2011检仪器分析实验.docVIP

实验 吸收曲线的绘制 4月12日 一、目的：1.巩固分光光度计的使用方法。2.学会测绘吸收曲线的一般方法。 二、提要：有色溶液对可见光的吸收具有选择性。利用分光光度计连续变换波长，可测绘出固定浓度的有色溶液在可见光区的吸收曲线。如果仪器所能提供的单色光不够纯，测得吸收曲线不够精密，但它仍可反映出溶液吸收最强的光带波段；所以，仍可用作光电比色时选择波长的依据。 本实验用分光光度计测定在可见光区的吸收曲线。 三、仪器和药品 722型分光光度计（或721型分光光度计） 2．、50g/mL 溶液 操作步骤 3.1 将50、20g/mL 溶液（后两溶液自己稀释）置于1cm厚的吸收池中.将蒸馏水装于另一只1cm厚的吸收池中作空白，分别置于吸收池架上 3.2 在仪器波长范围内，由小到大测量A值。即，从350 ~ 750 nm（或430~690nm）每间隔20nm测一数据，而在470nm ~ 590nm的吸收波段，为确保曲线精确, 应以每5nm间隔测定一次。 3.3将测得数据写在数据记录表中。以波长为横坐标，吸光度为纵坐标绘制吸收曲线(A~曲线)。 三、注意事项 1、每变换一次波长，应用空白调T( 100％)。2、绘制曲线的坐标标度大小适中，应符合要求。 3、要标明曲线名称, 坐标单位, 箭头要规范。 四、数据记录和实验报告 数据记录 （nm） A 2、绘制A~曲线，标出 五、思考题 1、单色光不纯, 对测定吸收曲线有什么影响？ 2、为什么每变换一次波长需用空白重调T(100％)。 EXPERIMENT Spectrophotometric Determination of Iron 4月19日 I. Outline Traces of iron are determined spectrophotometrically as a complex of iron (II). The classic reagent used to determine iron (after reduction to iron (II)) is the organic reagent 1,10-phenanthroline (Phen) .This reagent has the empirical formula C12H8N2 and the structural formula its another name is ferroin. The complex contains three molecules of 1,10-phenanthroline to one of iron: Several other metal ions also form complexes with 1.10-phenanthroline , but none is as intensely colored as the ferrous complex . The principal interferences are silver(I), cobalt(II) , copper(II) , and nickel (II) . A mixture of citric acid and ethylenediaminetetraacetic acid can be used to mask silver (I) , copper(II) , nickel (II) , and large amounts of other common metal ions . The method can be used for absorptivity (1.11×104) of the iron complex . The detection limit (A = 0.01) is about 1×10-6mol/L ,and the usual range for analysis is 0.4 to 8ppm of iron in a 1 cm cell. In the procedure, iron is first reduced to Fe2+ with an reducing agent , such as hydroxylamine hydrochloride .Then 1,10-phenanthroline solution is added in excess of the amount required to react with Fe2+,and the pH of the solution is adjusted by means of an ac