TELAH DIPERBAIKI 06 OKTOBER 2020 BUKU INI TIDAK UNTUK DI PERJUALBELIKAN UNIVERSITAS SUMATERA UTARA FAKULTAS MATEMATIKA DAN ILMU PENGETAHUAN ALAM PROGRAM S1 KIMIA LABORATORIUM KIMIA ANALITIK PRAKTIKUM KIMIA ANALITIK | : JOYS ALISA ANGELINA HUTAPEA + 190802108 + UNIVERSITAS SUMATERA UTARA + S1KIMIA : ARDHA MULYANINGSIH 29 SEPTEMBER 2020 : REAKSI PENDAHULUAN KATION GOLONGAN |' Date: BEB\ NAMA + JONS A.A. HUTAPEA NIM ‘ (90802408 FAKULTAS /JURUGAN + MATEMATLFA DAN Tum PENGETAHUAN ALAM /SL-tCOMTA LABORATORIOM /PAEMER: ARDHA MULYANINGSIH. WART /TANGGAL PERCOBAANY: SELASA/29 SEPTEMBER! 2020 ol a ral 0D O CT) | om percopann | REAKSL PENDAHLLAN KATION EOLONGAN T | Towan Percowsn | Untwle mergetoltui tation - kation yang termasule a gplowpn 0 = Untuk margetdhui reatsi— reaksi dan sigat Ratton O Golorgan T . © _|=_uatus_mergetahur Hasglest tahon goloyan O 7 D |nav oan pawn [Dt Ala O | — Tatura, realesi - OT fe Rae Glug rallsi a Peep taburg Q | — Bunsen = - Korek api YQ = Tse oO T-2. Satan _ Dipindai dengan CamScanner Dipl degen Camscarer| ta ) [ENG tag) NOK oy — NarSa03 (04) = Tay = Ya. Oy oy) NaOH any = Aa NOs ayy - PolNOs TINAVAN RUSTAKA __fpenvtirg_dalam avalisis Fualitatie , yatta pe— Pemniathan dan Tdentigikas: Ada dua _aspek hrisaton dan idefticikast . Kedua aspect Ailandasi deh \elaraian, keasoman dan ke- ) Foasaan , penloentutean senyawa Komplete , Oo isidasi_redulsi_, sigat wudah tenguap oe sorta akstralsi . 4. Pomisanan. 5 Katio. — GB Fation yang aban ciarolists_, perla_di_- i pisahkan seca sistematie . Katia - kation J int_diteagi dalam golongan - gelorgan_dan | |selanuunya_dtoagi werjadi_Farporennyar | Recdascrkan peroedaan sitat_timianya dalam 1 asam Kloridy dan YaS sebagai Pereates Qo” golongen , katin ~ Kation dlodgi dalam lima & goloraan_, yfity +. Golongan 4 5 Agt — ul Dipindai dengan CamScannerDato: Rerbaitean ALAT daN RAMAN |W. b Alat (1) wie ONT Talalng ‘reas = pyroe Gare Ra taloury veal - ee eh | Bunsen = ~ HE APY SH costo rR ah -_ _F Panjopt tala - = L Tasue _ = rb Seber = 7 UO OU OS ;LU i! |HO op aigle dlojololo|o gocceep\ Pbo* at a, clon in ‘| al ig mT cu or a 2 ee st 3, Gdogaa TM tert Feat ADT, Get, NIM, Cot Mat 4ne. 4-Gclayan W, Ga, Sr™% Pye. S- Golorgan V, Mop, Nat, 1h, NMA”. Tdenti¢icasi . Setelah in - ton dtpigahtan , ion= ton porlu_diidentigras: untule wreualeinkan ebormdaan tor tenet . Hal ini dilakukan ‘[derman ongaunat-an _renesi identigtcast fealsi pengenal_, atau venti penentuan : _|Pengenalan ini clapat dilakukan dengan_* Ja. Wama ; warra larutan misalnya + Untuk srongidentigirasi_ddanya ion Fee" gla \arutan | diver lautan SCA™ akan senabasillean Fest Hp leerwarna merah . b. Remogkukan _enddtpan atau elanttur erdapan . Untuk tenentukan adanyp tm Po** tartan dive asam Ya ever. ferdagan_pulth PoSO4 terventule yi terdlapat Rutt. c. Erdayan yorg, torwama. Tor Na * Peer a A rovasikan endaan Ava Atamlaah _pereaksi 2-urani acta. a. Adcorpsi 2a Wama - Pada _pawarraan ‘eect digueakan Peinsip | ladsorpet Padi proses ini serat test didertcin tordan , Sperti aluminium bidroksida dan =" bvergatnuira, dergan ‘aware. ohne Ghia, 2042), Dipindai dengan CamScanner ips degen camscarnee\o\o\0 ano OW’ Ooo Date: Renguiuiran avoiiic gada_dawaraya adalale Subj kekidakpastian divnara_lvertangai_ jews paruimpangan (eecalaran) dayat_mureal dan hoi turgein Aertutp hinge Carag vary \eartoady~ lbeda . Bantan Kelika pemoawan instumen duup atu, Pengueamin larg davi_Sannper fimnloal, Rear uum Unt ang utatr has yar me nutnnparg dengan jummlah yang Wervari asi don Katy sara tain dan dar nat yang Wena dan camper. Sebelum ‘eroagai semis Penyimpangan dratoarcan | secora Terpennci , beberapa istlan || xiting hans dipertinlangkan. Dalam Emin | OC [ U i lanalitis., Stila galt (diguratan dalam ach | eviasi) qiderenisica deh perkedaan anor OW rasil tvs [xtest) dan nilat seoerteny (xtrue) | INilai regerensi gin ditenea 618957; FLENING | 119943, Tsk ini mungtin erkaitan Unhak | Hwerduleur otal 4 don araltis Mat x yay sosvai salu Sawa lat menurat folctor sense. | vitos 0 dan prosedur analihs . Menuruk ka~ Gio{a(o[a olololo Tal fatter dan besarnua , Aenis - Jenis_penytmn ~ _fpargan berikub dapat Atbedatan + Penyin — parqan ACak atau Kesalahan reroulacin pang, Wervlary —ulang dan _perulin Mgan_Stemats latau Rxalahan re aantitan oa Oiee Maus ; 200) Dipindai dengan CamScannerDate: | 4 | | Lida alektroda celektie ha tar electroda 4994). | OL Kidatc Atpertionloang kan . Halver_dan Cleenonsiewice O adalah yang, perkama worgamas adany ing ~ | OL laxpan potensdt teeradap peniodran attivttas toy} ey t 20. Meteka_ |), O pada_dekade perorna aoa e a] Krenemuban balwon veborapa jens Kaccmatcr oO, frctopicah forerst clekteda sbagat twgtat fe- O asatran dani solusi Forme vewlath . Secara oO] strikraral, tegatgan yang dteembaarg ban. anya Oo doyat diulcuc Moroqunatcan instrumon dengan ed tesistensi_ Masulean Varn foe reroatas yan di- O eout dlekrostat. temudiin , gerelitian yang is _[intensi€ mula’ wenyingkapkan alasan pembentukan Oo potancia\ vty . Sehuburgan dengan berloagat_feno- O —_ frora Donran varq Aiperteratikan pda decade | oO kedua_avacl ine , Warm hubungan yang Melibat- | oO kan yenyelaaran yang diloatosi_ untae tmen- O olakan swath sitem dimana sduah wombran O nemisalican Plough KolotA dan sclusi_ yang se= =e looramyp . Mula saat ini_, pores Wemoran | OC | fercatt doran dust a seluuh wembran . Tey © acetroda Sache yeeogarmrana deeoutican SJ Donvan adalah yang potkama nonyy\ican yon aa dekatan Teoritis untule fengganbaran pote nal oO yang ditetacan soda pparrataan (Séle ‘aw 6d, 1a = Dipindai dengan CamScanner ips degen camscarneeDate: ___ [becval_dai_neratconsume’_makanan Manus. wencampur (doin dai 20 Yo sreti werkud _|dtarmgap 0,02 pm Roda tranusia, séeagian Velar | | Merkuri tus vats dalam ete ranusi¢ in air minum. dari Suter — sumber ini, dan hanya sologran dan Torkati wernt dalam makanan dan _sektar 1S % dalam’ ar. Knconterasi nortan’ dal am romout dan darah diqunatan. weagai irakkaton _(Asuyan_werkurt_ dan boar tubuh . Menunt WHO, kadar neteun dalam dara dan vamiut yang | rot porta tercargenterasi di_rati coin ginpl | dengan $0-45°%> Ai oak. Roda wanusia_, tet nereuri lebih orceun danpada tett anerganit. Karena at polanut Wp yong lebin_toesar_yang __[tremurgintcan logan atta tronyolorerg Memloran Jovologi \eth trudah , Yeutama ke dla otak, Icora_, “ula ealakag_ dan saree Yepi_ can ge- fluc plasertin. Merturi ivorqanie _terteosenterasi dalain gral manusia don nelatakan eek utony ny _doara . Keraaunan Net ween fenyetatn Ikan ganguan Yenranen pada Sotem saaE. . Hol ini netyoloatekan_tehilangan SRISAAK Pada arojgetn. twain» Alle mertur dtahan ci Lperan oak untié vodloa. yang tama. Apek hargerat: