chapter1-preface.ppt

1、WELCOME TO INSTRUMENTAL ANALYSIS,(1) Water analysis Ca2+ Mg2+ ?,氨性緩沖液 pH=10 EBT EDTA,NaOH pH=12 Ca Indicator EDTA,Water Quality Standard for Urban Water Control CJT 206-2005 CJT 141 城市供水 SiO2 Silicon molybdenum blue spectrophotometry CJT 142 城市供水 antimony 原子吸收分光光度法 CJT 143 城市供水 Na Mg Ca 離子色譜法 CJT 14

2、4 城市供水 有機(jī)磷農(nóng)藥的測(cè)定 氣相色譜法 CJT 145 城市供水 VOCs CJT 146 城市供水 酚類化合物的測(cè)定 液相色譜法 CJT 147 城市供水 多環(huán)芳烴的測(cè)定 液相色譜法 CJT 148 城市供水 糞性鏈球菌的測(cè)定 CJT 149 城市供水 亞硫酸鹽還原厭氧菌(梭狀芽胞桿菌)孢子的測(cè)定 CJT 150 城市供水 致突變物的測(cè)定 鼠傷寒沙門(mén)氏菌哺乳動(dòng)物微粒體酶試驗(yàn),(2) Food analysis,“Sudan red I”是一種紅色的工業(yè)合成染色劑,溶劑、油、蠟、汽油增色 鞋、地板等的增光,導(dǎo)致鼠類患癌，人類肝細(xì)胞研究中也顯現(xiàn)出可能致癌的特性,2004年6月14日，英國(guó)食品

3、標(biāo)準(zhǔn)管理局就此前在超市一批新食品中發(fā)現(xiàn)含有潛在致癌物的蘇丹紅1號(hào)色素，向消費(fèi)者和貿(mào)易機(jī)構(gòu)發(fā)出了警示，禁用產(chǎn)品目錄中的蘇丹紅1號(hào)。,2005年2月18日，英國(guó)食品標(biāo)準(zhǔn)署就食用含有添加蘇丹紅色素的食品向消費(fèi)者發(fā)出警告，并在其網(wǎng)站上公布了亨氏、聯(lián)合利華等30家企業(yè)生產(chǎn)的可能含有蘇丹紅（一號(hào)）的產(chǎn)品清單。,Past: heavy metals and persistent organochlorine pesticide However, the irrational use of organophosphorous (有機(jī)磷) and carbamate pesticide(氨基甲酸酯農(nóng)藥) 造成不

4、少食用果實(shí)蔬菜者的急性與亞急性中毒。 1).毛細(xì)管氣相色譜法（GC） 2).氣相色譜/質(zhì)譜聯(lián)用法（GC/MS） 3).高效液相色譜法（HPLC） 4).液相色譜/質(zhì)譜聯(lián)用法（LC/MS） 5).氣相色譜/原子發(fā)射聯(lián)用法（GC/AED） 6).酶抑制和免疫檢測(cè)技術(shù)等快速篩選檢測(cè)技術(shù),(3) pesticide residue analysis,室內(nèi)空氣檢測(cè) 土壤質(zhì)量監(jiān)測(cè) 固廢分析 室內(nèi)裝飾裝修材料有害物質(zhì)限量檢測(cè) 大氣質(zhì)量監(jiān)測(cè),(4) Environmental analysis,如何分離?,如何鑒定?,(5) Pharmaceutical Synthesis and analysis,麻醉藥

5、anaesthetic 鎮(zhèn)靜催眠藥、抗癲癇藥和抗精神失常藥sedative-hypnotics 非甾體抗炎藥 non-steroidal anti-inflammatory drugs 鎮(zhèn)痛藥analgesics 中樞興奮藥及利尿藥 抗過(guò)敏、抗?jié)兯?擬腎上腺素藥 擬膽堿藥和抗膽堿藥 心血管系統(tǒng)藥物 抗菌藥和抗病毒藥 抗生素 抗腫瘤藥 甾類藥物 維生素 藥物的化學(xué)結(jié)構(gòu)與藥效的關(guān)系 藥物研究與開(kāi)發(fā)的途徑和方法,島津GC-2010,HP-1100液相色譜儀,上海辰華 CHI660,PAR2273電化學(xué)工作站,Beckman P/ACETM MDQ,FTIR-8400S 島津,UV-vis光譜儀,日

