CN1134661C - Method for analyzing 1,3-diaminosulfourea by using high-performance liquid-phase chromatography - Google Patents

Abstract

The present invention relates to a method for analyzing 1, 3-bisthiosemicarbazide by high performance liquid chromatography, Zorbax-ODS is selected to be used as a supporter of a chromatographic column, methanol and water are prepared into a mobile phase, an ultraviolet multiwavelength detector is used for detecting a high performance liquid chromatograph, and a chromatographic external reference method is used for a quantity. The method has the advantages of product analysis instrument, little error of analysis result, quick analysis course, convenience and easy operation, the purity of a 1, 3-bisthiosemicarbazide product can be detected, and the method can also be used for detecting the content of 1, 3-bisthiosemicarbazide in solution and waste liquid containing micro 1, 3-bisthiosemicarbazide.

Description

A kind of with efficient liquid phase chromatographic analysis 1, the method for 3-diamido thiocarbamide

The invention belongs to a kind of 1, the analytical approach of 3-diamido thiocarbamide, relate in particular to a kind of with efficient liquid phase chromatographic analysis 1, the method for 3-diamido thiocarbamide.

1,3-diamido thiocarbamide is a kind of important chemical detection reagent and industrial chemicals, because it has important use value, people have carried out and develop synthetic from different channels.But present 1, the detection of 3-diamido thiocarbamide purity is that titrimetry is finished with chemical method, and error is bigger, and general error is greater than 3%.

The purpose of this invention is to provide a kind of efficient liquid phase chromatographic analysis 1 of using, the method for 3-diamido thiocarbamide is little with the resultant error of this methods analyst.

Goal of the invention of the present invention is to implement like this, and choosing Zorbax-ODS is chromatographic column carrier, is mixed with mobile phase with the first alcohol and water, analyzes with the ultraviolet multiwavelength detector on high performance liquid chromatograph, carries out quantitatively with the chromatogram external standard method.

Concrete operations step of the present invention is as follows:

(1) use high performance liquid chromatograph, the ultraviolet multiwavelength detector, column size is long 10-30cm, diameter 4-5cm;

(2) be chromatographic column carrier with Zorbax-ODS, it is methyl alcohol that the first alcohol and water is mixed with volume ratio: water=0: 100-20: 80 mobile phase;

(3) be mixed with the analytic sample solution that 0.1mg/ml-1mg/ml and separation system are complementary;

(4) after the stability and high efficiency liquid chromatograph, to chromatogram system sample introduction, sample size is 4 μ l-20 μ l; Flow velocity is 1.1ml/min, and the stratographic analysis time is 15-46 minute;

(5) after sample to be tested is separated, make the outer marking quantitative sample purity with standard model.

The present invention compared with prior art has following advantage:

1. errors of analytical results is little;

2. analytic process is quick, and is convenient easy to operate;

3. not only can detect 1, the purity of 3-diamido thiocarbamide product also can be used for detecting and contains trace

Embodiment 1

Use Tianjin, island LC-3A high speed liquid chromatograph SPD-1 ultraviolet multiwavelength detector, wavelength is 254mm, column size is that 25cm is long, 0.46cm diameter, chromatographic column carrier is Zorbax-ODS, mobile phase is that first Queensland alcohol and water is formed methyl alcohol: water=9: 91 (v/v), and sample ligand sample concentration is 0.2944mg/ml; Sample size is 10 μ l, and flow velocity is 1.1ml/min, and analysis result is 1, and 3-diamido thiocarbamide purity is 98.808% (w%) chromatographic fractionation figure such as Fig. 1.The error statistics that this analysis sample carries out measuring for four times is listed in table 1.

The same sample determination error examination of table 1

Sequence number	1	2	3	4
					Result (w%)	98.808	98.952	98.228	98.612

Embodiment 2

Mobile phase is a methyl alcohol: water=11.89 (v/v), sample ligand sample concentration 0.2950mg/ml; Sample size is 10 μ l; All the other are with embodiment 1, and analysis result is 1, and 3-diamido thiocarbamide purity is 96.503% (w%), chromatographic fractionation figure such as Fig. 2.

Embodiment 3

Mobile phase is a water, sample compound concentration 0.58mg/ml; Sample size is 20 μ l, and with embodiment 1,1,3-diamido thiocarbamide purity is 97.730% (w%), chromatographic fractionation figure such as Fig. 3.

Embodiment 4

Mobile phase is a methyl alcohol: water=20: 80 (v/v), sample ligand sample concentration 0.2952mg/ml; Sample size is 5 μ l, and analysis result is 1, the purity of 3-diamido thiocarbamide, chromatographic fractionation figure such as Fig. 4.

Claims (1)

1. one kind with efficient liquid phase chromatographic analysis 1, and the analytical approach of 3-diamido thiocarbamide is characterized in that operation steps is as follows:

(1) use high performance liquid chromatograph, the ultraviolet multiwavelength detector, column size is long 10-30cm, diameter 4-5cm;

(2) be chromatographic column carrier with Zorbax-ODS, it is methyl alcohol that the first alcohol and water is mixed with volume ratio: water=0: 100-20: 80 mobile phase;

(3) be mixed with the analytic sample solution that 0.1mg/ml-1mg/ml and separation system are complementary;

(4) after the stability and high efficiency liquid chromatograph, to chromatogram system sample introduction, sample size is 4 μ l-20 μ l; Flow velocity is 1.1ml/min, and the stratographic analysis time is 15-46 minute;

(5) after sample to be tested is separated, make the outer marking quantitative sample purity with standard model.

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