nongialangi placenta Stora 8. ; 202 Dipindai dengan CamScannerDate: o | Keocdirasi Karnin golorgan I dencgin ieteleyen oO retral didominasi oleh \gan_donor_olaigen Rect s O alcool eter, dana, termasule Yang mana CO Tratkora, eter dan Gyptards yang Seting at - O - gueakan sekagai_ligan_tehadap elompol. CO [Ration T. Proses Emin Yaw Verhuloungan oO deren Pouea maket yor eran bopigat OO elekteno_, Furarg felt - Komplel® é& gang_tidale CO bia alae foods’ Nat UA 4 | oO —__ fawetit- 14,7 Ariasasdere). Komplete “ye Ol] __ parang wal Fada awalnyr tei@tir decay Le) | —Heduan dan’ tedlai Nal@r} dengan S20 SG, oO]. _|AU_depan odanup_sfttus doror_, renujn fee © staan _potersial_untub eleleropasiss cairan O —__|Supertssitis (SCFED) dari akan semi tordubhon OC Nat lebih Menyytai dikeordinastean dengan O Sklus_takwida Kl = doror Grup yarg_le- ) bin wort | alll waskipan Seyumlaly Foor © Nrontin Nergfin Yang berungsé Woagpi N= perdoror oO Hiketalui_tomboertuk Fanplets dengan alleati oO loam, Complets dan Makpdoror Tetral a dengan ation Ti Saroat sedlet untuk =) di pelayari doripada pal Relay arn scloolumnja © (nets ow. research gate . ree /palolicat'on / © 179304054 A%O_ macrmcylic_canper_og gap) — Dipindai dengan CamScannerDates ___— w PROSEDUR PEECOBAAN| | Ay “= A. Tatura, T CO - Dimasukkan AgNOs teddlam tabury reali CO — Dtamioahkan HCl © = Diamnati penioahan yang teyadi O fe. Vatourg, oO = Dimasuikkan AgNOs kedalam tabuney realest O —_ Dtamoahkan Hel CO = Diamati peruoahan yarg teat O ~ Ditatalahtan Ntia OC _|= Diarati_gerutaran yar tetjade J |e. Tabury Wo os) {= Dimasutkan AgNOs tedalam ibang cents’ OC — Ditambahkan NaaSo0s OC _|= Diamati_peruboban yey tena oO Dow O - Dinrosuiekan AgNO: kedalam ‘tury reales CO ~ Daambahtan #2 (rO4 O = Diamatt penbahan yang terpadt © &- Tau Z O —_Dinwsutcan AgNO; Kedalam tabung reaksi O = Ditamlahtan NaOH C — Dramas perloahan yard fejadi Oo F. Tawny 1 : GI - Dirrasuickan AgNO; tedalam tatoury tears Dipindai dengan CamScanner ips degen camscarneeal - Dtameankan Kt @_) t Damati peruoahan yang terjadi O Oo ln. Pb? = A- Tabung T @ — Dinusulekan Po(NOs)2 Fedalary telouny reali © = Dtomteahkan Wa O —Viamati_peruoaran yang terjadi CO B. Toloury T : oO — Dinasutekan PoLNOs}s Kedalam talouiny reast oO ~ Dxtamtonhkan HO (es) |= Diamati_feruvaran yang tejadi = Digaraskan datas nupla bancen J - Diamati_perdloaran yan terjad CO Cc. Tau oO — Vinasukkan Pb(N0s). kedalam tnlung recitsi Oo - Qitamoahean KL es) — Tiamat peubaran yang ter aa CO 0. Tow W © = Dimaculckan PbINOs)» kedalam tabung rarksi oO — Ditamoahkan telrDa © - Diamati perbahan yang terjadi an) - Tatu V (= - Tiracuekan PoINO,). \edalam toaing reabsi © - Oitamloahtan 12804 — Dipindai dengan CamScannerDate: _Fdlamati_perubahan yang terjadli |F. Aabung Wo _ Ditnasutekan Po(NOs).Yedalam tetoung reali | |e Ditantcahtan NAOH | — Diawati_porb atin yang rer : Dipindai dengan CamScanner Dipl degen Camscarerwr : | 4. Agt 4. + WG + HNO: ) AgNOs wd > Mis, 5 4a > Myily ; \ My patil, \ fo) Agqdh +antiqOh = AgINHs CY + 2t20__ larudan yerin | Aggl Na 20K Ay(NWs)a + 280 \autan Jini C)_WyNOs + NasS:03 > AyaS0s 4 + 2NANOs Putt eaning -Cokdot -hitam [Ait + OF A605 4 pata Keun, = Welge -hitam No, + KOK . OIKNO. {o) 24,No: + Or Pye LOra + 28 ue ul! yt + C7 —> Ay alrOh us worah bata é) 2AgNOs + NadK yO a + 2NaNO, Foe IH = Ay. 2 F) AgNO, + KT > Ag hd + ENDS Faming, GEE Ee OOO 0)0 000 0\qo}\g\do\o\0 ! Dipindai dengan CamScannerDate: Oi | r J ) oo Rorlanttcan + iF T Rest EERO \ Aq ; Mook sR J le) tae a hy ai Ag Tm Ag ngs Aan Holelclalg|algwe _ JA} RbINOa)s + aNCA > PoC & tn Rte 7-7 PCa v futth ~{b) PoINGS). * aka = Pott 2HNOS ph “Ppl, — Po 2U-T> Phe. v Tarra gern, krittal garam [C) PeIND,), + IKE 7 Poly 4 2ENOs Funiny 7 Wort 4 21 > Poly Fung ‘|) PoINDs. + Kaley > PoCrO4 y + ISNDs kang Bort + GO? > PoCrO4 - eu TE) PULND,), +t Woy > PolDx Y_ + 2UNO, —— RR Re + 9042 9 PoSDae a iho ee +t 20H = 2 Rb(OH). a lO putih Dipindai dengan CamScanner ips degen camscarneems TECOBAAN 2. PU?* * #3038 {8} ‘Po(NOs). 4 ~~ pb. ot £ HN), § Poll: a> om 4 207 = aS Varun ernie a 0) feo’): # 2a ~ hed + 9ENO, 12 Gwenn Kinny telur owe 4217 Pola L unig fue see eee eee ee[ewe PUSTA A [Achmad Viskia. 2012. timia Anattie Kiunltabe. to Gal jetta. Todonesia + PT Cit Aaltya oO Batti. Halangn 1-3 Dato: Danzer, lous . 2007, Analytical Chemisty + Theove Vial_and Metrological fundamentals . Germany + Springer. Yalaman 65-66 Seiler Wan .G, dkke . 1444. Haidlook on Metale in Clinical aed Analytical Chemisry. New York: Martel Decker ‘Tre. Kalaman 40% -408 — [Sharir BK. 2006, Annlytiat Chamitry . Secerd Eaitvon . Meeiut . Krichna Rakashan Malu (r) Ud. Halaman 478 btkys / vow). researhaate , we /qublcation ee) 0109 AtO__ macrocyltc— complex _ OF gp Medan, 29 Septemveray Asisten Patian , dofojolg/oo|op}oo}ofp}ojacja|cgjaey (ARONA MuLvANINstH (Ys A.A. HUTAPEA) Dipindai dengan CamScannerlolclaloiolas Il Pocbaikan _ PORETAR ROSTALCA. Date: VAchmad Visa ADDIE tanta Andalite {Wott Edisi Pertama . Wloresia: PT Cin Miya | Rae Halaman £-3 —Treoretical_ard_Metralagicat Suramar — Germany: Springer. Page bs - 66 + Dangor , Claus, 2007. Analytion Chemisry : ‘(Seiler _, Han -@ , de 1994. Hardbook on Metals in Clinical anal Aralytcal 1) Chomirhy New York + Maret Detter Ine, Page sur -'05. Sharma, &, 6-206. Aralurtcal Chorney - © s+ Sownd Editon, Meerut: Krichina Yerbeahn Iolelolok 818 Media (P) Ltd. alalol ) ANE pet 8 yey Nets + // was, tesoarchgate «roe /pulication SOL O97 AO_ trace — Ngee = 9 “Arou | Asisten Medawn 29 September 200 Pakitan alololololala [lAepea. el Ss GUOgS Aan As ROTATEKimia Analitik Kualitatif AnalisisiKualitatif Konvensional fe nek Drs, vrs, Hise Achmad Mtns Dipindai denganHak cfpta yang olindung) undang uncang pada: Peegarang Hint Penerpitan paca; Penerot PT Gera Acrya Bak Cotakan Ko t wen 2012 No Wode Ponetaian =: 12KTOIT ‘Sebagianalau veluruhrya isi buku is dlararg Ogzraban ‘lau dperbaryak dalam bone apapun tanga Le Werte ri Penertot Cra Aciya Dah acu clara pongutipan untuk keportsan perutsan arth! ala harargan Brat Comptes vag, ayo oleh Peet CPTCITRA ADITYA BART) ISBN : 978 - 979 - 491 - 0: Anggota IKAP! Dipindai dengan CamScanner ips degen camscarneePengantar Analisis Kualitatit BABI PENGANTAR ANALISIS KUALITATIF Dalam imu kimia, salah satu aspek dari materi yang dipelajari ialah komposisinya. Kimia analiik adalah cabang dari iimu kimia yang mempelajari metode dan teknik untuk menentukan komposisi zal. Tentang komposisi dapat diajukan pertanyaan “apa dan berapa banyak". Dengan demikian, kimia analitik masih dibagi lagi sesuai dengan informasi yang ingin diperoleh tentang komposisi zat. Analisis kualltatif menjawab “apa yang dimaksudkan di atas”. Dengan analisis kualitatif