第一章 仪器分析实验的基本知识 1
一、实验室安全知识 1
二、仪器分析实验的基本要求 1
三、实验数据处理和结果表达 2
(一)评价分析方法和分析结果的基本指标 2
(二)分析数据和结果的表达 3
第二章 仪器的结构及使用 5
一、光谱分析仪器的结构及使用 5
(一)722型分光光度计 5
(二)T9紫外可见分光光度计 5
(三)LS 45荧光分光光度计 6
(四)Nicolet iS50 傅里叶红外光谱仪 7
(五)GGX-810原子吸收分光光度计 8
(六)5100 ICP-OES原子发射光谱仪 9
二、电化学仪器的结构及使用 10
(一)pHS-3C型酸度计 10
(二)KLT-1型通用库仑仪 11
(三)CHI660E电化学工作站 11
(四)Titrando 888型自动电位滴定仪 12
三、色谱分析仪器的结构及使用 13
(一)7820A气相色谱仪 13
(二)LC-20AD高效液相色谱仪 14
(三)BECKMAN P/ACE MDQ毛细管电泳仪 15
(四)Metrohm 861型离子色谱仪 16
(五)7890B-5977B GC-MSD气质联用仪 17
(六)6230 TOF液质联用仪 18
第三章 仪器分析实验 20
实验1 邻二氮菲分光光度法测定蜂蜜中铁含量 20
实验2 食品中NO- 2 含量的测定 22
实验3 紫外吸收光谱法测定蒽醌的含量和摩尔吸光系数 24
实验4 分光光度法同时测定铬和钴的含量 26
实验5 标准加入分光光度法测定钢中锰含量 27
实验6 硫酸阿托品片剂的染料比色法测定 29
实验7 紫外双波长法测定对氯苯酚存在时苯酚的含量 30
实验8 荧光法定量测定维生素B2 32
实验9 荧光分析法测定邻羟基苯甲酸和间羟基苯甲酸 33
实验10 荧光光谱法测定茶叶中铝离子含量 34
实验11 阿司匹林片剂中乙酰水杨酸的荧光测定 36
实验12 苯甲酸、乙酸乙酯的红外光谱测定 37
实验13 火焰原子吸收光谱法测定自来水的钙镁硬度 39
实验14 火焰原子吸收光谱法测定黄铜中的铜和铅 40
实验15 石墨炉原子吸收光谱法测定土壤中镉的含量 42
实验16 石墨炉原子吸收光谱法测定硒补充剂中的硒 44
实验17 电感耦合等离子原子发射光谱分析法测定废水中的镉、铬含量 45
实验18 ICP-AES法测定纯锌试样中的杂质元素 46
实验19 微波消解-ICP-AES法同时测定火腿中多种微量元素 48
实验20 电感耦合等离子体质谱法测定饮用纯净水中24种金属元素 49
实验21 直接电位法测定未知溶液的 pH 51
实验22 氟离子选择性电极法测定牙膏中总氟含量 53
实验23 氯离子选择性电极对溴离子选择性系数的测定 54
实验24 电位滴定法测定阿司匹林片剂中乙酰水杨酸的含量 56
实验25 自动电位滴定仪测定弱酸浓度及其解离常数 57
实验26 亚铁氰化物/铁氰化物氧化还原电对的循环伏安法研究 59
实验27 微分脉冲伏安法测定果汁饮料中的维生素C 61
实验28 阳极溶出伏安法测定水样中微量铅和镉 62
实验29 库仑滴定法测定维生素C药片中的抗坏血酸含量 64
实验30 混合酸的电导滴定 66
实验31 气相色谱法测定正构烷烃的组成和含量 68
实验32 气相色谱法测定漱口水中百里酚的含量 69
实验33 高效液相色谱法测定水样中间硝基苯酚含量 70
实验34 高效液相色谱法测定槐米中芦丁的含量 72
实验35 高效液相色谱法测定头孢氨苄的含量 73
实验36 高效液相色谱法测定绿茶饮料中咖啡因和茶碱的含量 75
实验37 高效液相色谱柱的性能考察及分离度测试 76
实验38 气相色谱-质谱联用分析菜籽油的脂肪酸成分 78
实验39 液相色谱-质谱联用技术对中药黄芩中黄芩苷的定性和定量分析 80
实验40 氨基酸的纸色谱鉴别 82
实验41 黄连药材的薄层色谱鉴别 83
实验42 离子色谱法测定自来水中的阴离子 85
实验43 毛细管区带电泳法分离氧氟沙星对映异构体 86
Chapter 1 Fundamentals of Instrumental Analysis Experiments 89
Ⅰ Laboratory Safety 89
Ⅱ Basic Requirements for Instrumental Analysis Experiment 89
Ⅲ Data Processing and Results Expression 90
(Ⅰ)Basic criteria to evaluate analytical methods and results 90
(Ⅱ)Data analysis and result expression 93
Chapter 2 The Structure and Operation of Instruments 94
Ⅰ The Components and Fundamentals of Spectrometers 94
(Ⅰ)722 spectrophotometer 94
(Ⅱ)T9 ultraviolet-visible spectrophotometer 95
(Ⅲ)LS 45 fluorescence spectrophotometer 96
(Ⅳ)FTIR Nicolet iS50 spectrometer 97
(Ⅴ)GGX-810 AAS 98
(Ⅵ)5100 ICP-OES 99
Ⅱ The Components and Fundamentals of Electrochemical Instruments 101
(Ⅰ)pHS-3C pH meter 101
(Ⅱ)KLT-1 universal coulomb meter 102
(Ⅲ)CHI 660E electrochemical workstation 103
(Ⅳ)888 Titrando automatic potentiometric titrator 104
Ⅲ The Components and Fundamentals of Chromatograph 106
(Ⅰ)7820A gas chromatograph 106
(Ⅱ)LC-20AD HPLC 107
(Ⅲ)BECKMAN P/ACE MDQ capillary electrophoresis system 108
(Ⅳ)Metrohm 861 ion chromatograph 109
(Ⅴ)7890B-5977B GC-MSD gas chromatograph-mass spectrometer 110
(Ⅵ)6230 TOF LC/MS 112
Chapter 3 Instrumental Analysis Experiments 114
Exp.1 Spectrophotometric Determination of Iron in Honey with 1，10-Phenanthroline 114
Exp.2 Determination of Nitrite in Food 117
Exp.3 Determination of Anthraquinone and Its Molar Absorptivity by Ultraviolet-Visible Spectroscopy 120
Exp.4 Simultaneous Determination of Chromium and Cobalt by Spectrophotometry 122
Exp.5 Measuring Manganese in Steel by Spectrophotometry with Standard Addition Method 123
Exp.6 Dye Colorimetric Determination of Atropine Sulfate Tablets 125
