Macro and semimicro qualitative inorganic analysis 5ed vogel

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VOGEL'S TEXTBOOK OF MACROAND SEMIMICRO QUAUTATIVE INORGANIC ANALYSIS FIFTH EOmON Revised by G.SVEHLA VOGEL'S TEXTBOOK OF MACRO AND SEMIMICRO QUALITATIVE INORGANIC ANALYSIS Fifth Edition Revised by G Svehla, Ph.D., D.Se., F.R.I.e Reader in Analytical Chemistry, Queen's University, Belfast ~ ~ Longman London and New York Longman Group Limited London Associated companies, branches and representatives throughout the world Published in the United States of America by Longman Inc., New York © Longman Group Limited 1979 All rights reserved No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, or otherwise, without the prior permission of the Copyright owner First Published under the title 'A Text-book of Qualitative Chemical Analysis' 1937 Second Edition 1941 Reissue with Appendix 1943 Third Edition under the title 'A Text-book of Qualitative Chemical Analysis including Semimiero Qualitative Analysis' 1945 Fourth Edition under the title 'A Text-book of Macro and Semimicro Qualitative Inorganic Analysis' 1954 New Impression (with minor corrections) 1955 New Impression 1976 Fifth edition 1979 Library of Congress Cataloging in Publication Data Vogel, Arthur I Vogel's Macro and semimicro qualitative inorganic analysis First-3d ed published under title: A text-book of qualitative chemical analysis; 4th ed published under title: A text-book of macro and semimicro qualitative inorganic analysis Includes index Chemistry, Analytic-Qualitative Chemistry, Inorganic I Svehla, G 11 Title Ill Title: Macro and semimicro qualitative inorganic analysis QD81.V6 1978 544 77-8290 ISBN 0-582-44367-9 Printed in Great Britain by Richard Clay (The Chaucer Press) Ltd, Bungay, Suffolk iv CONTENTS CHAPTER I THE THEORETICAL BASIS OF QUALITATIVE ANALYSIS A Chemical formulae and equations 1.1 Symbols of elements 1.2 Empirical formulae 1.3 Valency and oxidation number 1.4 Structural formulae 1.5 Chemical equations B Aqueous solutions of inorganic substances 1.6 Electrolytes and non-electrolytes I Electrolysis, the nature of electrolytic conductance, ions 1.8 Some properties of aqueous solutions 1.9 The theory of electrolytic dissociation 1.10 Degree of dissociation Strong and weak electrolytes 1.11 The independent migration of ions Calculation of conductivities from ionic mobilities Modem theory of strong electrolytes 1.12 1.13 Chemical equilibrium; the law of mass action 1.14 Activity and activity coefficients 1 6 9 11 15 17 19 22 C Classical theory of acid-base reactions 1.15 Acids, bases, and salts 1.16 Acid-base dissociation equilibria Strength of acids and bases 1.17 Experimental determination of the dissociation equilibrium constant Ostwald's dilution law 1.18 The dissociation and ionic product of water 1.19 The hydrogen-ion exponent (PH) 1.20 Hydrolysis 1.21 Buffer solutions 1.22 The experimental determination of pH 25 25 28 D The Brensted-Lowry theory of acids and bases 1.23 Definition of acids and bases 61 61 v 33 35 36 39 48 53 1.24 1.25 Protolysis of acids Strength of acids and bases Interpretation of other acid-base reactions with the Brensted-Lowry theory 64 E Precipitation reactions 1.26 Solubility of precipitates 1.27 Solubility product 1.28 Applications of the solubility product relation 1.29 Morphological structure and purity of precipitates 1.30 The colloidal state 67 67 68 75 83 85 F Complexation reactions 1.31 The formation of complexes 1.32 The stability of complexes 1.33 The application of complexes in qualitative inorganic analysis 1.34 The most important types of complexes applied in qualitative analysis 89 89 92 96 66 97 G Oxidation-reduction reactions 100 1.35 Oxidation and reduction 100 101 1.36 Redox systems (half-cells) 1.37 Balancing oxidation-reduction equations 104 1.38 Important oxidizing and reducing agents 108 1.39 Redox reactions in galvanic cells 112 1.40 Electrode potentials 115 1.41 