BUKU INI TIDAK UT PERJUALBELIK UNIVERSITAS SUMATERA UTARA FAKULTAS MATEMATIKA DAN ILMU PENGETAHUAN ALAM PROGRAM S1 KIMIA LABORATORIUM KIMIA ANALITIK LAPOR PRAKTIKUM KIMIA ANALITIK | NAMA ADE APRILIA BATUBARA NIM 210802095 UNIVERSITAS UNIVERSITAS SUMATERA UTARA PROGRAM STUDI S1 KIMIA GRUP/ PARTNER ZAHWA FAHRADINA TANGGAL PERCOBAAN: 14 APRIL 2022 PERCOBAAN » REAKSI PENDAHULUAN ANIONDato: fp NAMA Amun gaa NIM 2002095 Pékuctas/Jupusay —_:MATEMATIKA DAN Tumu pENGeTANWAN —_AuaM / SL KIA CaporaTurium /taprver :2AKWWA FAHRADINA Hae HancGAL Peacoeaan: FAMIs/21 APRIL 2022 JUOUL PERCOGAAN | REAKSI PENDAHULUAN ANIOM O O oC] G) O () UOUAN PeRCoBAaH |- Untuk Mengetehui dasar Klasifrkas’ amen me- CO Aunt Voge} dan Tread well =) [Enns mengetahui featsi pergena dan reapsi i) O O 2 os O O O Stesitik dant anion - Unni mengetahui Afat hatil reakh’ dan anton Auat pan panany [Ut Alat Nama Alat Merk Ukuran ~ Talung reaks! Pyrex - ~ Rak falung nakii - _ Of; | fpee betes a - i) = Boll Aquades t - _ Ol Surbet <= - Gi aes Penyepit A Dipindai dengan CamScanner— Bunsen - - cKonk Ai filam ~- Bruh talung - a = Hashk = - ex - karet = a C = Tissue Passeo - O - Spatila - a (3) - Maker - =. O - Jamung fangan oe O = das lab i a O O 2. Bahan 7 Mama Gahan Fase Konsentresy CO j- Nacl a4 = O — Hrs0y e % i) ~ Chel a4 = oO a AgNiog aq - oO ~ KBr ag 2 O - kt 4q 7 oO I= Po(cH scot) > ai - O j- Ker Oy ay a oO - Kens ag = Oo Cute age lap en - Fels a4 = ia) - Cla coolty aq = Dipindai dengan CamScannerDate: fuatu Sen wa Aapat divratkan menjadi = Ahatisa anion borhij uen nalita adanya ton dalam _ a fe = Allcoho! aq 2 O Naa Soy a - O oCM05), a4 - oO Bala a - O - Cacl, a4 ~ Oo = Aseton 44 z= 0 - (NHy)2 dy 44 : Oo - Nanos aq - = - PA aa - O - Nar cds 24 - O = NiSoy aq - O - kMn by aq - O = th (Nos) a = fe) ~ Fesdy a s O @)_Honuan Pustaka Unnk kav ini yang akan dbehas ada. O lah Spenipkasi dan analisa huabtany O Anat Kualitarf insendin kerbagi loo, O metjadi dua bagian, yaity aralifa Kua. O Litaty ation dan analira Kualitatt Kafron . a a a OS I Sam pel. Ahalia anion n dapat juga oly Ld uta dalam bebaga | Stdeng ke — ‘Dipindai dengan CamScannerDate aT —S>> C J | Widupan tl pet dalam penetra darah,_ C J unin, dan alnya . Unuk anion dt - oO festa ke dalam beberapa belas the oO Antalanyar + Anion fedorhana sepen :% \ US FT, atau CN, + dnion okso disknet Kpern: Nos, Sy? + Anion polimer okso Apert: PUKat, borat atau pos fal yang eer - koadensag’. » Anion Komplees halida ¢e- perh Tats dan Kompleks anion 9425 by- basa bany at orn oksalaé. Malisls Kualitoenp mongg unakan dda matam “fe yaitu reakh keying dan reaksi basah. Reaksr konng dapat diquaakan fede tat padat dan reakit balah UNMK tat dalam lautan. kebanyakan K- aki Ruing yarg diucalkan dig unaken untuk analiciS femimikte deagah hanya moditikat’ kecil. Dengan emp erha fe ont daftar Klamtan berbagar galam [dalam air dan polant yang lara, je— bita diperkirakan, Misaln ala th fulfi'da teak lant dalam asam gram Karbonat trdals laqe talam fal fide. (sus | Y., 2019) Dipindai dengan CamScanner gogofgjojojojgjjcjqaa\a\a\ \\\\ \ \ f \ Date = | Mede Yang prfedie untnik men ce RA at tidak froemans Aperh’ yaa, fla dijelaskan dalam bab febolumnya “unnic c\ \ a kation. Belum ada Skema yang benar- Genar memuaskan Klah diusulkan yang Memung kiakan fortsabo Anion -ANlon_ unm men padi ompok - kelompok beser, dan pemisahan tegas berkunya Aan Sehap felompok mesjact koastryen (ncle - endennya.