AA Technique.ppt

October 99 VGE/EX/T/0: Issue 1 AA The Technique Flame, Furnace, Vapour The AAS Technique Introduction to AAS Theory of Atomic Spectroscopy Relation between Energy States and Wavelength Principle of Atomic Absorption Absorption from the Hollow Cathode Lamp Schematic of an Atomic Absorption system Optical system Optical system Optical system-Single/Double beam Optical system-Single/Double beam Hollow Cathode Lamp Lamp Power Supplies Flame-Burners Flame-Burner Jaw Profile Flame-Nebuliser Flame-Spray Chamber Flame Process 雾化 M+ A- (solution) M+ A- (aerosol) 蒸发 M+ A- (aerosol) MA (solid) 液化 MA (solid) MA (liquid) 气化 MA (liquid) MA (gas) 原子化 MA (gas) M° + A° (gas) 原子化后: 激发 M° + A° (gas) M* (gas) 离子化 M* (gas) M+ + e- (gas) 或: 吸收 M° + h? M*(gas) Flame Types Air Acetylene Flame 贫燃火焰 = 0.8 to 1.0 L/min 热焰通常用于Bi, Cu, Au, Li, Mn, Ni, Ag等元素. 化学计量火焰 = 1.0 to 1.2 L/min 用于 Sb, Cd, In, Ir, Pb, Hg, Pd, Pt, K, Rb等元素. 富燃火焰 = 1.2 to 2.3L/min 冷火焰用于 Ru, Mo等元素. Nitrous Oxide/ Acetylene Flame 贫燃火焰 = 3.8 to 4.2 L/min 用于测定 Se. 化学计量火焰 = 4.2 to 4.6 L/min 用于测定 Al, As, Ba, Ca, Cr. 富燃火焰 = 4.6 to 5.0L/min 用于测定 B, Dy, Mo, W. View Height View Height Limits of Flame Sensitivity 试样停留时间 原子的停留时间很短，一般只有 10-5- 10-4 秒, 低于许多原子被激发的时间 Principle of Graphite Furnace Graphite Furnace Advantages 原子化器传输效率 事实上100%的样品都被激发. 停留时间 原子被限制在狭窄的热的石墨管壁中 停留时间一般为 10-3 - 10-2 秒 Graphite Furnace Sensitivity Cuvette Heating 用电加热石墨管（低压大电流） 电压约 10V 电流约 300A 电源 3 kW 加热到 3000°C 升温速率 3000°C/ Second Voltage Control 实际电压与温度的关系 Voltage Control Temperature Control 使用光学反馈系统测量与控制温度 热辐射聚焦到光纤上 用光二极管将其转换为电信号 与设定的电压比较 提供石墨管不同的控制电压 Temperature Control 测量的实际温度 600°C 消除了石墨管损耗的影响 无温度的漂移 加热速率取决于设定的温度 通常最大速率 3000°C/ second 对于许多元素，低温也可获得最好的灵敏度 Cuvette Ideal Material Properties Electrographite Electrographite Electrographite - Problem Pyrolytically Coated Cuvettes Pyrolytically Coated Cuvettes Extended Lifetime Cuvettes Cuvette Design Furnace Programme Furnace Programme-Dry Furnace Progr