Oxidation-reduction potentials 119 1.42 Calculations based on the Nernst equation 124 1.43 Conclusions drawn from the tables of oxidation-reduction potentials126 1.44 Equilibrium constant of oxidation-reduction reactions 128 H Solvent extraction 1.45 The distribution or partition law 1.46 The application of solvent extraction in qualitative analysis 130 130 131 CHAPTER 11 EXPERIMENTAL TECHNIQUES OF QUALITATIVE INORGANIC ANALYSIS 135 11.1 11.2 11.3 11.4 11.5 11.6 135 136 145 153 173 180 Introduction Dry reactions Wet reactions Semimicro apparatus and semimicro analytical operations Micro apparatus and microanalytical operations Spot test analysis CHAPTER III REACTIONS OF THE CATIONS 191 IIU III.2 191 192 Classification of cations (metal ions) into analytical groups Notes on the study of the reactions of ions vi 111.3 IlIA III.5 III.6 III.7 III.8 III.9 Ill 10 Ill 11 Ill 12 III.13 Ill 14 IIU5 Ill 16 III.17 IIU8 Ill 19 III.20 111.21 III.22 III.23 III.24 1II.25 III.26 III.27 III.28 III.29 Ill 30 III.31 III.32 III.33 III.34 111.35 III.36 III.37 111.38 First group of cations: lead(II), mercury(l) and silver(l) Lead, Pb (A r : 207'2) Mercury, Hg (A r : 200'59) - Mercury(l) Silver, Ag (A r : 107'9) Second group of cations: mercury(II), lead(II), bismuth(III), copper(II), cadmium(II), arsenic(III) and (V), antimony(III) and (V), tin(lI) and (IV) Mercury, Hg (A r : 200'59) - Mercury(lI) Bismuth, Bi (A r : 208'98) Copper, Cu (A r : 63'55) Cadmium, Cd (A r : 112'90) Arsenic, As (A r : 74'92) - Arsenic(III) Arsenic, As (A r : 74'92) - Arsenic(V) Special tests for small amounts of arsenic Antimony, Sb (A r : 121'75) - Antimony(III) Antimony, Sb (A r : 121'75) - Antimony(V) Special tests for small amounts of antimony Tin, Sn (A r : 118'69) - Tin(lI) Tin, Sn (A r : 118'69) - Tin(IV) Third group of cations: iron(lI) and (Ill), aluminium, chromium(III), nickel, cobalt, manganese(lI) and zinc Iron, Fe (A r : 55'85) - Iron(ll) Iron, Fe (A r : 55'85) - Iron(III) Aluminium, Al (A r : 26'98) Chromium, Cr (A r : 51'996) - Chromium(III) Oxianions of group III metals: chromate and permanganate Cobalt, Co (A r : 58'93) Nickel, Ni (A r : 58.71) Manganese, Mn (A r : 54'938) - Manganese(lI) Zinc, Zn (A r : 63'58) Fourth group of cations: barium, strontium, and calcium Barium, Ba (A r : 137'34) Strontium, Sr (A r : 87'62) Calcium, Ca (A r : 40'08) Fifth group of cations: magnesium, sodium, potassium, and ammonium Magnesium, Mg (A r : 24' 305) Potassium, K (A r : 39'098) Sodium, Na (A r : 22'99) Ammonium, NH (M r : 18'038) 193 194 199 204 208 209 212 215 221 223 225 228 231 234 236 237 240 241 241 245 250 254 259 259 264 268 272 277 278 281 282 285 285 289 291 293 CHAPTER IV REACTIONS OF THE ANIONS 297 IV.l IV.2 IV.3 297 298 300 Scheme of classification Carbonates, CO~Hydrogen carbonates, HC0 vii IV.4 IV.5 IV.6 IV.7 IV.8 IV.9 IV.lO IV.ll IV.12 IV.13 IV.14 IV.15 IV.16 IV.17 IV.18 IV.19 IV.20 IV.21 IV.22 IV.23 IV.24 IV.25 IV.26 IV.27 IV.28 IV.29 IV.30 IV.31 IV.32 IV.33 IV.34 IV.35 IV.36 IV.37 IV.38 IV.39 IV.4O IV.41 IV.42 IV.43 IV.44 IV.45 Sulphites, SO~Thiosulphates, S20~Sulphides, S2Nitrites, N0 Cyanides, CNCyanates, CNOThiocyanates, SCNHexacyanoferrate(II) ions, [Fe(CN)6]4Hexacyanoferrate(III) ions, [Fe(CN)6]3Hypochlorites, OCIChlorides, ClBromides, BrIodides, 1Fluorides, FNitrates, N0 Chlorates, CI0 Bromates, Br0 Iodates, 10 Perchlorates, CIO; Borates, BO~-, B40~-, B0 Sulphates, soiPeroxodisulphates, S20~­ Silicates, SiO~Hexafluorosilicates (silicofluorides), [SiF6]2Orthophosphates, PO~Pyrophosphates, P20~-, and metaphosphates, P0 Phosphites, HPO~Hypophosphites, H 2P0 Arsenites, AsO~ -, and arsenates, AsO~­ Chromates, CrOi-, and dichromates, Cr20~­ Permanganates, MnO; Acetates, CH 3COOFormates, HCOOOxalates, (COO)~Tartrates, C4H40~Citrates, C6HsO~Salicylates, C 6H4(OH)COO- or C 7H s0 Benzoates, C 6HsCOO- or C 7H s0 Succinates, C 4H 40iHydrogen peroxide, H 202 Dithionites, S20iSpecial tests for mixtures of anions viii 301 305 308 310 