\ Pada dasarn proses yang diguaakan dapat dba haenja olt” (4) ya ng meth atkan 1 en fia dengan product volant Arp enh bada perlakuan Men asam Yan (b) yang bergannin a - da teak’ dalam (an ahs OOOO OJO|O\O\WW\a Kalas (i) dibagi lagi meajacte Li) gas ang ferbent dengan alam klonda ener atay ajam Julfat enor dan (ii) gal atau wap yang tet en tug den an asam sul cassia Kelas (8) Aib aon (ac gen adi (i) teakyi Jesgenda fea de dan ta oksidaste al aa Rduks¢ alam _lanitan| Svehla G. 4429 Dipindai dengan CamScannera ee \ UE \ 0 Anion Grup f. Pengupion uank ang gota 1 up t dapat ai ldeuken , dalam banyak Kets yen la_padlat yang hdak Ake tah’ jadi, icon fost momerlukan | Jam pad 2 fetes lamtan yang nelak diketahur , 5e- bagran padacan yang dihaluskan feu - karan Febuns berat dapat Aguaakan. Protedur ini cukup Unk! mendelen’ Karbenat , fale, {ro tul fat hiknt_, hanida, dan beberapa fulfrda . Namua, Jal pro dan loeberepa lejam hdak laut dalam Kol young digunakon, dan uj( sulfrda dapat terlewa tKan pike belerancy liga. buhgkan dengan logam -logam tai Ditka hail nega diperleh Saat meng ap Sulfide 1 mneaggurakan fpadatan. pataskan sampel £ atan yang hdak di ketahu (Rita Kir, wiurag Kepala kote age) felama (o JO[0 dlofolalolo|clolo\o\c\o alo J | | I Og i hinggp (5 Honit . clengan lariten kKuge Naxos dan faling. Ue sulfrela Kemy- dian hans aiulang ada ren'dy ag | CG ff padat (ikea ada) “dan pada flerae. hyo. Anion Grup U. Unrk ‘ine gunakan fampel ukuran Kepa (| Takes apr ale (Aer Po) Dipindai dengan CamScannerDate Gelongan T, LT ALamn yang gatam pees nga f dak ame dam aur dan alam MefaL, Reap garam banumnya [aAue dalam aie. Un tlk felompok (ni termasuk. asam klenda hid rom , hed a dk, Hesianat, ferri fianit, Kobal efkanat, ‘eto Rona , dan lipo klont. Gelongan L, Asam yang garam perakaya lame da- lam asam Alerat ,eebap trdak lant Blau _sukar (amt dalam air dan ga- ram banumaya faut dalam or. Unnik Klompot thi termasuk asam_hrdrJa(fat, idee Wlenat, hidio eluate, arbre asetas Gantk, dan htpo fisfat - Gelongan ti Asam yang garam _pesabnya berwama fatth dan lame dalam alam nitrat pi garam banurneer Sukar atay dak lant dalam air cfetapi lame da. lam asam nttrat . Untuk €elompok ne lermasut Sulful __deenous lars, spor, Karbonat ofesalat, Codite , by ne, rmaolibde (Rlena aan flume | bartane , Strat_, meta _- dan Asan, / golqqo{o[oja|o|ojojo|ojoojo}o|q|oo\a\c\n tf Gelong an ly, Asam Yan Jaren, Pemelje bert b ertiarna, ‘Tread uaF. 8 ae Dipindai dengan CamScannerDate ee | kartonat vr at_ di (dunk tah dalam enda- pan pn_kelompek_ dong dengan buth an bal fat fe am Laban Asam aftat pike pean Untuk membuat lamtan Ming eagn- tan_Karbonat hams dilakutan pada O eben adatan asli febagai ben fut : O UA Sebagian dan pada tan dit ambah - O fan _katiuin klorat dalam jamlah ganda, air ditam bahkan , dicompar Secata tneayelumh , dan Afam fulfat Mer ditambahkan. Sebuah luth me- Auiyakkan adanya karbonab- Pemicahan dai, ton fi kasi Auonde dan exalate: Residu yang frelak laut dalam sam asetat _dipeslarukan pada filter cle- ngan_asam Salfat encer dan dreug’. fluoride oli rent fikon dalam rendu deagan_tindakan paca kaca. Oksalat ditdent fan dalam frleeat cling an dakolon asi 0/01N ermanganat . Filerat dan vagelah én Blam apetae dae Im Ongandung fon beakut : Sulfit, arsenat , arkewe , fost , dan farerate Creeps fubs. acs. 214 [48 fo. Fedde) Dipindai dengan CamScannerq pose DUR. PERLOBAAH Phd A. talung I = Dimasutkan Mad ke dalam tabung reakh = Ditambahkan HeSoy (p) = Diamah pensbahan yang knadi = _Ditambahkan Konforin - Diamati penbahen yang tenacls” = Ditambahkan tees krunoy Drcumart Pembahan yang _tenads Vikocok - Didiamkan Diamar perubahan yang tradi 8. Tabung T = Oimasukkan Nacl Ke dalam tabung rath = Ditambahkan Ag Nos a eee oe. Dima fi pene han_yang tera + g. bre A. Tabung 1 ~ Dimasukkan Ker kedalam tabunag Rakh’ - Ditambahkah Hs50y (p) - Dlaman_peubahan yang tench = Ditambahken _klo IZ Dikutup dengan plese dan ditkat Lagan karet. Dipindai dengan CamScanneriamah persbahan yang, ter acti - Ditambankan _KMncy = Dikocok = Diamar peribahan yang tenecli 8. Tabung i ~ Dimasukkan KBr ke dalam falung reakh’ = Mambahkan Agnos <_Diaman pembahan yang tenjacls a A Tabung 1 - Mambahkan KI ke dalam tabung reakh’ ~ Ditambahkan tr5oy Cp) \ Viamat penubahan yang teraclé Deambahkan Klor form - Yiamax perutahan yang frac” = Ditambahkan | teks KMnoy = Diamat pertbahan yang terjacti = Dikoook Kuat -kuat a - Diamati penbahan yang tenacté |e Tabung fl = Olmasukkan