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Jingdong book

分析化学中的样品制备技术

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分析化学中的样品制备技术

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分析化学中的样品制备技术》汇总了目前各种先进的、用于各类分析仪器的样品制备技术。其中涉及的技术力求广泛、全面、系统、深入、先进,为化学、生物学、药学、环境和材料科学领域中的工作者提供参考,也为本科生和研究生的深入学习提供素材。
Content Description

《分析化学中的样品制备技术》的主要内容包括:液体和固体样品中挥发性有机化合物的萃取;金属分析的样品前处理方法;DNA分析中的样品制备;RNA分析中的样品前处理;核酸的提取、分离和纯化技术;固体薄膜显微表征与光谱表征的样品制备;拉曼光谱和红外光谱表面增强分析中样本和基底制备技术。
Catalogue

第一章 分析视角的样品制备
1.1 测试过程
1.1.1 定性与定量分析
1.1.2 定量分析方法
1.2 定量分析误差
1.2.1 准确度
1.2 2精密度
1.2.3 样品制备中的统计学
1.3 方法性能与方法认证
1.3.1 灵敏度
1.3.2 检测限
1.3.3 定量范围
1.3.4 其他重要的参数
1.3.5 方法确认
1.4 样品的保存
1.4.1 挥发性
1.4.2 存储容器的选择
1.4.3 空气中的气体吸附
1.4.4 化学变化
1.4.5 不稳定固体的保存
1.5 萃取后的样品制备程序
1.5.1 样品萃取物的浓缩
1.5.2 样品净化
1.6 样品制备过程中的质量保证和质量控制
1.6.1 准确度与精密度测定
1.6.2 统计控制
1.6.3 基质控制
1.6.4 污染控制
参考文献

第二章 萃取原理及液体中半挥发有机物的萃取
2.1 萃取原理
2.1.1 挥发
2.1.2 疏水性
2.1.3 酸碱平衡
2.1.4 疏水性离子有机化合物的分配
2.2 液液萃取-
2.2.1 回收率
2.2.2 液液萃取方法
2.2.3 液液萃取程序
2.2.4 液液萃取技术研究进展
2.3 液固萃取
2.3.1 吸附
2.4 固相萃取
2.4.1 固相萃取中的吸附剂
2.4.2 吸附剂选择
2.4.3 回收率
2.4.4 方法
2.4.5 程序
2.4.6 固相萃取技术最新进展
2.5 固相微萃取
2.5.1 吸附剂
2.5.2 吸附剂的选择
2.5 3 方法学
2 5.4 最新技术进展
2.6 搅拌棒吸附萃取
2.6.1 吸附剂与待测物回收
2.6.2 方法
2.6.3 最新技术进展
2.7 方法比较
参考文献

第三章 固体基质中半挥发有机物的萃取
3.1 引言
3.1.1 萃取原理
3.1.2 预萃取程序
3.1.3 萃取后程序
3.2 索氏萃取和自动索氏萃取
3.2.1 索氏萃取
3.2.2 自动索氏萃取
3.2.3 索氏萃取和自动索氏萃取的对比
3.3 超声波萃取
3.3.1 超声波萃取的应用及与索氏萃取的对比
3.4 超临界流体萃取
3.4.1 超临界流体萃取的基本理论
3.4.2 超临界流体萃取的仪器
3.4.3 超临界流体萃取的操作程序
3.4.4 超临界流体萃取的优缺点及应用
3.5 加速溶剂萃取
3.5.1 加速溶剂萃取的基本理论
3.5.2 加速溶剂萃取的仪器
3.5.3 加速溶剂萃取的操作程序
3.5.4 加速溶剂萃取的操作参数
3.5 5加速溶剂萃取的优点和应用
3.6 微波辅助萃取
3.6.1 微波辅助萃取的基本理论
3.6.2 微波辅助萃取的仪器
3.6.3 微波辅助萃取的操作程序和优缺点
3.6.4 微波辅助萃取的操作参数
3.6.5 微波辅助萃取的应用
3.7 各种萃取方法比较
参考文献

第四章 液体和固体样品中挥发性有机化合物的萃取
第五章 金属分析的样品前处理方法
第六章 DNA分析中的样品制备
第七章 RNA分析中的样品前处理
第八章 核酸的提取、分离和纯化技术
第九章 固体薄膜显微表征与光谱表征的样品制备
第十章 拉曼光谱和红外光谱表面增强分析中样本和基底制备技术
Book Abstract

如上所述,固相萃取中微粒可能导致吸附剂堵塞或者形成通道,因此在进行同相萃取或者其他分析程序时,必须考虑样品中可能存在的与待测物有关的微粒和胶体物质的污染。有机待测物在溶液相、胶体物质和悬浮微粒中的分配受多种平衡的控制。根据待测物和杂质的化学特性,一些待测物分子可能会吸附在样品中的杂质微粒或胶体物质上。待测物能黏附在生物颗粒,如细胞残核上或者结合在胶体蛋白质上。同样,待测物也能黏附在环境微粒上或与胶体腐殖物质结合。如果样品没有经过过滤,微粒可能部分或者全部从吸附剂中洗脱,当对样品进行分析时,导致溶解杂质和颗粒杂质对结果的影响。除了考虑水样中的固体悬浮微粒可能会堵塞固相萃取吸附剂以及待测物会被吸附在微粒上外,如果有细小的微粒通过固相萃取剂的孔洞,则会导致待测物的损失。
为了,避免这些问题,确保获得一致的分析结果,需要在固相萃取分析之前过滤除去样品中的杂质微粒。测定待测物与溶液中杂质的结合程度,或者相反,测定真实溶液中待测物与杂质的不相关程度很重要,因此样品应该在进行固相萃取或者液液萃取之前进行过滤。不含有机黏合剂的玻璃纤维过滤器,在捕获微粒的同时对待测物是惰性的。直径在1um以上的杂质可以通过重力从溶液中清除。文献中普遍报道的用于固相萃取样品制备的常用过滤器孔径为0.7、0 45或0.22/um。根据被分析样品的特殊基质选用合适尺寸的过滤器,并在固相萃取之前一直使用该过滤器。然后对保留在过滤器上的物质进行分析,以确定结合的待测物的量。还需要仔细评估用水或者用一种有机溶剂清洗过滤器,然后将清洗液与过滤的样品合并是否满足分析的目的,对指定的分析是否合适。
……

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