

[0085] Step is with embodiment 1

[0086] (2) prepare cyanamide standard solution

[0087] Step is with embodiment 1

[0088] (3) Standard curve drawing

[0089] Step is with embodiment...

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Abstract

The invention discloses a quantitative method of detecting cyanamide by utilizing an HPLC method. According to the quantitative method, a Shimazu high performance liquid chromatograph instrument SPD-20A is adopted, an Inertsil ODS-SP chromatographic column is used as a separation chromatography column, and the column temperature is 30 DEG C; a variable wavelength ultraviolet absorbance detector is adopted the detection wavelength is 240nm; methanol and water (5+95)(V+V) (i.e. 5 percent methanol aqueous solution) is used as a mobile phase and the flow rate of the mobile phase is 0.3ml / min; and dicyandiamide is used as an internal standard, a concentration ratio-peak area ratio standard curve of cyanamide and dicyandiamide is drawn by using an internal standard method to obtain a regression equation of the standard curve, and the content of the cyanamide is worked out by virtue of the regression equation. The quantitative method is capable of directly detecting a sample without any pretreatment of the sample, so that the analysis time is greatly shortened; in addition, the quantitative method is simple, feasible, convenient and reliable.

Description

technical field [0001] The invention belongs to the technical field of analysis, and relates to a quantitative analysis method for cyanamide, in particular to a quantitative method for detecting cyanamide by using an HPLC method. Background technique [0002] Crystal cyanamide (Cyanamide, CN 2 h 2 ) is unstable, diamond-shaped, colorless, deliquescent, and its melting point is 46°C. Cyanamide has high solubility in water and is weakly alkaline, and it is completely miscible with water at 43°C. Cyanamide contains cyano group and amino group, both of which are active groups. They have the multiple reactivity of the above-mentioned functional groups, and are prone to reactions such as addition, substitution, and condensation. [0003] The industrial production of cyanamide in foreign countries began in the late 1930s. It was obtained by the action of calcium cyanamide and acid, and then gradually evolved into calcium cyanamide, CO 2 , Water raw material process route. Mode...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 董昭苹吴文雷姚刚徐萍萍张锐李晓红吕印美
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD