c第三章 前处理与效能指标.ppt

Sample pre-treatment and method validation ;基本要求;Fundamental requirement ;Pre-treatment of qualitative analysis and typical validation characteristics;Pre-treatment of qualitative analysis;（一）湿法破坏：硝酸-高氯酸法、硝酸-硫 酸法、硫酸-硫酸盐法、其他湿法； （二）干法破坏：本法适用于湿法不易破坏完全的有机物以及某些不能用硫酸进行破坏的有机药物。不适用于含易挥发性金属（如汞、砷等）有机药物的破坏。 （三）氧瓶燃烧法：系将有机药物放入充满氧气的密闭的燃烧瓶中进行燃烧，并将燃烧所产生的欲测物质吸收于适当的吸收液中，然后根据欲测物质的性质，采用适宜的分析方法进行鉴别、检查或测定含卤素有机药物或含硫、氮、硒等其它元素的有机药物。;（一）Wet destruction：nitric acid- perchloric acid method、nitric acid-sulfuric acid method、sulfuric acid-sulfate method、and other wet methods； （二）Dry destruction：This method is used for organic substances which are not easily destroyed by wet method and some organic drugs which can not be destroyed by sulfuric acid. Organic drugs containing easily volatile metals, such as mercury and arsenic, is not suitable. ;Oxygen flask combustion ;INSTRUMENTATION;The absorbing liquid and assay;Amiodarone NaOH solution the determination of iodine, excess hydrochloride 2ml of acetic anhydride-bromine is added, ; Sodium sulfo- concentrated H2O2solution the determination of sulfur, bromophthalein 0.5ml and H2O30ml adding barium chloride, gravimetric methods ;Precautions: We should operate as the prescriptive procedure. Saturation of the liquid with oxygen is essential for the successful performance of the combustion procedure. The combustion is completely absorbed by the absorbing liquid, shake the flask vigorously, and allow to stand for 15min with intermittent shaking. The smog of iodine is purple. The smog of bromine is umber. The smog of chlorine and fluorine is white. Quartzose flask is used for the determination of fluoride. ;Typical Validation Characteristics;Accuracy;Accuracy;Example of an Accuracy Data Set;Precision;Example of a Precision Data Set;Precision: Repeatability;Intermediate Precision;Repeatability;Rep