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作 者:杨晓峰[1] 李巧玲[1] 陈志萍[1] 田翠芳[1] 王海花[2]
机构地区:[1]中北大学理学院化学系,山西太原030051 [2]山西生物应用职业技术学院,山西太原030031
出 处:《化学试剂》2008年第9期669-671,共3页Chemical Reagents
基 金:山西省高等学校优秀青年学术带头人支持计划资助(2005);山西省科技攻关项目(051151);中北大学校基金项目
摘 要:以自制双(4-甲苯基)苯基硫化膦(BMPPS)粗品为原料,经多次重结晶提纯后,用薄层色谱(TLC)、高效液相色谱(HPLC)进行分析,纯品BMPPS的纯度为99.2%,可用作定量分析对照品。对纯品UV扫描发现,BMPPS的吡啶溶液在303nm处有稳定吸收,在浓度为8×10^-4~4×10^-3mol/L范围内吸光度与浓度呈良好的线性关系,回归方程为:y=190.6x+0.377,r=0.9978。加标回收率为98.5%~103.8%,方法重现性良好,可用作合成BMPPS粗品的定量分析。The control sample of bis (4-methylpbenyl) phenyl phosphine sulfide (BMPPS) was obtained by recrystallization of a serf-prepared crude starting material. And the purity of BMPPS, which was measured with thin-layer chromatography and high pressure liquid chromatographic analysis, was 99.2 %. The ultraviolet-visible spectruphotometric scanning showed that the solution of BMPPS in pyridine revealed a maximum stable absorption at 303 nm. And the concentration of BMPPS was correlated very well to its optical density in the range of 8×10^-4mol/L-4×10^-3mol/L mol/L.The regression equation is y = 190.6x + 0.377 with a relativity coefficient of 0. 998 7. When the method was used to analyze the crude BMPPS, recovery of control is 98.5% - 103.8% with a better repeatability. Ultraviolet spectruphometric method is a feasible instrument, for quantitative analysis of crude BMPPS.
关 键 词:双(4-甲苯基)苯基硫化膦 对照品 制备 定量分析
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