SMALL-BORE COLUMNS OF 1 mm I. D. FOR HPLC

The performance of small-bore columns of 1 mm I. D. for HPLC is described. The effect of mobile phase velocity and connecting effect on the values of H, a′, b′ and β are investigated. By operating at mobile phase velocity of 0.8 mm/s, the column of 200×1 mm I. D. packed with YWG-5μm (silica gel) can give the efficiency of about 11,000 plates which meet the needs of ordinary analysis. Oompared with column of 150×2 mm I. D., the solvent consumption is reduced to 1/3. The value of n~∞/t_r~0 about 700 T. P./s can be obtained. But the value of β is rather large. It needs further to be improved. Coupling 5 columns of 200×1 mm I. D., the efficiency of about 50,000 plates can be obtained. For a column of 1000×1 mm I. D. packed directly, the efficiency of 70,000 plates was achieved. Some applications of 1 mm I. D. column are given. We propose to use the column of 200×1mm I. D. in the routine analysis.     

细内径高效液相色谱柱

本文采用自制的专门设计的柱系统可使“边壁效应”减至最小.不同溶质在不同内径的柱子上其保留体积V_R和峰宽(体积单位)间有一近似的线性关系,2△V_1/2=a’+b’V_R. 文中系统考查了鉴定器系统体积对a’和b’值的影响,指出鉴定器系统的体积对a’值有很大的影响,而对b’值几乎没有什么影响.使用改进的柱系统和自制的紫外鉴定器.在2毫米内径10厘米长的柱子上获得了6000理论塔板数.     

色谱流出曲线的曲线拟合法

通常人们把色谱流出曲线假设为高斯分布函数,但实际上真正的高斯峰很难由实验获得。由于实际峰型是非高斯型分布,往往使得理论预测值与实验值之间存在一定误差。例如由高斯计算的分离度K_1(及K_3)总是大于实测值。这主要由于实际峰往往是不对称的拖尾峰,峰尾使得实际分离度不如理论上由高斯对称曲线所预测的结果。为了定量描述拖尾峰的特征,许多作者采用了按指数规律卷积的高斯分布曲线数学模型:     

1mm细内径高效液相色谱柱

本文报道了内径为1mm的高效液相色谱柱性能,考察了冲洗剂线速度和接头效应对理论塔板高度H和a′,b′,β′值的影响.当流动相线速为 0.8mm/s时,φ1×200mm柱柱数可达11000理论塔板以上,已能满足大多数常规分析的需要.其溶剂消耗量仅为柱效相近的φ2×150mm 柱的 1/3,n~∞/t_r~o值可达700 T.P/s,但此时β较大,有待进一步改进.5根20 cm长柱串联后柱效可达50000 T.P,直接装填的1m 柱柱效可达70000 T.P.文中给出了快速分离谱图和复杂样品的分离谱图.建议在日常分析中采用φ1×200mm柱。