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Vogel's - Textbook of quantitative chemical analysis (5th Edition PDF

906 Pages·2005·6.53 MB·English
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TEXTBOOK OF QUANTITATIVE CHEMICAL ANALYSIS FIFTH EDITION G.HLJEFFERY * J. BASSETT + J.MENDHAM + R.C.DENNEY VOGEL’ TEXTBOOK OF QUANTITATIVE CHEMICAL ANALYSIS purres RBIS Hes the fllsciny veers of the Sehgil uf Cherise ‘Thames Paltechie, Landon GH Jeffery, BSc, PRL. C Chem, FRSC ‘Former Principal Lecurer ad Deputy Head of te School of Chenctrg TBassett, MSc, C-Chem, FRSC Former Senior Lecture 1 Fnorgaaiv Chenisiry ‘J Mendham, MSe, C Chem, MRSC Principal Lecturer in Analstcal Chemisty RCNeoney, BS, PAD, CChem, FRSC, MBIM Prigciogl Tectia i Organke Cheney ener etc So Mrghcscome: np fhe Ce ee ne meatal shonin ence ob F NR, BAT, wo as chef mete ei ay Canine ein De Tecnica SON DeseeNGI-? “Uta of ange Caton Pio Dale Eastham rade eH toe ind SE inicot al geemerne mci a 3. ak CONTENTS PART A FUNDAMENTALS OF QUANTITATIVE CHEMICAL ANALYSIS CHATER 1 INTRODUCTION 11 Chemica! anni 3 ‘Aprlcation, of choca qos 4 3 Sampling 2 ‘ones a analysis & (ae of teranie & ‘Common cechaits. 7 5 trent ethos UX Omer webrigues 9 25. Factors alfectag dhe choice of ara Ei lmeferenoes 1 LLL Daca nequistion and temtmeat 13, Summary 1 CHAPTER 2 FUWDAMENTAL THEORETICAL PRINCIPLES OF REACTIONS IK SOLUTION 21 Cheeal quiibeamn 15 22 The law of maze action 1S 23 Factors afetng ebomical reactions ia solution 18 24 Flectrlytie as 26 at aa as 210 Eifel af tenperaare on 241. Pie af the toon on he LID At-iase eqalts ta water 3 2LIQ Strength of acs and ses. 34 preiliare 28 ofa preipcre 3 214 Disstinin ot poteprovic acids 33 215 Commenion fleet 216 The tage produc! of wate 36 212 the hedeveen on expen — 8 he hsdpa a salle 3D 219 Mydraests consent and degre oF hydeobsis 2 2:0 tater sawtous 6 225 actos aiuceeing the stably of complewes, 8 226 Complevones 2277 Sainte ceomtone of EDTA comphses St ‘rig Pleeteoie potato 218 Concemention cols 63 20 Catealton of he ean. ofa soak eal Gd 2M Ontdaton-reductin cle 292 Cateabaion of the spiard tlocion ptertlal 65 AN Teuiirai coattans of oxidation redetion rears 67 CHAPTER 3 COMMON APPARATUS AND BASIC TECHNIDUES B tavohution 71 BALANCES 122 The aunytoe Baynes 72 Other balaseet TA J Wealght. reference maces, 75 AS Care and une of anayrieal Balances 75 136 Env tn weighing. 6 UGRAMUATED GLASSWARE. BT Unite of eolame 8 38 Gradeated wpoaentos 79 39 Terperature mandir 80 310 Gradeated asks 81 an B12 Raretie R B13 Weir barets_ 36 214 Pistou boretan 47 SUS Gredunted (moturing) «vind 47 [316 Catlaation of soutetric apparacat | 47 \WATFR FOR LABORATORY USE SIT Pare war 49 BIW Wash hotdes at GENERAL APPARATUS 519 Cassar, curamies, poste ware 92 " n n oy 2 320 Meal apparatus 93 321 Heatigg upportus 7 322 Desiecstors urd ry Box, 98 25 Weighing Bottles 103 EAGENTS AND STANDARD SOLUTIONS 108 226 Reageuts 1Dd 227 Pantieation of subatances 105 328 Preparation and storage of standard salons. U7 SOME BASIC TECHAIOUES, 18 ‘329 Preparation ofthe sabstnee for analyte (09 1330 wedging the sample 10 5H Soften of the AR Precision 118 383 Fitrason 115 XM Filter pers 118 38 Couclfes with getmancat porous plates LIT 4 ANB Refomcot for Part A. 122 [339 Solsted biography for Wart 4.122 