313 316 317 319 322 323 325 327 329 332 334 337 339 340 342 343 346 349 350 353 354 358 358 360 361 361 364 366 368 369 371 374 376 377 378 379 382 383 CHAPTER V SYSTEMATIC QUALITATIVE INORGANIC ANALYSIS V.l V.2 V.3 VA V.5 V.6 V.7 V.8 V.9 V.IO V.11 V.l2 V.13 V.l4 V.15 V.16 V.17 V.18 V.19 Introduction Preliminary tests on non-metallic solid samples Preliminary tests on metal samples Preliminary tests on liquid samples (samples in solution) Preliminary tests on insoluble substances Dissolution of the sample Examination of the insoluble residue Separation of cations into groups Separation and identification of the Group I cations (silver group) Separation of Group 11 cations into Groups IIA and lIB Separation and identification of Group IIA cations Separation and identification of Group lIB cations Removal of interfering ions before the precipitation of the Group III cations Separation and identification of Group IlIA cations Separation and identification of Group IIIB cations Separation and identification of Group IV cations Identification of Group V cations Preliminary tests for and separation of certain anions Confirmatory tests for anions CHAPTER VI SEMIMICRO QUALITATIVE INORGANIC ANALYSIS VI.l VI.2 VU VIA VI.5 VI.6 VI.7 VI.8 VI.9 VI 10 VI.ll VI.l2 Introduction The study of reactions of cations and anions on the semimicro scale Systematic analysis on the semimicro scale General considerations Preliminary tests on the semimicro scale Testing for anions in solution on the semimicro scale Confirmatory tests for anions on the semimicro scale Special tests for mixtures of anions on the semimicro scale Preparation of solution for cation testing on the semimicro scale Separation of cations into groups on the semimicro scale Separation and identification of Group I cations on the semimicro scale Separation of Groups IIA and lIB and separation and identification of Group IIA cations on the semimicro scale Separation and identification of Group lIB cations on the semimicro scale ix 395 395 395 405 406 407 411 411 413 420 421 424 428 431 436 437 441 444 446 458 461 461 461 463 464 470 473 476 479 480 485 485 487 VI.l3 VI.l4 VI.l5 VI.l6 VI.17 VI.l8 VI.l9 VI.20 Separation and identification of Group IlIA cations on the semimicro scale Separation and identification of Group IIIB cations on the semimicro scale Separation and identification of Group IV cations on the semimicro scale Identification of Group V cations on the semimicro scale Modifications of separation procedures in the presence of interfering anions Separations by paper and thin layer chromatography General introduction Apparatus and technique for chromatographic separations Procedures for selected chromatographic separations 488 489 490 492 493 495 497 500 CHAPTER VII REACTIONS OF SOME LESS COMMON IONS 507 VII.l VII.2 VII.3 VII.4 VII.5 507 507 509 509 VII.6 VII.7 VII.8 VII.9 VII 10 VII 11 VII.12 VII.13 VII.14 VII.15 VII 16 VII.17 VII.18 VII.19 VII.20 VII.21 VII.22 VII.23 VII.24 VII.25 Introduction Thallium, Tl (A r : 204·34) - Thallium(l) Thallium, Tl (A r : 204·34) - Thallium(III) Tungsten, W (A r : 183·85) - Tungstate Separation and identification of Group I cations in the presence of thallium and tungsten Molybdenum, Mo (A r : 95·94) - Molybdate Gold, Au (A r : 196·97)- Gold(III) Platinum, Pt (A r : 195·09) Palladium, Pd (A r : 106·4) Selenium, Se (A r : 78·96) - Selenites, SeO~Selenium, Se (A r : 78·96) - Selenates, SeOiTellurium, Te (A r : 127·60) - Tellurites, TeO~Tellurium, Te (A r : 127·60) - Tellurates, TeOiSeparation and identification of Group 11 cations in the presence of molybdenum, gold, platinum, palladium, selenium, and tellurium Vanadium, V (A r : 50·94) - Vanadate Beryllium, Be (A r : 9·01) Titanium, Ti (A r : 47·90) - Titanium(lV) Zirconium, Zr (A r : 91·22) Uranium, U (A r : 238·03) Thorium, Th (A r : 232·04) Cerium, Ce (A r : 140·12)- Cerium(III) Cerium, Ce (A r : 140·'12) - Cerium(lV) Separation of Group III cations in the