Studies On Analytical Method Of The Intermediate Of Pyrimidine Thiadiazolidines Herbicide PTL-6 By Chromatography

Gas chromatography is a simple and effective method with quick and sensitive reaction. At present about 70% of the retention analysis uses gas chromatography.With a wide application, high performance liquid chromatography can be employed in retention analysis with little disturbance, high speed,which also makes up for the deficiency of gas chromatography. This thesis makes systematic research about analytical method of the new herbicide the intermediate of PTL-6 synthesis with these two machine analytical methods . This thesis mainly deals with:1. A method for the determination of 2,4- dichlorbenzoxy acetyl chloride of derivation before column, with gas chromatography has been developed. With a column ov-17 (2%); on Chromosorb W AW-DMCS (60-80mesh). 1.5m glass column with 3.2mm i.d. at 160℃,FID at 190℃ ,N2 as carrier gas with flow rate of 40mL/min , H2 as burning gas with flow rate of 50mL/min ,air flow with a rate of 500mL/min ,the attenuation is 2 ,and the paper speed is 2mm/min, range 102. Using octadecane as an internal standard ,the average recoveries are 96.89-99.65% while the relative standard deviation is 2.67, the coefficient of variation is 2.83%. A good linearity is obtained in the concentration range of 0.82-1.64mg/mL, r=0.9998.2. A gas chromatography method for the quanti- tative of 2-amino-4, 6-dimethyl pyrimidine is described. With the column ov-17(2%) on Chromosorb W AW- DMCS(60-80 mesh), 1.5m glass column with 3.2mm i.d. at 130℃,FED at 160℃,N2as carrier gas with flow rate of 40mL/min ,H2 as burning gas with flow rate of 50mL/min ,air flow rate is 500mL/min,attenuation is 3, and the paper speed is 2mm/min, range 102 .Using pentadecane as an internal standard ,the linear range of this method is 0.26-0.78mg/mL,r=0.9966, the average recoveries are 101.76-106.33% while the relative standard deviation is 1.55, the coefficient of variation is 1.66%.3. In this paper a high performance liquid chromatographic method for the separation and determination of herbicide GS-6 is described. Impurities in the herbicide GS-6 does not interfere with the determination. Chromatographicconditions are Agilent ZORBAX XDB-C8 (4.6mm i.d. 150mm,5um),with the mobile phase of methanol-water(77:23 v/v) and DAD detector UV at 232nm. Quantification is carried out with the external standard. The standard deviation is 1.23,variation coefficient is 1.61% and average recoveries are 95.67-99.84%. The linear range is 0.016-0.048mg/mL, Linear relative coefficient is 1.0000.4.It also deals with the study on the waste recycle in synthesizing herbicide PTL-6. With an analysis of the kinds and the amount of waste produced from synthesizing course, and the proper process of recycling.