KT ke dalam tabung peaks; - Dtambahkan Cusoy =_Diamak_pembahan yang tejach Dipindai dengan CamScannerDate _[e-Tabung aj = Dimasuktan KC ke dalam tabung reqkh’ - Ditambahkon PbCCHs C00 Je = Diamant feribahan yang tesjacli 4. Croy>> A. tabung L ~ Dimasukkan Ketroy ke dalam tabung rears’ - Ditambahkan Ag Nos - Diamah perubahan yang tenjarol 8. tabung — Dimasuckan KeCrdy ke dalam tafung reath’ - Ditambahkan Pb (CtsCoo) 2 - Diamat permbahan yang teruelr y > CONST A-Tabung t J Dimasugkan KeMs Kedalam tabung reakh’ - Ditambahkan Fecls - Diamat® perubahan yang terjade B. tabun a L__ Drmasutkan KCMS Fe dalam taba reat |-_Drtambah kan Cu $0, |- Diamati penbahan ang eihadi - pitambah kan afeton Dipindai dengan CamScannerDate - Diaman’ perubahan yang ten acl C-Tabung tt = Dimasukkan KONS Kedalam tabung reakh’ - Ditambahkan Co (NOs) - Dioman fenubahen yang ten adv - Ditambah kan aseton ~ Olamati fenbahan yang tered oO G. CH3Coo- O A. Talung | O = Dimasukkan NHyCHscoo dalam tabung wats’ O = Ditambahkan — HeSoy O = Viaman perbahan yang ejacl’ O i” Ditambahkar alkohol ) =p, arr Viamani pembahan yang teyocks Dtpanarkan - Diamar arema yang dhahlkan 6 .Tabung 2 — Dimasukkaa Ky 3000 ka dalam Satong teakh* - Drtambahkan Fecls = Drpadaskan - Diaman perrbahan yang tenaolt EEN | =n) aman PertoahanEyangl terse ee IC Tabung ll | Dimasukkan NHy CHsCoo Ke dalam tabung rath’ - Ditambaikan AgNO, Dipindai dengan CamScanner| : = Dlamati_pentbahaa yany ten acl - Ditambahkan alkohol = Diamat penbahan yang tena 9. Soy A-Tabung 1 = Dimasukkan Narsdy ke dalam tabung ak h - Ditambahkan Bache _ Diamar permbahan yang terjadt b.Taburg Ul = Ditrasurkan Narsoy ke dalam tabung reaksr - Ditambahkan Pb (MUs)2 - Diaman penbahan yang ty adi ¢.Tabung - Dimasukkan Naz Soy ke dalam tabung rath - Drtambahkan GClr ~ Diamar pertbahan yang tefjacti — Pitambahkan aseton - Diamar perbahan yang tefadi @- C20y* — Dimasukkan CNHy eCedy keolalam tabung heakh’ L Ditambahkan Hr50, (9 fo fe Diamar: perubahan yang tefpad Dipindai dengan CamScanner[_ on Dambahkan kin Oy - Diamar pembahar yang tenads a) B. Tabuing 0 a Dimasutckan (MHu)2 (204 ke dalam labung Aeak A’ ) ~ Ditombahkan Catle = Diamant penbahan yang bey acl 9. Nog” 4-Tabung IT - Dimasukkan NaNos ke dalam tabung Rakh’ oO - Ditambahkan H250y ¢p) OC i Di dingin kan - Diamant perbahan yang fenjacl = Ditambahkan Fesoy melalui dinding tabuag fecara perlahan = Diamar pembahan yang terjadr 8. Tabung u — Dimasukkkan DPA Ke dalam tabung hath’ = Ditambahkan Nanos melalur dining babuag Secota_perlahan - Diaman pembaben yang fer cle lo. C03 ?- A. ‘tabung t de Dimasukkan Nart03 dalam tabung reaki” Dipindai dengan CamScanner- Ditambahkan NiJoy = Diamar pembehan yang Bjadt B. Tabung = Dimasuxtean NarCos kedalam tabung realh’ - Ditambahkah Cade - Diamar peubahan yang terjacl” Dipindai dengan CamScannerDate ee abst PeRCOBAAN | T cf- | — = IMacl 4 Hesoy AS Nasloy F2HEIT ee —Hyou er a= att +20 9 2Helt nb higjau kopor - Natl + Ag Nos > Agel 4 + Na NO3 Putih Agt tel- —» Agel L Purh 2.0r- = Kor + HoS0y pM KHON 4 HBr | xo DKMnOy + 3HrMOy => Kr50y + 2trInSOy 43496 FSOn tar ton 9 bre tHed | ks IKGr-FUGHeS0y F.2kMady —7lOKH Sout + KaS04 + giasou + gHeo t SBr2 t + CHCl t coklat_kemerahan |= ker t AgNos > Ag Br +KNOs Putth Ag*+5r7 > Ag Br puhh Dipindai dengan CamScanner[3.1 =kEHHeS0ua) 9 kHs0, + HE [ x10 Lk Ou +3HS0y —7 ke60yt2Maso4 +3H-o+ SOW IH FON 9 Tat + Heo [XS LRT + BHrS0y ta KMady > lOkHSOy + Krsou + LMnSoy +812 PtOHoo + CHC ole I 2KT tCusoy —9 Cule L + Krsoy huning pucat Get 420° Gate L towing pucat _ akt + Pb CCH3Coo)2 > Pbt2 ) t2cHscook kuning L7* +at° > Polad kuning 4. CrOy> _ K2Crdy + 24gN03 2 AgeGrdy L F2KNO3 Merah bata ohgt + Croy” 9 Agecroy L merah bata — Kalroy + PG (cHstoo)s > PoCroy b +2CHs Cook kuning Wh F CrOy?