dapat di- kenal unsur radikal atau ion yang terdapat dalam zat tunggal atau campuran zat. Sedangkan anall- sis kuantitatif dapat menjawab “berapa banyak jumlah unsur atau senyawa dalam suatu zat”. A. PENGEMBANGAN METODE ANALISIS KUALITATIF Motode analisis kualitatit “sistem HzS" mula-mula dikombangkan oleh van Bergman, komudian oleh Fresenius, Treadwell, dan Noyes yang didasarkan atas pengendapan sulfida dalam larutan dengan pH tertentu. Buku tentang analisis kualitatit karangan Fresenius, Qualitative Chemical Analysis, diterbitkan pada tahun 1840. Beberapa metode analisis kualitatif telah dikembangkan ‘untuk menggantikan sistem H2S, yaitu “metode natrium suifida” oleh Vortmann dan “metode fostat” oleh Remmy. Akan tetapi, kedua metode tersebut tidak sepopuler “sistem H2S". Pada masa kini sistem HeS jarang dilakukan dalam pekerjaan analitk karena telah digunakan analisis yang lebih copat dengan roaks|-reaksi totes. dengan berbagai peroaksi organkk yang seloktit yang dikembangkan oloh Fogel sorta analisis kation secara copat oleh Charlot dan Bezier (1943), juga ‘nalisis instrumen yang menggunakan alat-alat moder. Namun, dengan mempelajari analisis kua- ltatit, membiasakan mahasiswa mengenal reaksi-reaksi kimia serta mempelajari cara pemisahan yang merupakan dasar metode analisis modern. Selain itu, dari analisis kualitaif dapat dikembang- kan penalaran dan berpikir secara analitis }. PEMISAHAN DAN IDENTIFIKASI ‘Ada dua aspek penting dalam analisis kualitatif, yaitu pemisahan dan identifikasi. Kedua aspek ini ilandasi oleh kelarutan, keasaman dan kebasaan, pembentukan senyawa kompleks, oksidasi reduksi, sifat mudah menguap, serta ekstraksi. 1, Pemisahan Kation-kation yang akan dianalisis, porlu dipisahkan secara sistematk. Kation-kation ini dibag! ‘dalam golongan-golongan dan selanjuinya dibagi menjadi komponennya. Berdasarkan perbedaan Kira Anaiitk Kualtatt 7 Dipindai dengan CamScanner ips degen camscarneeiat kimianya dalam asam klorida dan HeS sebagai pereaks| lima golongan, yaitu: Golongan! Ag’, Pb**, Ho®* ou Golongan ll: Pb, Hg?, Cu*, Gd, Bi?*, AS, AsOs™, sb Sbox®, Sn?*, Sn* Golongan Ill : Fe, Fe, AIM, CP", Ni, Co**, Mn®*, Zn®* Golongan IV: Ca®*, S?**, Ba’? | GolonganV: Mg”, Na’, K*, NH&* Dari kelarutan garam-garam dapat disimpulkan aturan kelarutan seperti yang i golongan, kation-kation ibagi dalam dibahas di bawah ini. Aturan Kelarutan Kelarutan garam-garam dalam air adalah sangat penting dalam analisis kualitatit. 1. Semua garam klorida, bromida, dan yodida melarut dalam air, kecuali garam timbal, perak, dan merkuri(!). Garam merkuri(ll) yodida tidak melarut dalam air. Timbal klorida melarut dalam air panas. 2. Semua garam nitrat, nitrit, Korat, dan asetat melarut dalam alr. 9. Semva garam kalium, nalrium, dan amonium melarul dalam air, kecuali (NHs)2PICle, KoPICle, KHCuH«Os, KaCo(NOz)s, NazSiFe, dan NaSb(OH)s agak sukar melarut. 4. Semua oksida dan hidroksida tidak melarut dalam air, kecuali oksida dan hidroksida logam alkali. Sedangkan oksida dan hidroksida dari barium, stronsium, dan kalsium agak melarut dalam air, 5. Semua garam sulfida, kecuali sulfida dari unsur alkali dan alkali tanah tidak molarut dalam air. 6. Garam sulfat dari barium, stronsium, dan timbal tidak melarut dalam air dan asam. Kalsium ‘sulfat sedikit melarut dalam air. Garam sulfat yang lain melarut dalam air. 7. Semua karbonal, fostat, borat, oksalat, kromat, arsenat, heksasianoferat(til), kecuali garam alkali tidak melarut dalam air atau sangat sedikit melarut dalam air; CaCrOs dan MgCrOs agak melarut dalam air. Garam ini melarut dalam asam encer. 