presence of titanium, zirconium, thorium, uranium, cerium, vanadium, thallium, and molybdenum Lithium, Li (A r : 6·94) The borax bead test in the presence of less common cations x 511 511 514 516 518 520 521 522 523 524 527 530 532 535 538 540 541 542 544 546 548 CHAPTER VIII AN ABBREVIATED COURSE OF QUALITATIVE INORGANIC ANALYSIS VIII Introduction VIII.2 Reactions of cations and anions VIII Systematic analysis General considerations VIllA VIII.5 VIII.6 VIII.7 VIII VIII Preliminary tests on solutions Testing for anions in solution Confirmatory tests for anions Special tests for mixtures of anions Separation and identification of cations in solution Modifications in the presence of anions of organic acids, fluoride, and phosphate 550 550 550 551 552 553 556 557 560 564 IX APPENDIX 566 IX.l IX.2 IX.3 IXA IX.5 IX.6 IX.7 IX.8 568 589 592 593 595 597 598 Relative atomic masses of the elements Reagent solutions and gases Solid reagents Solubilities of salts and bases in water at 18°C Logarithms Antilogarithms Concentrated acids and bases Periodic table of the elements INDEX 566 599 xi VI 10 IV IX.4 SOLUBILITIES OF SALTS AND BASES IN WATER AT lSOC* Cl Br I F N0 CI0 Br0 10 80 e-o, (COOh C0 OH K Na Li Mg 32-95 65-86 137'5 92'56 30'34 6·6 6'38 7-62 11·11 63-1 30'27 108'0 142-9 35-86 88'76 177-9 4'44 83'97 97'16 36-67 8'33 16·83 61'21 3-34 19'39 116·4 77-79 168'7 161·5 0'27 71'43 313'4 152'5 80'43 35-64 111·6 7-22 1·3 12'04 55-81 103·1 148·2 0·0076 74·31 126'4 42-86 6·87 35-43 73-0 0·03 0·1 0·001 Ba 37-24 103'6 201'4 0'16 8'74 35-42 0'8 0·05 2'3 x 10- 3·8 x 10- 0'0086 0'0023 3'7 8r 51'09 96'52 169'2 0'012 66'27 174'9 30'0 0'25 0'011 0'12 0·0046 0'0011 0'77 * The solubilities are expressed in grams of anhydrous salt dissolved by lOO ml of water Ca 73'19 143-3 200'0 0'0016 121·8 179·3 85'17 0'25 0'20 0'4 5·6 x 10- 0'0013 0'17 Zn 203'9 478'2 419'0 0'005 117-8 183'9 58-43 0·83 53'12 7·9 X 10- 0·0005 Pb Ag 1'49 0'97 0'08 0'06 51'66 150'6 1'3 0·002 0·0041 x 10- 0·0001 0·0001 0'01 1'4x 10- I x 10- 3'0 x 10- 195-4 213'4 12'25 0'59 0'004 0'55 0'0025 0'0035 0'003 0'002 (?) E I:> c:: > r- ~ o-l Z o > Z > r- -< VI 10 -.I VI 10 00 IX.8 PERIODIC TABLE OF THE ELEMENTS The relative atomic masses have been rounded off to a maximum of significant figures An alphabetical list of the elements with precise relative atomis masses and their logarithms is to be found in Section IX.t I:> He H 1·008 Li 11 Be Na K 39'10 37 21 22 23 24 Ca Se Ti V 40·08 38 44·% 39 47-90 40 50·94 41 Rb Sr 85-47 55 87-62 56 Y 88·91 57 C N F Ne 12·01 14 14·01 16·00 16 19'00 20·18 AI Si S a 28·09 32 30·97 33 32·06 34 35-45 35 Zn Ga Ge As Se Br 63'55 65-38 47 48 69·72 49 72'59 74'92 51 50 78'96 52 79·90 53 Rh 102-9 77 Ta W Re Os Ir Pt Au Hg rt Pb Bi Po At Rn 180·5 183-9 186'2 190·2 192·22 195'1 197·0 200'6 204-4 207·2 209'0 (209) (210) (222) Hf r - 58 59 Pr Ce 140·1 90 14O'~ 91 75 61 60 62 63 64 Cd In UN1 80 114·8 65 81 66 So Sb 118'7 82 121·8 83 67 68 Te I Xe 127·6 126·9 13B 84 69 85 70 86 71 Eu Gd Tb Dy Ho Er Tm Yb Lu 150·4 94 152·0 95 157-3 % 158'9 162'5 98 164'9 99 167·2 100 168·9 101 173·0 102 175·0 103 Pm Srn 144'2 145 92 93 Nd Ag 97 Tb Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr 232·0 231·0 238·0 237'0 (244) (243) (247) (247) (251) (254) (257) (258) (259 (260) Table for Appendix IX.8 ~:::c ~ ~ !- Ru 107-9 79 tTl 83-80 54 IOH 76 Pd < o (97) 106·4 78 ~ E Kr Tc 178·5 Ae 58·71 46 Cu 36 Mo La 227·03 55·85 5893 44 45 Ni 30 95·94 74 138·9 226·0 Co 29 Ar 39·94 Nb Ba (223) 28 P 18 92'91 73 137-3 88 89 Fe Mo 52'00 54-94 42 43 27 17 Zr Cs Ra 26 15 91·22 72 132·9 87 Fr Cr 25 4·003 10 26·98 31 Mg 24·31 20 B 10·81 13 9'012 12 22-99 19 l;:! Qc en INDEX Abbreviations: AC: in abbreviated course CHR: chromatographic, or by chromatography CT: confirmatory test for D: detection of I: idendification of ip : in the presence of MS: on micro scale PT: preliminary test for R: reactions of S: separation of SM: on semimicro scale T: tabulation, or table of acetate ion CT, 