~ 9 PbCrOu | ~ kuaing Dipindai dengan CamScannerDate SONS” - BKCNS + Feely 9 FeCens)3 +9 KCI lantan mepech darah FeSF + BCNS= 5 Fe CONS)s ~— Latutan merah dearah DENS + CuSdy MAP CuCCNSIr + Ker5Oy gelatin hijau Korr Cut F acns- 28 Cu (Cus)e gelatin Wijau kofor | 2KCNS + CoCMOs)2 9 Cy CONS)» +2 NOS gelatin bina Cot + RONS~ BA Co CONS) gelatn bir G. CH3Coo7 L 2NHyCHsCoo +H2S0y “> actscool * +(NHe)eia, arma lalon hup accom Ht SY acHscool aroma lealoa hup = 3KHyCHy Coottedls 47 te CHslo) 1 +3NHuY Codat kemerahan teh #3cHs(ou” 7 Fe (cHscoo)s 1 Coklat Kemercahen Dipindai dengan CamScannerDate: Nity CHs(00 + Agios “HAY Ag CHs Coo + My NOs Gelaha pth ha + Hs Coo mi Ag CHs Coo gelatin peeth tT: £047 - HarSoy FBach 9 Ba Soy L $2 Nacl yurh Bar £ Soy —5 Ba Sy L puth ~ Marsoy + Pb CNOs)2—7 flo soy L +2Nahos purh et + L0y* —> Po soy L punh IG OWUU O/OJOJUJU|UJO\O\O|O\O\ ~Nos5ey + Cath 225 Casoy +2Nacl gelahn putih (a4 +80y'7 9 CaSOu gelatn put 9. (104 D(C MHy)2C20y + Cath Garo | +2NHvol putih (at + Gdy 9 CaGdyd punk Dipindai dengan CamScannerAn Date -(N Hue Gy +HrL04 (py Key Hr G0y +CNHa) 2 S04 cincin violet 2UT t Gogh Ren yc 04 Cacin volt 4. Nog™ -INaMos +Hes0u gerdtintan? Fee (soy)3 - ENO Cincin coklat ~ DPA + NaNo3 —> Co HsNH Ce Hs cincin bin Karbaole (O[G/O[E[O[O/O[Q|Jo|O|9\O\0}0|0\0 lo. CO3*” = Nar C03 FNiS0y I NiCOz | + Nar Sdy path Nit + Cos” 5 Nicos L push LL Marto3 +Cath —9 Cater) +2Nacl futih Cart + C03 5 Ccord puth (HOO / Dipindai dengan CamScannerDate vorantstaa _— Atthar , P., 1930. Semi micro Qualitative Analysts. London : McGraw - Hill Book Company , Inc. Page 43 Grehla, @, (949. Vogel's Text book of Macro and femimicre Guatitanve Inorg atic Analysis - New York + longenan Group _ Limited Page 293 Tredwell, FP, 19e.. Anal ticed Chemistry Volt . Net York: ohn Wiley & Soas, (nc. Page 284 Yarn , Y., 2019. Belajar Mudah _Kinia Analisis. Jakarta: Educenter tndonesia Haman 84-85 Herp: pubs. acs oty [doi /to.t0x fed ol2 poe Access on 1} Desember 1935 4 Medan, (H April 2022 Asisjen Yrakiikon, af Q [aha Farad) (He Anta Banshee) Dipindai dengan CamScannerPenerbit EduCenter Indonesia Dipindai dengan CamScanner2) mempelajari kimia dan unsur-unsur serta ion-ionnya dalam larutan. ku Dalam metode analisis tif kita menggunakan beberapa pereaksi diantaranya pereaksi selektif, sensitif, dan pereaksi spesifik. Pereaksi- pereaksi ini dilakukan untuk mengetahui jenis anion / kation suatu Jarutan. Analisa kualitatif dilakukan untuk mengetahui jenis unsur atau n yang terdapat dalam suatu sampel. Analisa kuantitatif| Adalah penyelidikan kimia mengenai kadar unsur atau ion yang, terdapat dalam suatu zat tunggal atau campuran, Terdapat dua langkah utama dalam analisis adalah identifikasi dan estimasi_ komponen- komponen suatu senyawa, Langkah identifikasi ini dikenal sebagai analisis kualitatif sedangkan estimasinya adalah analisi kuantitatif Untuk kali ini yang akan dibahas adalah spesifikasi dari analisa kualitatif. Analisa kualitatif itu senditi terbagi lagi menjadi dua bagian, yaitu analisa kualitatif anion dan analisa kualitatif’ kation, Suatu senyawa dapat diuraikan menjadi anion dan kation, Analisa anion bertujuan untuk menganalisa adanya ion dalam sampel. Analisa anion dapat juga digunakan dalam berbagai bidang kehidupan, seperti dalam pemeriksaan darah, urin, dan sebagainya. © Analisa kualitatif anion Analisa anion adalah analisa yang bertujuan untuk menganalisa adanya ion dalam sampel. Sedangkan analisa kualitatif dilakukan untuk mengetahui jenis unsur atau ion yang terdapat dalam suatu sampel. Jadi, analisa anion secara kualitatif merupakan analisa yang dilakukan untuk mengetahui adanya anion serta jenis anion apa saja yang terdapat dalam suatu sampel. © Analisa kualitatif kation Analisa kation adalah analisa yang bertujuan untuk menganalisa adanya ion dalam sampel. Sedangkan analisa kualitatif dilakukan untuk mengetahui jenis unsur atau ion yang terdapat dalam suatu sampel. Jadi, analisa kation secara kualitatif merupakan analisa Dipindai dengan CamScanneryang dilakukan untuk mengetahui adanya kation serta jenis kation ‘apa saja yang terdapat dalam suatu sampel. Macam-macam