PART B ERRORS, STATISTICS, AND SAMPLING 15 CHAPTER 4 ERRORS AND STATISTICS iar At Liniatons of anatyical methods 127 ‘12 Clutton of rors 127 43 accuracy 128 44 Preckson 129 3X5 Minimison of eres 191 46 Sienna Noutes 20 conspuratons 132 G7 The ane of callous and mrocempucrs 133 44 Vicurd standard deviation 134 ‘0 Disutbution of random errs 136 4410 Belial of rests 137 LAL Cadence interval {402 Conmparicen of resus, 139 4413 Compacson of the ments of two cumple AM Us aied ston UT 4445 ‘The mumber of replicate determiuacons (42 Aig Crcelaben and regrewion ta IT Taneae reprendon 8 118 Cuenparkon of mote thas ore means (amass of vacianeed 146 419 The ave of eaten GH CHAPTER 5 SAMPLING 0 ‘The basis of sampling 150 Sunpag procoance 150 Sumpbeg sess. ISL Sumpling and physi ste 163 Coushiog and pedi 158 Hzuds ia spliog 155 Referouoee for Pare B 186 Seletel tiogeaphy for War 156 PART C SEPARATIVE TECHNIQUES 189 CHAPTER & SOLVENT EXTRACTION 161 64 General discussion 161 {62 Factors avouring soltent extactioa 263 {63 Quuutiacve treatment of calent extraction equilibria 165 664 Stuergise extraction. 167 ‘85 larcusocition compleves 16% ‘66 Lxtractioncewgemts 169 {65 Som peuial coailernions 172 ‘SOME APPLICATIONS 16 GR Taeterinaion of herslinm a the aceylacetone complex 175 69. Deereigattn of heron alee ferrin 178 G10 Teerotnaion eopper a the dershithnearbarrate stingleg 177 G11 Tetereteation of copper asthe ‘ase-cuprie’ complex 178 ‘612 Deteruination of fru a5 the t-evdronvauiacate 178 ‘613 Deternination of lead by the dithzene method 179 ‘S14 Determination of maybdcaum by the rhigeyamsie method 180 sis ti of eft a he dimiglyocime comple #81 516 a7 eit CHAPTER 7 DN EXCHANGE 6 “24 Goneraldicunsion 186 122 Action af fou exchange fesins 188 13 lon exchange 4 ‘Cheating ou eachage resis 202 17 Vays exchangers 204 APPLICATIONS IN ANALYTIGAL CHENISTRY 0% 118 Expovineucalechniques 208 79. Determination ofthe eapacity of an fon exshange ein (cola method) 207 1240 "Separetion of rine vad magaesiun on an anion exchanger 208 TAL Separation of chloride and brousie on an anion exchnager 209 TAR Deterainaon ofthe tral ction concentration i mater 210 ZS Separetion of adam aud rin an an snibg exchanger 210 TAS Comemmration of copper (2) ous trom a bene solution wsing ‘eating tr exchange roxio 212 34s Duterafoation of anions usiag ion voromatograghy: 213 CHAPTER a COLUMM AWD THIN LAYER LIQUID CHROMATOGRAPHY 216 AL farrofucton 246 RZ Types of Tq cha 83. guipmencfor HPT 4 Deritacsadan 228 MS Qunaritarve analysis 229 86 Thirlavercbromcogeaphs 229 87 Tah performance thi layer cbromtography (HPTLC). 232 Determieation of asprin, phenacetin and eae ina crure 233, ‘chromatography — The ceotey of separated saltacees by ion toehaigues 233 tgeanhy 218 0 CHAPTER 9 GAS CHROMATOGRAPHY 25 5 Tmoduction 295 32 Apparacus 248 93 Prorammed-Tomperacuce gaa chromatagraphy 244 BA Quangtatwo auajuis by GLC. 205 3 Elemental aulyds ocug gas chromatogragly 247 96 Detecuination of aluminium by gas hronalographlessalyis of ies rin actslacetonato) comples 248 97 Analysis of « misture stag the fterual uormatiaton teeta 239 (8 Thetermsation of sueowe a ite imethy tl derivative wing ss Tiynldchroaatogsoghy. 