460; SM, 476 D ip, organic acids, 392 R,366 acid, 26, 61 concentrated T, 597 dibasic,29 dilution of, 597 monobasic, 26 polybasic, 26 protolysis of, 64 strong, 26, 65 tribasic, 29 weak, 26, 65 acid base reaction Bronsted-Lowry theory of, 25 classical theory of, 61 acid base system conjugate, 62 corresponding, 62 activity, 22 activity coefficient, 22 T,24 adsorption, 85 alkali metals, S CHR, 503 alkaline earth metals, S CHR, 503 aluminium(III) ion R,250 S CHR, from Be, 504 ammonium ion PT, 400; SM, 466 R,293 ammonium sulphide test, 410 ampholyte, 63 anion(s) classification of, 297 CT, 485; AC, 556; SM, 473 PT, 446; AC, 553; SM, 470 R, 297; AC, 551; SM, 460 S, with AgN0 , 451, 453; SM, 471 S CHR, 504 anti-bumping device, 151 antilogarithm T, 595 antimonate, see antimony(V) antimonite, see antimony(III) antimony(III) ion, R, 231 antimony(V) ion, R, 234 antimony, special tests for, 236 apparatus, cleaning of, 152 MS, 177; SM, 169 appearance test, 395, 408 arsenate ion CT, 460; SM, 475 D ip, AsO~- and POl-, 388; AC, 559; SM,478 PT, 449 R,225 arsenic(III) ion, R, 223 see also arsenite ion arsenic(V) ion, see arsenate ion arsenic, special tests for, 228 arsenite ion CT, 460; SM,475 D ip, Asol- and pol-, 388; SM, 478 see also arsenic(III) ion asymmetry effect, 19 599 atomic mass, relative T, 556 atomic weight, see atomic mass, relative autoprotolysis, 64 barium carbonate, solubility of, 82 barium(lI) ion, R, 278 base, 27, 61 concentrated, T, 597 dilution of, 597 strong, 27 weak, 27 beaker, 146 benzene ring, benzoate ion CT,460 D ip organic acids, 392 R,377 beryllium(lI) ion R,530 S from A, CHR, 504 bismuth(I1I) ion, R, 212 blowpipe test, 136 boiling point, elevation of, borate ion CT, 459; SM, 476 Dip, Ba2+ and Cu2+, 389 PT, 404 R,343 borax-bead test, 142, 399 SM,466 ip less common ions, 548 bromate ion CT,459 R,339 bromide ion CT, 458; SM,474 Dip, CI-, 1-, 386 Dip, CI-, r, SCN-, SM,477 Dip, r, AC, 558; SM, 477 R,327 bromine, removal of, by solvent extraction, 131 Brownian motion, 87 Bronsted-Lowry theory, 61 buffer solution, 48, 61 Bunsen flame, 138 cadmium(lI) ion, R, 221 calcium chloride test, 454 SM,472 calcium(II) ion, R, 282 calomel electrode, 59 capillary dropper, 155 carbonate ion CT, 459; SM, 475 D ip, SO~-, 383; AC, 557; SM, 476 R,298 cation(s) classification of, 192 Group 1,193 Sand t 420; SM, 485 600 S and lip TI and W, 511 S CHR, 500 Group 11, 208 S into groups IIA and liB with (NH 4hS, 421 with KOH, 423 SM,485 Sand lip, Au, Pt, Pd, Se, Te, 524 Group IIA Sand I by H 2S04 method, 424 by NaOH method, 426; SM, 486 SCHR,501 Group liB S andl by (NH ) 2S2 method, 428 by KOH method, 436 SM,489 SCHR,502 Group Ill, 241 Sand lip, Ti, Zr, Th, D, ce, V, TI and Mo, 544 Group IlIA, Sand t 436: SM, 488; ,cHR, 502 Group IIIB Sand I by HCI-H 20 method, 437 by HCI-KCI0 3-H 202,method, 439 SM,489 S CHR, 502 Group IV, 277 Sand I by SOi - method, 442 by NO; method, 443 SM,490 S CHR, 503 Group V, 285 I cations 444; SM, 492 Sand I CHR, 503 R, 191; AC, 550; SM, 461 S ip interfering ions SM, 493 S into groups, 413; AC, 560; SM, 480 central atom, 89 central ion, 89 centrifugate, transferring of MS, 175 centrifuge, 157 theory of, 157 tube, 154 MS, 174 cerium(I1I) ion, R, 541 cerium(IV) ion, R, 542 charcoal block reduction, 399 SM,465 chelate, 89 chemical equation, chlorate ion CT, 459; SM, 475 Dip, CI-, CIOi, 386 R,337 chloride ion CT, 458; SM, 474 D jp, Br-, 385; AC, 558; SM, 477 ip, sr ' r, 384; AC, 558; SM, 477 ip, Br-, r, SCN-, SM, 477 ip, CIO;, CIO;, 386 ip, CN-, 391 jp, 1-, 386; AC, 558; SM, 477 R,325 chromate ion CT, 459; SM, 475 PT, 457 R,361 chromatography, 497 chromium(III) ion, R, 254 citrate ion CT,46O D jp, organic acids, 392 R,374 cleaning, see apparatus, cleaning of coagel,87 coagulation, 86 value, 88 cobalt(II) ion, R, 259 colloid lyophilic, 87 lyophobic, 87 protective, 88 solution, 86 colloidal state, 85 complexation reactions, 89 complex(es) ammine-,98 aquo-,97 charge of, 91 chelate-, 99 cyanide-, 99 formation