8. Semua sianida tidak melarut dalam air, kecuali sianida dari logam alkali dan merkuri( Il). 9. Kecuali garam logam alkali semua silikat tidak melarul dalam air, 2. Identitikast Selelah ion-ion dipisahkan, ion-ion perlu diidentiikasi untuk meyakinkan keberadaan ion tersebut. Hal Ini dilakukan dengan menggunakan reaksi identifkasi, reaksi pengenal, atau reaksi penentuan. Pengenalan ini dapat diketahui dengan: : Dipindai dengan CamScanner ips degen camscarneea. Warna ‘Werna larutan misalnya: 4) Untuk mengidentikasi adanya ion Fo®, jka larutan diberi larutan SCNT akan meng- hasilkan FeSCN** yang berwama merah. 2) Untuk menentukan adanya ion Mn®*, larutan diberi pereaksi HNOs dan NaBiO3 kemu- dian dipanaskan sehingga akan memberikan warna ungu karena terbentuk MnO« yang berwarna ungu. Pembentuken endapan atau melarutnya endapan 4) Untuk menentukan adanya ion Pb**, larutan dibori asam H2SOs encer. Endapan putih PbSOs terbentuk jika terdapat Pb". 2) lon Pb®* dapat juga ditentukan dengan ion CrOs?_ yang menghasilkan endapan PbCrOs. Endapan ini melarut dalam larutan NaOH (e Endapan yang berwarna | 1) lon Na* menghasiikan endapan jika ditambahkan pereaksi Z-uranil asetat. 2) lon Ba** dan lon S?** menghasilkan endapan kromat yang berwarna kuning. @) Adsorpsi zat warna Pada pewaraan tekstil digunakan prinsip adsorpsi. Pada proses ini serat tekstil diberikan. | mordan, sepert aluminium hidroksida dan mordan akan bergabung dengan zat warna. Ga- bungan ini disebut “iake*. Pada analisis kuantitatif prinsip ini digunakan untuk menentukan beberapa ion, misalnya: 1) AK(OH)3 dengan aluminon menghasilkan wana merah. 2) Mg(OH)2 dengan magneson menghasilkan warna biru. 3) Mg(OH)2 dengan titan kuning menghasilkan warna merah jambu. Cara yang Lain Setelah ion bromida diubah menjadi brom, dalam pelarut kloroform brom berwarna cokelat. Sotelah ion yodida diubah menjadi yod, dalam pelarut kloroform yod berwarna ungu. {on nitrat ditentukan dengan reaksi cincin cokelal. C. PRINSIP KIMIA DALAM ANALISIS KUALITATIF Prinsip-prinsip kimia yang mendasari penyusunan skema kualitatif termasuk aspek pemisahan dan identifikasi, yaitu kelarutan, keasaman dan kebasaan, pembentukan ion kompleks, reaksi redoks, silat penguapan, dan ekstraksi. ‘Kimia Anak Kualitatit 3 Dipindai dengan CamScanner ips degen camscarneeK. Danzer a V, Aen tse % 2 pee BN! g Springer‘Am Friedensberg e-mail:clausdanzer@jetzwebde LUbrary of Congress Control Number 2006932265 ISBN-10 3-540-35988-5 Springer Berlin Heidelberg New York ISBN-13 978-3-540-35988-3 Springer Berlin Heidelberg New York DOI s0.1007/b203950 This work Is subject to copyright. All rights are reserved, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of ilustrations recitation, broadcasting, feproduction on microfilm or in other ways, and storage in data banks. Duplication of this publication or parts thereof is permitted only under the provisions of the German Copyright Law of September 9, 1965, in its current version, and permission for use must always be obtained from Springer. Violations are lable to. ‘prosecution under German Copyright