kelompok anion Untuk anion dikelompokkan ke dalam beberapa kelas, diantaranya: Anion sederhana seperti : 0”, F, atau CN’. Anion okso diskret seperti : NO*, SO. Anion polimer okso seperti: silikat, borat, atau posfat yang terkondensasi. Anion kompleks halida seperti: TaFs dan kompleks anion yang berbasa banyak seperti oksalat Analisis kualitatif. menggunakan dua macam uji, yaitu.reaksi ering dan reaksi basah, Reaksi kering dapat digunakan pada zat padat dan reaksi basah untuk zat dalam larutan, Kebanyakan reaksi kering yang diuraikan digunakan untuk analisis semimikro dengan hanya modifikasi kecil. Dengan memperhatikan daftar kelarutan berbagai garam dalam air dan pelarut yang lain, jenis anion yang terdapat dalam larutan bisa diperkirakan, Misalnya garam sulfida tidak larut dalam asam, garam karbonat tidak larut dalam sulfida, Untuk mendeteksi anion tidak diperlukan metode sistematik seperti pada kation, Anion dapat di Hhkan dalam golongan-golongan utama, bergantung pada kelarutan garam peraknya, garam kalsium atau bariumnya dan garam zinknya, Namun, ini hanya dianggap berguna untuk memberi indikasi dari keterbatasan pada metode ini, 2. Identifikasi Analisis Anion Pros proses yang dipakai dapat dibagi kedalam proses yang melibatkan identifikasi produk-produk yang mudah menguap, dan proses yang bergantung pada reaksi-reaksi dalam larutan, Secara kasar, reagensia atau pereaksi yang dapat dipakai adalah : - Zat kimia kualitas teknis 85 Dipindai dengan CamScannerVOGEL'S TEXTBOOK OF MACRO AND SEMIMICRO QUALITATIVE INORGANIC ANALYSIS FIFTH EDITION Revised by _ G.SVEHLAVOGEL'S| TEXTBOOK OF MACRO AND SEMIMICRO QUALITATIVE INORGANIC ANALYSIS Fifth Edition Revised b G. Svehla, Ph.D., D.Sc., F.R.LC. Queen's University, Belfast >m> RAR ann Longman London and New York Dipindai dengan CamScannerLongman Group Limited London Associated companies, branches and representatives throughout the world by Longman Inc., New York 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 Semimicro 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. 1. Chemistry, Analytic-Qualitative, 2. Chemistry, Inorganic. I. Svehla, G. Il. Title. III. Title: Macro and semimicro qualitative inorganic analysis. QD81.V6 1978 54477-8290 ISBN 0-582-44367-9 Printed in Great Britain by Richard Clay (The Chaucer Press) Ltd, Bungay, Suffolk © Longman Group Limited iv Dipindai dengan CamScannerCHAPTER IV REACTIONS OF THE ANIONS The methods available for the detection of anions are not as systematic as those which have been described in the previous chapter for cations. No really satisfactory scheme has yet been proposed which permits of the separation of the common anions into major groups, and the subsequent unequivocal separation of each group into its independent constituents. silver salts, of their calcium or barium salts, and of their zinc salts; these how- ever, can only be regarded as useful in giving an indication of the limitations of the method and for the confirmation of the results obtained by the simpler procedures to be described below. The following scheme of classification has been found to work well in practice; fi Essentially the processes employed may be divided into (A) those involving the identification by volatile products obtained on treatment with acids, and (B) those dependent upon reactions in solution. Class (A) is subdivided into (i) gases evolved with dilute hydrochloric acid or dilute sulphuric acid, and (ii) gases or vapours evolved with concentrated sulphuric acid. Class (B) is subdivided into (i) pre- cipitation reactions, and (ii) oxidation and reduction in solution. CLASS A (i) Gases evolved with dilute hydrochloric acid or dilute sulphuric acid: Carbonate, hydrogen carbonate, sulphite, thiosulphate, sulphide, nitrite, hypochlorite, cyanide, and cyanate. (ii) Gases or acid vapours evolved with concentrated sulphuric acid. These include those of (i) with the addition of the following: fluoride, hexafluorosilicate,* chloride, bromide, iodide, nitrate, chlorate (DANGER), perchlorate, permanganate (DANGER), bromate, borate,* hexacyanoferrate(II), hexacyanoferrate(III), thiocyanate, formate, acetate, oxalate, tartrate, and citrate, * This is often included in Class B(i). 