250 99° eforemes for Past © 251 10 Selected bitograly foe Pant €: 253 PART 0 TITRIMETRY AND GRAVIMETRY CHAPTER (0 TITRIMETRIC ANALYSIS THEORETICAL CONSIDERATIONS. (04 Titvimetsc anlgss 287 la of renctions fn Ginkmetee anaes 288 lutions, 250 1.4 Equivalents, normalities and exidaion apmbers 361 1S Preparation of sandard soions 60 We Primary aol sscoodacy stnadide 260 ANBUTAALISATION TITRATIONS 107 Newtrafization indica 262 UNE Pecparation of indicator slecons. 268 US ‘aixed indore 267 100 Usinersal or maulps eunge indicators 268, 1011 ‘Newealfation saves 269 1022 Newtslistion ofa sruny uci wih w stony base, 269, 1043 Newalbution of« weak nod wih strong base” 272 Ad Nevteuiaio of a wenk be with som weed 274 1015 Nevteafeaton af» weak acd widh 2 weak baye 275 1016 Newalkation af a pelsprotie ald with a tong hate 276 LIT “Vitacon of aniooe of weak cide mith 2t0ng aid ‘eplaceniem rations” 277 2018 Choice a indicatrs i neraliation reactions 240 1619 “Tiatons ia eae-aquedus solsens 281 1020 Solvents for aow-agheous teradaos 283 1021 sediaters Yor eonvaqueeustieaions 283 AZZ Preparation ofa standard ac. 28 1025 Preparation uf constant Bling point brdrochore aid 243 1024 Direct peeparsion of 0.194 hydrochloric ci fromm the oust billing point oid. 245 1028 Preparaion of approximately DAM Wydeachloie standardeation 386 (Other srandaedcabetances for acimetry and alkalimecry 203 ‘Standard tartan hydroxide ekrbin 204 Deterniaadon af the Na;CO) content of washing sada. 295 ‘Determination ofthe seth of concentrated acks 296 [Deteemieadon of mixure of earboaute ad hydroxie (Gabel of eomanrcal couse sda) 97 109. Desermoaton of 4 tor of carbone wd Indengencarbte 293 10.24 Betersuuton of bare achd_ 299 su 300 an of erpane niragea (The Riedl procure) M2 A137 Derermnatin of ntaten 303 255 aI mT st uss on as galling 40299 Dever the lave oetseular wae of an organic seit 48 lon Determination of wydeosy] groupe ic carbohydrates 306 1041. Deteemini of a ricore oF ali ad etbuavlene wz ‘tanagucons tigation. 307 naz Deteeminatin of the saponification vale of ols ua fats 308 COWPLEXATION TITRATIONS 08 1043 fetrodncon 309 1044 simple complexation 1443 ‘itatinn cures 310 1046 types of EDIA Seton 311 GAT Traton of mixtuces, sede ages 312 1948 Viel ho indicators 314 (049 Seandatd EDTA solitons 324 ston 308 ty masking and tenahing (9.5) Sune pestis] condbeeahone 322 DETERMINATION OF WOKMDUAL CATIONS oa aust ion of alain: Icleteyton 324 LS2 Delormnton of gear: aleve retfow 322 nga ‘ect deration 424 HL84 Deterniadon of cateou aubeteton theadon 28 {088 Detereniacan of copy: divest Gation 326 10486 Deteaniuaion af rou (TI divest ation 326 ns? joa of wick: dice itrations 327 1038 oa of siberodiact meted. 327 M3 Details for he decrvination ofa sekction of metal im by EDTA dation 328 ANALYSIS OF MIXTURES OF CATIONS sa 1460 Detecninstoa of calcio und magaesuea 324 {Wet Deteroninition af ealeinm ithe prcsence of cn mea 186d Deteetnaton of calcu i the presence of sium wig DIA ss throm 335 thet on of caleinm and Td fam mites 3b 65. Determination of magne, maine i 8 tnisfore: use of fhe fon tsa detaching agent 3M 1066 Deteraication of elvoninea(UIL) aod ont TM) faa wixare an example of kinerie masking. 35 1067 Deterrisaion of manganest te prescac of cea: seals of ferro-miagansee 236 1068 Determination of eickel ia presen of ron: unas of aiche sed 136

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