of, 89 halide-,99 hydroxo-, 98 instability constants of, T, 93 masking with, 97 nomenclature of, 89 specific tests with, 96 sta bility of, 92 thiocyanate-, 99 composition, percentage, concentration limit, 181 conductance, 13 ratio, 19 specific, 13 conductivity, 13 coefficient, 19 molar, I T, 13 conical flask, 146 coordination number, 89 copper(II) ion, R, 215 coprecipitation, 85 crystal growth, rate of, 84 cyanate ion CT,46O R,316 D D D D D cyanide ion CT, 459; SM, 476 D ip, CI-, 391 PT, 449, 456 R,313 Daniell-cell, 7,115 dative bond, 90 Debye-Hiickel-Onsager theory, 18 decantation, 149 dialysis, 86 dichromate ion, R, 361 digestion, 182 dilution law, see Ostwald's dilution law dipole, 18 direct vision spectroscope, 140 disperse system, 86 displacement reactions, 66 dissociation degree of, 11 electrolytic, equilibrum constant, 28 T,31 dissolution of samples, 411 distillation, MS, 189 distribution law, 130 dithionite ion, R, 382 dropper, 154 drop-reaction paper, 170 dry reactions, 136 electrical double layer, 116 electrochemical series, 118 electrode chlorine-, 123 calomel-, 59 g1ass-,58 hydrogen-, 122 oxygen-, 123 standard hydrogen-, 117 standard reference-, 117 electrode potential, 115 absolute, 116 standard, 116 T, 118, 121, 122 of combined redox and acid-base systems, 120 of gas electrodes, 122 of inhomogeneous redox systems, 121 of metal electrodes, 120 of simple redox systems, 120 electrolysis, electrolyte, strong, 11 theory of, 17 weak, 11 electrolytic dissociation, see dissociation, electrolytic electromotive force (e.m.f.), 114 electrophoretic effect, 18 Emich filter stick, 187 equilibrium, chemical, 19 601 equilibrium constant, 20, 128 Erlenmeyer flask, 146 evaporation, 151 SM,I64 Faraday's nomenclature, ferric, see iron(III) ferricyanide, see hexacyanoferrate(III) ferrocyanide, see hexacyanoferrate(II) ferrous, see iron(II) filter pipette, 186 filtration, 148 filtration aids, 149 flame spectra, 139 T, 142 flame test, 137, 397, 409 SM,465 Fleitmann's test, 231 flocculation, 86 fluoride ion CT, 459; SM, 474 D ip, [SiF612 - , soi-, 390 PT, 449, 455 R,332 formate ion, CT,46O D ip organic acids, 392 R,368 formula empirical, I structural, fractional precipitation, 82 freezing point, depression of, funnel Buchner, 1,0 Jena,150 sintered glass, 150 fusion, MS, 188 gamma, 180 gas(es) I MS, 179; SM, 168 volume of, gas reactions, 188 glass electrode, 58 gold(III) ion R,514 S CHR, from Pt-metals, 505 Gutzeit's test, 229 hafnium, S CHR from Zr, 506 halide(s), S CHR, 503 half cell, 113 heating in steam, 188 heating, MS, 171; SM, 162 heating test, I 36, 396, 408 SM,464 hexachloroplatinate(lV) ion, R, 516 hexacyanoferrate(II) ion CT,46O D ip, [Fe(CN)613 -, SCN-, 392 602 R,319 hexacyanoferrate(III) ion CT,46O D ip, [Fe(CN)614 - and SCN-, 392 R,322 hexafluorosilicate ion CT,459 D jp, F- and soi-, 390 R,353 hydrogen carbonate ion, R, 300 hydrogen ion exponent, 36 hydrogen peroxide, R, 379 hydrogen scale, 117 hydrogen sulphide, precipitation with, 147 MS, 177; SM, 166 hydroiodic acid test, 410 hydrolysis, 39, 67, 133 constant, 40 degree of, 41 hypochlorite ion CT, 459; SM, 475 R,323 hypophosphite ion CT,46O R,36O impregnated reagent paper, 184 impregnation, 185 indicator(s), colour changes of, T, 54 indicator electrode, 57 insoluble residue, 411 insoluble substances, PT, 407 interfering ions, removal of, 431 AC, 564; SM, 493 interionic attraction theory, 18 iodate ion CT,459 Dip, 1-, 387 PT, 457 R,34O iodide ion CT, 459; SM, 474 D ip, Br - , Cl -, 386 D ip, Br-, AC, 558; SM, 477 D ip, Br-, Cl -, SCN-, SM, 477 D ip, 10;, 387 R,329 iodine, removal of, 131 ion(s) hydrated, 18 independent migration of, 15 ionic strength, 23 ionisation constant, 65 iron(III) chloride test, 454 SM,473 iron(II) ion, R, 241 iron(III) ion, R, 245 lead(II) ion, R, 194 lead salt(s), removal of, 412 levelling effect, 65 less common ions, R, 507 ligand field theory, 90 limit of identification, 180 Iithium(I) R,546 S, from alkali metals, 548 