297 Dipindai dengan CamScannerFrees SEMI MICRO QUALITATIVE ANALYSISFIRST EDITION.SEMI-MICRO QUALITATIVE ANALYSIS BY PAUL ARTHUR, Pu.D. saitant Projessor 0} Analyfica msery Oklahoma Agricultural and Mechanical College AND OTTO M. SMITH, Px.D. Oklahoma Agricultural and Mechanical College First Eprrion McGRAW-HILL BOOK COMPANY, Inc. NEW YORK AND LONDON 1938 Dipindai dengan CamScannerCopyricut, 1938, BY THE McGraw-Hitt Book Company, Inc. PRINTED IN THH UNITED STATES OF AMERICA All rights reserved. This book, or parts thereof, may not be reproduced in any form without permission of the publishers. THR MAPLE PRESS COMPANY, YORK, PA. Dipindai dengan CamScannerPRELIMINARY TREATMENT OF SOLIDS 143 ions were present in the original unknown. Addition of some anions cannot be avoided, but it is possible to use the different solvents in places where this causes no trouble. For this reason, it is best to prepare the solid unknown, using a special Procedure for each, group. 1. ‘Anion Group I. The tests for the center of Group I may be performed, in most cases, on the solid unknown. Thus, where the procedure calls for 1 to 2 drops of a solution of the unknown, a portion of the pulverized solid about the size of a grain of rice may be used. This procedure is adequate for the detection of the carbonates, sulfites, thiosulfates, nitrites, cyanides, and some sulfides. However, the sulfides of a few metals are insoluble in the HCl used (see Group II Metals), and the sulfide test may be missed if the sulfur is combined with these metals. In case negative results are obtained when testing for sul- fides using the solid, heat a sample of the solid unknown (about the size of a match head) for 10 to 15 min. with a strong solution of Na,COs, and filter. The sulfide test should then be repeated on both the solid residue (if any) and on the filtrate.* 2. Anion Group II. For this, use a sample about the size of an an ordinary match head. —— water as is possible. Filter, and save the filtrate. Heat the residue, on the steam bath, with saturated Na2CO; solution for 10 to 15 min. Filter, discarding the precipitate. Combine the aqueous and Na;CO; filtrates and acidify with dilute H.SO,.t Filter, if any precipitate forms, and use the filtrate for the Group II tests. * Many of the insoluble sulfides will react, to some extent, with strong, hot solutions of NazCOs, forming the metallic carbonate and some Na;S. ‘The latter is soluble in water and reacts readily with dilute HCl. + Add the acid cautiously as otherwise the CO: given off on acidifying the Na,CO, will cause the solution to overfiow the sides of the container. Dipindai dengan CamScannerANALYTICAL CHEMISTRY Based on the German tert F. P. TREADWELL, Px.D. Professor of Analytical Chemistry at the Polytechnic Institute of Zirich TRANSLATED AND REVISED WILLIAM T. HALL, 8.B., Aasistant Professor of Analytical Chemistry, Massachusetts Institute of Technology Vorume I QUALITATIVE ANALYSIS FOURTH ENGLISH AFTER THE EIGHTH GERMAN EDITION TOTAL ISSUE, TWENTY-ONE THOUSAND NEW YORK JOHN WILEY & SONS, Ino. Lonvon; CHAPMAN & HALL, Limrrep Dipindai dengan CamScannerPART IIL REACTIONS OF THE ACID CONSTITUENTS OR ANIONS DIVISION OF THE ACIDS INTO GROUPS ‘The classification of the acids which is given here was first pub- lished by R. Bunsen in 1878 (in manuscript form) for the use of his students; it was adopted (with his consent) by V. Meyer and F. P. Treadwell in their “Tabellen aur qualitativen Analyse.” It is based upon the different solubilities of the barium and silver salts. Group I Acids whose silver salts are insoluble in water and in nitric acid, but whose barium salts are soluble in water. ‘To this