Exp.7 Determination of Phenol in the Presence of P-chlorophenol by Dual-wavelength UV Spectrometry 128
Exp.8 Quantitative Analysis of Vitamin B2by a Fluorometric Method 130
Exp.9 Determination of O-hydroxybenzoic Acid and M-hydroxybenzoic Acid by Fluorescence Analysis 132
Exp.10 Spectrofluorimetric Determination of Aluminum Ions via Complexation with 8-Hydroxyquinoline 133
Exp.11 Fluorometric Determination of Acetylsalicylic Acid in an Aspirin Tablet 135
Exp.12 Determination of Benzoic Acid and Ethyl Acetate by Infrared Spectroscopy 137
Exp.13 Determination of Water Hardness of Tap Water by Flame Atomic Absorption Spectrometry 139
Exp.14 Determination of Cu and Pb in Brass by Flame Atomic Absorbance Spectroscopy 141
Exp.15 Determination of Cadmium Content in Soil by Graphite Furnace Atomic Absorption Spectrometry 143
Exp.16 Determination of Selenium in Selenium Supplements by Graphite Furnace Atomic Absorption Spectrometry 146
Exp.17 Determination of Cd and Cr in Wastewater by ICP-AES 148
Exp.18 Determination of Impurity Elements in Pure Zinc Samples by ICP-AES 149
Exp.19 Simultaneous Determination of Trace Multi-element in Ham by Microwave Digestion-ICP-AES 151
Exp.20 Determination of Metal Elements in Purified Drinking Water by Inductively Coupled Plasma Mass Spectrometry 153
Exp.21 Determination of pH of an Unknown Sample Using Potentiometry 155
Exp.22 Determination of the Total Fluorine Content in Toothpaste Using Fluoride Ion Selective Electrode 157
Exp.23 Measuring Selectivity Coefficient of Chloride Ion Electrode to Bromine Ion 159
Exp.24 Determination of the Acetylsalicylic Acid in Aspirin Tablet by Potentiometric Titration 162
Exp.25 Determination the Concentration of Weak Acids and Its Dissociation Constants by Automatic Potentiometric Titration 164
Exp.26 Study of Ferrocyanide/Ferricyanide Redox Couple by Cyclic Voltammetry 166
Exp.27 Determination of Vitamin C in Fruit Juice Beverages by Differential Pulse Voltammetry 169
Exp.28 Determination of Trace Lead and Cadmium in Water Samples by Anodic Stripping Voltammetry 171
Exp.29 Determination of Ascorbic Acid in Vitamin C Tablets by Coulometric Titration 173
Exp.30 Conductometric Titration of Mixed Acids 176
Exp.31 Determination of the Composition and Content of n-Alkanes by Gas Chromatography 178
Exp.32 Quantification of Thymol in Mouthwash by Gas Chromatography 180
Exp.33 Determination of m-Nitrophenol Content in Water Samples by High-performance Liquid Chromatography 181
Exp.34 Determination of Rutin in Locust Rice by HPLC 183
Exp.35 Determination of Cephalexin Capsules by HPLC 185
Exp.36 Determination of Caffeine and Theophylline in Green Tea Beverages by HPLC 187
Exp.37 Evaluation of the Performance of HPLC Column and Determination of Resolution 189
Exp.38 Analysis of the Composition of Fatty Acid in Rapeseed Oil by Gas Chromatography-Mass Spectrometry 191
Exp.39 Qualitative and Quantitative Analysis of Baicalin in Radix Scutellariae by Liquid Chromatography-Mass Spectrometry 194
Exp.40 Paper Chromatography Identification of Amino Acids 197
Exp.41 The Identification of Rhizoma Coptidis by Thin Layer Chromatography 199
Exp.42 Determination of Anions in Tap Water by Ion Chromatography 201
Exp.43 Chiral Separation of Ofloxacin Enantiomer by Capillary Zone Electrophoresis 203
参考文献 206
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