logarithm, T, 593 Lovibond comparator, 56 macro scale, 135 magnesium(I1) ion, R, 285 manganese(I1) ion, 268 Marsh test, 228 mass action, law of, 19 medicine dropper, 155 mercury(I) ion, R, 199 mercury(I1) ion R,209 S, CHR from metals, 504 metaborate, see borate metal hydroxide(s), precipitation of, 79 metaphosphate ion, R, 358 metavanadate, see vanadate micro apparatus, 173 micro scale, 135 microanalytical operations, 173 microcosmic salt bead test, 144, 409 mobility, ionic, 16 T, 16 molybdate ion, R, 511 Nernst-equation, 116, 124 neutralisation, 27, 66 nickel(I1) ion, R, 264 nitrate ion CT, 459; SM, 474 D ip, Br-, r, 384; AC, 558; SM, 476 D ip, CIO;, 384; AC, 558; SM, 477 D jp, NO l , 383; AC, 557; SM, 476 PT, 403; SM, 467 R,324 nitrate ion CT, 459; SM, 474 PT, 403; SM, 467 R,310 non-electrolyte, nucleation, rate of, 84 occlusion, 85 organic acids, S, 393 orthoborate, see borate orthophosphate ion, R, 354 see also phosphate Ostwald's dilution law, 34 oxalate ion CT, 460; SM, 476 D ip, F-, 391 D ip, organic acids, 392 R,369 oxoanions, of group III metals, 259 oxidation, 11, 100 number, -reduction equation, 104 potential, 119 reaction, 100 oxidizing agent(s), 108 PT, 449; SM, 471 flame, 136 palladium(I1) ion, R, 518 paper chromatography, 495 partition coefficient, I 30 law, 130 peptization,87 perchlorate ion CT,459 Dip, CI-, CIO;, 386 R,342 periodate ion, PT, 457 periodic table, T, 598 permanganate ion CT,46O R,364 peroxodisulphate ion CT,459 R,349 persulphate, see peroxodisulphate pH, 36 determination of, 53 -rneter, 60 phosphate bead, see microcosmic salt bead phosphate ion CT, 460; SM, 476 D jp, Asol-, 387 D ip, Asol- and AsO~-, 388; AC, 559; SM,478 PT, 449 R,354 removal of, 432, 433, 435; AC, 564; SM,494 phosphite ion CT,46O R,358 platinum(IV), see hexachloroplatinate(IV) platinum electrode bright, 119 platinised, 117 metal/s), S CHR, 504 wire loop, 181 post-precipitation, 85 potassium(I) ion, R, 289 precipitate ageing of, 85 digestion of, 85 dissolution of, SM, 166 drying of, 152 purity of, 83 removal of, 149 603 ripening of, 85 structure of, 83 transfer of, MS, 176; SM, 161 washing of, 149; MS, 175; SM, 161 precipitation, MS, 174 reaction(s), 67 preliminary test AC, 552; SM, 464 on liquid samples, 406 on metal samples, 405 on non-metallic solids, 395 on solutions, 406 protolytic reaction(s), 63 pyroborate, see borate pyrochromate, see dichromate pyrophosphate ion, R, 358 rare earth(s), S CHR from Se, Th, 505 reagent dropper, 154 gas(es), preparation of, 568 solution(s), preparation of, 568 volume, calculation of, 170 reagent(s), solid, 589 redox half cell, 100 redox reaction(s), 100 in galvanic cell(s), 112 system(s), 100 reducing agent(s), 110 PT, 449; SM, 470 flame, 136 reduction, 100 reference electrode, 57 Reinisch's test, 231 relaxation effect, 19 time of, 18 resistance, 12 specific, 12 resistivity, 12 salicylate ion CT,46O D ip organic acids, 392 R,376 salt, 27 effect, 72 salting-out, 88 scandium(III) ion, S CHR from Th and rare earths, 505 selenate ion, R, 521 selenite ion, R, 520 selenium, S CHR from Te, 505 semimicro apparatus, 153 check list, 172 604 boiling tu be, 154 operations, 153 reagent bottle, 155 scale, 135 test tube, 154 work, practical hints for, 171 sensitivity, 181 separation of cations, see cation(s) silicate ion CT,459 PT, 455 R,350 silicide(s), fusion of, 412 silicofluoride, see hexafluorosilicate silver(I) ion, R, 204 silver halide(s), PT, 449 silver nitrate test, 449; SM,471 silver salt(s), removal of, 412 soda extract, 447, SM, 470 sodium carbonate bead, 145 fusion with, 412 + KN0 test, 409 on charcoal test, 408 sodium hydroxide test, 409 sodium(I) ion, R, 291 sol, 87 hydrophilic, 87 hydrophobic, 87 solvent extraction, 130 solvent(s) for chromatography, 499 solubility, 67 T, 592 product, 68, 75 T, 70 spectroscope, 139 spot plate, 170, 183 spot test(s), 180 stirring rod, 146, 154 strontium(II) ion, R, 281 succinate ion CT,46O D ip organic acids, 392 R,378 sulphate ion