group belong hydrochloric, hydrobromie, hydriodic, ferro eyanic, ferricyanic, cobalticyanie, thiocyanic, and hypochlorous acids. Group I Acids whose silver salts are soluble in nitric acid, but are insoluble, or difficultly soluble, in water, and whose barium salts are soluble in water. To this group belong hydrosulfuric, hydroselenic, hydrotelluric, nitrous, acetic, cyanic, and hypophosphorous acids. Group I Acids whose silver salts are white and soluble in nitric acid, but whose barium salts are dificultly soluble or insoluble in water, but soluble in nitric acid. +» To this group belong sulfurous, selenous, tellurous, phosphorous, carbonic, oxalic, iodie, boric, molybdic (selenic and telluric), tartaric, citric, meta- and pyrophosphorie acids. Group 1V Acids whose silver salts are colored detelsshlaniamnitaiemeeiaipsients To this group belong phosphoric, arsenic, arsenious, vanadic, thiosulfuric, chromic, and periodic acids. 284 Dipindai dengan CamScannerDecember, 1935 oxour v Tons: chlorate, nitrite, and acetate, These ions are identified in the filtrate from Group IV without pre- cipitation. GRour VE Ton: nitrate. The nitrate iom is identified in some of the original solution. EXPERIMENTAL Preparation of te Solution for Analysis ‘The substance to be analyzed must be i the form of the sodium, ‘ammonium, or potassium salts. The “prepared solution is made in the usual manner by treating the solid substance with normal sodium carbonate solution, boiling, and filtering. The filtrate, or ‘prepared’ solution, is then ready to be analyzed for Gros T. Tn case the heavy metals are absent the “prepared” solution is ‘made by dissolving the sample in sodium hydroxide and water. Group I—Detailed Analysis Group I must be analyzed, for calcium hydroxide is always precipitated upon the adeltion of the group reagent, thus pro- hibiting the use of a suitable group test. If the color of the “prepared” solution indicates the possible presence of chromate, the procedure according to (a) must be followed; if not, the Procedure according to (3). (@). The “prepared” solution is diluted to 50 ce. with water, 2 ce. of AN sodium hydroxide js added, and the anions are pre- ipitated completely with 24 calcium’ nitrate solution, filtered, fand washed twice with water, and then with 5% ammonium hydroxide until free from the chromate fon. "The filtrate is boiled 40 precipitate completely any sulfite or tartrate remaining in solution. Any precipitate obtained on boiling this solution should be combined with the group precipitate. The residue is ‘then analyzed according to the scheme for Group I. ‘The fk trate, whieh contains Groups II-V, is reserved. (8) ‘The “prepared” solution is diluted to 60 ce. with water, 4N sodium hydroxide is added, and the anions are precipitated completely with 24 calcium nitrate, heated to boiling, fitered, fand washed twice with water, and then until completely free from the nitrate ion. The filtrate, which contains Groups II-V, is reserved. The precipitate may’ consist of calcium carbonate, calcium fluoride, calcium oxalate, ealeium sulfite, calcium ar senate, caleium ‘arsenite, ealcium phosphate, and calcium tar- trate. "The precipitate is then treated with 12.5% acetic acid, Carbonate is identified in the group precipitate DY an feevescence upon the addition of acetic acidp In case it was necessary to make the “prepared” solution, the test for cf Donate must be made on some of the original solid as follows: to.a portion of the solid is added a double quaatity of potassium chlorate, water is added, thoroughly mixed, and dilute sulfuric Acid ip added. An effervescence shows the presence of carbonate. ‘Separation. and identifeation of fluoride and oxalate: The residue which is insoluble in acetic acid is treated on the filter ‘with dilate sulfuric acid and washed ‘Fluoride is identified inthe residue by its etching action on glass. Oxelateis identified i the Bitrate by the