分析化学课件：第九章 分析化学中的分离方法.pptVIP

D and E Value versus [I-] for I2 in CCl4-H2O (R =1) lg[I-] 0 -1 -2 -3 -4 -5 -6 lgD -1.1 0.013 0.98 1.68 1.90 1.93 1.94 D 0.079 1.03 9.5 47.9 79.4 85.1 87.1 E 7.7 50.8 90.5 98.0 98.8 98.85 98.85 Extraction of Organic Acid (HA) pH = pKa KD A monoprotic acid with pKa=10-6 HA or A-? Which one is extractable? Relation expression between D and KD? For D=5， R=1，E = 83% for one extraction R=1/3，E = 94% for one extraction R=1，E = 99.5% for three extraction E is improved by subdividing organic solvent into smaller portion. 用同量溶剂多次萃取效果好 ntotal - total amount of analyte n1 - amount of analyte in aqueous phase after one extraction Calculation of E after i Extraction For Better Understanding and Memorizing Example：for I2, mtotal=1mg，Vaq＝10 mL，Vorg＝9mL，D＝85 sample sample Continuous Extraction1 Extracted solute +solvent Continuous Extraction2 Extraction of Metal Ions as Chelates Equilibrium in the Extraction of M as Chelates HL MLn nL- + Mn+ MLn (1) (2) (3) (4) Organic phase Aqueous phase HL H＋ + L- KD(HL) KD(MLn) KH(HL) Solid-Phase Extraction固相萃取--The way to save solvent 1-Conditioning; 2-Retention; 3-Rinse; 4-Elution; Preconcentration of analytes- 103 times ----1000 ml can be extracted and eluted by 1 mL! Separating Ions by Ion-exchange Ion exchange is a process by which ions held on a porous, essentially insoluble solid are exchanged for ions in a solution brought into contact with the solid, often called ion-exchange resins. xRSO3-H+ + Mx+ ? (RSO3-)xMx+ + xH+ xRN(CH3)3+OH- + Ax- ? [RN(CH3)3+]xAx- + xOH- solid soln solid soln Types of Ion Exchange Resins Types of Exchanger Functional Groups Examples Cation Strong acid Weak acid Sulfuric acid Carboxylic acid -SO3-，-CH2CH2SO3- -COO-， -CH2COO- Anion Strong base Weak base Quaternary amine Amine -CH2N(CH3)3+ -CH2CH2N(CH2CH3)3+ NH3H+， -CH2 CH2NH(CH2CH3)2H+ Separation by Chromatograph