CT, 45; SM, 475 Dip, F-, [SiF l - , 390 Dip, S2-, SO~-, S20~-, 388 PT, 449; SM, 470 R,346 sulphide ion CT, 459; SM, 474 Dip, SOi-, SO~-, S20~-, 388 Dip, SO~-, S20~-, 389 precipitation of, 76 R,308 sulphite ion CT, 459; SM, 474 Dip, SOi-, S2-, S20~-, 388 Dip, S2-, S20~-, 389 R,301 sulphuric acid concentrated, test with, 402, 409 SM,468 dilute, test with, 40 I, 402 SM,468 supersaturation, 84 symbol(s) of e1ement(s), I tartrate ion CT,46O D ip organic acids, 392 R,371 tellurate ion, R, 523 tellurite ion, R, 522 tellurium, S CHR from Se, 505 test tube, 146 tetraborate, see borate tetrachloroaurate(III), see gold(III) thallium(l) ion, R, 507 thaIlium(I1I) ion, R, 509 thallium, S from Group IIIB cations, 546 thin-layer chromatography, 495 thiocyanate ion CT, 460; SM, 476 D ip, CI-, Br-, 1-, SM, 477 D ip, [Fe(CN)6P-, [Fe(CN)6l - , 392 R,317 thiosulphate ion CT, 459; SM, 474 D jp, SOi-, S2-, SO~-, 388 Djp,S2-,SO~-,389 R,305 thorium(lV) ion, R, 540 S CHR from Sc and rare earths, 505 tin(II) ion, R, 237 tin(lV) ion, R, 240 titanium(lV) ion, R, 532 titanyl, see titanium(lV) T.K dropper, 156 transfer capillary pipette, 175 transference number, 16 tungstate ion, R, 509 Tyndall effect, 85 ultra-filtration, 86 ultramicroscope, 85 uranium, S CHR from mineral ores, 506 uranyl ion, R, 538 valency, vanadate ion, R, 527 van't Hoff coefficient, 11 vapour pressure, lowering of, Vogel reaction, 262 wash bottle, 146 SM,161 water dissociation of, 35 ionic product of, 35 wet reactions, 145 working hints, 152 zinc(II) ion, R, 272 zirconium(lV) ion R,535 S CHR from Th, 506 zirconyl, see zirconium(lV) 605 Qualitative Inorganic Analysis Vogel 's unique and comprehensive text has been completely revised and uPdated for this fifth edition, The book Begins with a discnssion of the basic physico"chemical aspects Qf, reactions utilised in qualitative inorganic ana'ly is A description of lab'oratory equif1ment tQlI ws and operations wfiich include sem'imicrQ ,and micre techniques, and simple eleotroehemical, speetroS!iol'!ic and chromatographic methods Tihe react'ions of the most impeftant cations and anions are described, followed by a f,r,eatment of systematic qualitative analysis Sample preparatjen, dissolution and fusion of insoluble materials are treated in detail A separate chapjer deals with the reactions of less common ions, with guidelines to their separation and identification in the course of systematic analysis Finall~ a simplified course of qualitative- analysis is given; this chapter will be particularly useful where the time allocated to qualitative analysis is limited This book will continue to be of immense value 10 A-level and ungergraauate students of chemistry and thelt teachers, as well as practising analysts r: Longm n Group £14.9!p not U K price nly , ISBN 582 44167 The late Arthur I Vogel was formerly Head of the Chemistry Department at Woolwich Polytechnic G Svehla, Ph.D., D.Se., F.R.I.C., is Reader in Analytical Chemistry at The Queen's University of Belfast ... text-book of macro and semimicro qualitative inorganic analysis Includes index Chemistry, Analytic -Qualitative Chemistry, Inorganic I Svehla, G 11 Title Ill Title: Macro and semimicro qualitative inorganic. .. Cataloging in Publication Data Vogel, Arthur I Vogel' s Macro and semimicro qualitative inorganic analysis First-3d ed published under title: A text-book of qualitative chemical analysis; 4th ed published.. .VOGEL' S TEXTBOOK OF MACRO AND SEMIMICRO QUALITATIVE INORGANIC ANALYSIS Fifth Edition Revised by G Svehla, Ph.D., D.Se., F.R.I.e
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Xem thêm: Macro and semimicro qualitative inorganic analysis 5ed vogel , Macro and semimicro qualitative inorganic analysis 5ed vogel , A. Chemical formulae and equations, B. Aqueous solutions of inorganics substances, C. Classical theory of acid-base reactions, D. The Bronsted-Lowry theory of acids and bases

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