decolorization of O01 permanganate. “The filtrate from the acetic acid treatment may contain the following ions: sulfite, arsenate, arsenite, phosphate, and tar- trate ‘crystalline mercurous chloride upon the addition of hot saturated imereutie chloride. sulfite has been shown to be present, the remainder of the ‘Altzate is boiled Co expel the sulfur dioxide completely, as shown by the sulfite test ‘Arsenate i identified inthe boiled Sltrate by the formation of a brown coloration upon the addition of concentrated hydroclorie acid and sold potassium iodide, 387 Arsenite is identified in the fltrate after diluting to double volume by te dccolorization ofa few drops of 0.0LN iodine. If ether arsenate or arsenite has been shown to be present, the remainder of the filtrate is treated with solid sodium sult, rade strongly aeid with hydrochloric acid, heated to boiling, land the arsenic is completely precipitated with hydrogen sulfide, filtered, and the filtrate boiled to.expel hydrogen sulfide ‘Phosphote is identified in the filtrate by the formation of a yellow preotate upon the adaton af atunonism molybdate Tartateis identified in the filtrate after the removal of calcium with sulfurie acid. The solution i treated with 2 or 3 drops of ‘normal cobalt nitrate, 4.V sodium hydroxide is added until the solution takes on a permanent blue color, then 6 cc. ia excess; hheat to boiling and filter. A deep blue coloration in the Bitrate shows the presence of tartrate. The observation must be made ‘om the hot fltrate, forthe blue color disappears on cooling. tivity ofthe tests for the ions of Group 1 areas follows, "The sensi Group II—Detaited Analysis iminary Test for Group I: A precipitate upon the adai- tion of 0.51 barium nitrate tothe filtrate from Group T shows the ‘presence of Group II. ‘Sulfate is identiied in the Strate from Group T by the forma- tion ofa white precipitate insoluble in water upon the addition of Ihydrochlori acid and barium nitrate 'f Group TI was shown to be present the entire filtrate from Group Lis precipitated completely with barium nitrate, heated to boiling, filtered, and washed twice with water, and then until fre from the nitrate jon. The filtrate, which containe Groups TII-Y, is reserved. The precipitate may consist of barium sul- fate and barium chromate Cliromate is identified in tie residue by the formation of a yellow precipitate by treating with hydrochloric acid, neutralizing ‘with ammonium hydroxide, and acidifying with acetic acid "The sensitivity of the tests for the ions of Group TT are as follows, expressed in milligrams pet'10 cc. $04 0.018; CrO, 0020. Group I1I—Detiled Analysis Preliminary Test for Group IIL: precipitate upon the addi- ‘on of normal zine nitrate to the filtrate from Group TT and boiling shows the presence of Group IIL. .A change in color of the solution during precipitation indicates that the ferricyanide nas been reduced. In such cases ferricyanide must be identified with the ferrous sulfae test im the filtrate before precipitating the group. There are instances when the ferricyanide will be reduced upon dissolving the sample, and such eannot be avoided by this scheme, 1 the preliminary testis postive, the treated with 0.8 to Og. of solid Sodium carbonate, and the Jeroup is’ precipitated completely with zine nitrate in excess, bcated to boiling, filtered, and washed twice with water, and then fecrocyanide. ‘Separation and identication of cyanide and borate: ‘The group precipitate is treated with 12.5% acetic acid on the filter and ‘washed. The acetic acid solution is treated with 6V ammonium hydroxide and ammonium polysulfde, acidified with hydrochloric acid, boiled, and filtered, ‘Cyanide is identified in the filtrate by the formation of a red ‘coloration upon the addition of 10% ferric nitrate. \Tocume, “Detection of citrates and tartrates (and malates).” F-Chem: Soe, 90, 818 (1900). Dipindai dengan CamScannerDipindai dengan CamScanner