Law. ‘Springer is a part of Springer Science+Business Media (espe vag Brin Heebery SSA The use of general descriptive names, registered names, trademarks, etc.in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. Product liability: The publishers cannot guarantee the accuracy of any information about dosage and appli- cation contained in this book. tn every individual case the user must check such information by consulting the relevant literature. Cover-Design: WMXDesign GmbH, Heidelberg Typesetting: PTP-BerlinProtago- 7X Production GmbH, Germany Production: LE-TX Jelonek Schmidt & Vockler GDR, Leipzig, Germany Printed on acid-ftee paper 2/3141/¥L-543210 Dipindai dengan CamScanner ips degen camscarneeBoth qualitative observations and quantitative measurements cannot be re- produced with absolute reliability. By reason of inevitable deviations, mea- sured results vary within certain intervals and observations, mostly in form of decision tests, may fail. The reliability of analytical tests depends on the sample or the process to be controlled and the amount of the analyte, as well as on the analytical method applied and on the economical expenditure available. 41 Reliability of Analytical Observations and Measurements Analytical measurements are fundamentally subject of uncertainty where various types of deviations (errors) can appear and these may be influenced to varying degree, Even when instrument readings are sufficiently accurate, repeated measurements of a sample lead, in general, to measured results which deviate by varying amounts from each other and from the true value of the sample. Before the different types of deviations are characterized in detail, some essential terms have to be considered. In analytical chemistry, the term error (used in the sense of deviation) is defined by the difference between the test result (Xie) and the true value (Xrue» ie., the accepted reference value, see ISO 3534-1 [1993]; FLEMING et al. (1997). The term may be related both to measured value y and ana- lytical value x nding to the sensitivity factor b of an analytical procedure. According to their character and magnitude, the following types of de- viations can be distinguished. i indom deviations (errors) of repeated measurements manifest them- selves as a distribution of the results around the mean of the sample where the variation is randomly distributed to higher and lower values. The ex- pected mean of all the deviations within a measuring series is zero. Random deviations characterize the reliability of measurements and therefore their precision. They are estimated from the results of replicates. If relevant, it is distinguished in repeatability and reproducibility (see Sect. 7.1) Dipindai dengan CamScanner ips degen camscarnee66 4 Statistical Evaluation of Analytical Results Systematic deviations (errors) displace the individual results of measure- mmient one-sided to higher or lower values, thus leading to incorrect results, In contrast to random deviations, it is possible to avoid or eliminate system- atic errors if their causes become known, The existence and magnitude of systematic deviations are characterized by the bias. The bias of a measured result is defined as a consistent difference between the measured value Jhesr and the true value Yrrue? bias(y) = Yiest — Yirue (4.la) The absence