6、立F-4500熒光光譜儀,ICP質(zhì)譜儀,J.W.Robison E.M.S.France G.M.Frame II Undergraduate Instrumental Analysis Six Edition Marcel Dekker,Text BOOKS:,Reference BOOKS:,Instrumental Analysis，Zhu Ming-hua，Higher Education Press(3rd)(Textbook for 21th Century), Beijing, 2001(in Chinese), Modern Analytical Chemistry, Davi

7、d Harvey, McGraw-Hill, Inter. Ed., Singapore, 2000, Contemporary Instrumental Analysis, K.A.Rubinson, J.F. Rubinson, Science Press & Prentice Hall, Inc., Beijing, 2000(影印版）,Instrumental Analysis，Liu Zhiguang，Higher Education Press(3rd)(Textbook for 21th Century), Beijing, 2007(in Chinese),Teaching P

8、urpose,儀器分析是化學(xué)類專業(yè)必修的基礎(chǔ)課之一。 通過(guò)本課程的學(xué)習(xí) 要求學(xué)生掌握: Principle of instrumental analytical methods in common use and simple setup； 要求學(xué)生初步具有 An ability to develop appropriate analytical procedure according to the analytical purpose based on the advantage and application fields of different instrumental analyse

9、s studied.,Chapter 1 PREFACE,Description of Validation Parameters Accuracy Closeness of agreement between the value obtained by the method and the true value.,Precision Expresses the closeness of agreement between a series of measurements obtained from multiple sampling. Precision is often expressed

10、 as the standard deviation or Relative standard deviation of replicate measurements (later on RSD). Note that a method can be precise, but not accurate (so all your measurements may be close together, but the result is wrong).,1.1 Some concepts in analytical chemistry,Specificity The ability to meas

11、ure the analyte in the presence of components which we expect to be present in the sample matrix. So if you are determining the concentration of Iron and Chromium in water by UV/Vis spectroscopy, if there are small amounts of Fluoride and Chloride in the sample, will that affect your measurement?,De

12、tection Limit The lowest amount of analyte in a sample that can be detected, but not necessarily quantitated. Usually the lowest limit is evaluated as the Signal-to-Noise ratio that is equivalent to 3 times the standard deviation of the noise ( S/N = 3s).,Quantitation Limit The lowest amount of anal

13、yte in a sample that can be quantitated with suitable precision and accuracy. Usually the Quantitation limit is evaluated as the Signal-to-Noise ratio that is equivalent to 10 times the standard deviation of the noise ( S/N = 10s).,Continued,Linearity The range of concentrations of analyte for which

14、 the procedure provides test results that are in direct correlation to the amount of analyte in the sample.,Continued,Analysis, Assay, Determination, Measurement, Identification These phrases are usually used to describe one process to determine the concentration of the analytes in a sample,Protocol

15、, operation, method, procedure, measure, technique These phrases means a method to evaluate the concentration of the analytes in a sample,1.2 分析化學(xué)化學(xué)分析、儀器分析,Analytical chemistry A subject to study chemical composition, structure and state of substances including chemical analysis and instrumental ana

16、lysis. Chemical analysis A method to determine chemical composition and content of the analytes in a sample based on chemical reaction and stoichiometric relation of teactants usually requiring chemical reagents, balance and glassware. Instrumental analysis is an analytical method based on determina

17、tion of physical and physical chemical properties which needs some complicated apparatus. 儀器分析的產(chǎn)生為分析化學(xué)帶來(lái)革命性的變化，儀器分析是分析化學(xué)的發(fā)展方向。,Characteristics of Instrumental Analyses（與化學(xué)分析比較）,Higher sensitivity, detection limit down to lower level 如樣品用量由化學(xué)分析的mL、mg級(jí)降低到儀器分析的g、L級(jí)，甚至更低。適合于微量（micro-)、痕量(trace)和超痕量(ultr

18、atrace)成分的測(cè)定。 Higher selectivity 很多的儀器分析方法可以通過(guò)選擇或調(diào)整測(cè)定的條件，使共存的組分測(cè)定時(shí)，相互間不產(chǎn)生干擾。 Simpler operation, faster assay & easy of automation Poorer relative error 化學(xué)分析一般可用于常量和高含量成分分析，準(zhǔn)確度較高，誤差小于千分之幾。多數(shù)儀器分析相對(duì)誤差較大，一般為5%，不適用于常量和高含量成分分析。 More expensive apparatus,常量分析、半微量和微量分析,Mass spectra (Mass/charge ratio),1.3 Classification of instrumental analyses,1.4 Development Tendency,Higher accuracy,