of a bias characterizes the accuracy of a measured result. The same holds for the analytical value: bias(x) = Xess — Xtrue (4.1b) Outliers are random errors in principle. However, they have to be eliminated because of their disproportionate deviation, so that the mean will not be misrepresented. Gross errors are generated by human mistakes or by instrumental or computational error sources. Depending on whether they are short- or long- term effects, they may have systematic or random character. Frequently, it is easy to perceive and to correct for them. They will not play any role in the following discussion. The relation between systematic and random di tions as well as the character of outliers is shown in Fig, 4.1. The scattering of the measured values is manifested by the range of random deviations (confidence interval or uncertainty interval, respectively). Measurement errors outside this range are described as outliers, Systematic deviations are characterized by the relation of the true value p and the mean ¥ of the measurements, and, in general, can only be recognized if they are situated beyond the range of random variables on one side. Conventionally, a measured result is said to be correct if the true value is situated within the confidence interval of the observed mean (1, case 1 in Fig. 4.1). If the true value is located outside of the range of random deviations (pp, case 2 in Fig, 4,1) then the result is incorrect, fe M ¥ Outlier Intervall of random deviations Fig. 4.1. Schematic representation of systematic and random deviations Dipindai dengan CamScanner ips degen camscarneehandbook rea METALS IN CLINICAL AND ANALYTICAL CHEMISTRY lero Mae RCM og Astrid Sigel BL ellehandbook on METALS IN CLINICAL AND ANALYTICAL CHEMISTRY exited by Hans G. Seller Helmut Sigel Institute of Inorganic Chemistry CH-4056 Basel, Switzeriand Marcel Dekker, inc. New York*Basel*Hong Kong Dipindai dengan CamScanner ips degen camscarneeLibrary of Congres Cataloging-in-Publication Data Handbook on metals in clinical and analytical chemistry / edited by Hans G. Seiler, Astrid Sigel, Helmut Sigel. Pp. cm. Includes bibliographical references and index. 1, Metals—Analysis, 2. Clinical chemistry. 1, Seiler, Hans G. ‘W3-39154 cr ‘The publisher offers discounts on this book when ordered in bulk quantities. For more information, write tw Special Sales/Professional Marketing at the address below ‘This book is printed on acid-free paper. Copyright ©1904 by Marcel Deter, I) All Rights Reserved Neither this book nor any part may be reproduced of transmitted in any form or by any means, electronic or mechanical, including photocopying, microfilming, and reconding, or by any in- formation storage and retneval system, without permistoa ia writing from the publisher Marcel Dekker, Inc. 270 Madison Avenue, New York, New York 10016 (Current 987654321 PRINTED IN THE UNITED STATES OF AMERICA Dipindai dengan CamScanner ips degen camscarnee7 lon-Selective Electrodes. Part I: An Overview Erné Pungor Institute for General and Analytical Technical University of Budapest Gellért tér 4 H-II11 Budapest, Hungary 1, HISTORY OF ION-SELECTIVE ELECTRODES 107 2. THEORY OF ION-SELECTIVE ELECTRODES 108 2.1. Donnan’s Theory 108 2.2. Nikolsky’s Theory 108 3. STUDIES REGARDING THE FORMATION OF THE ELECTRODE POTENTIALS 109 4. INTERPRETATION OF THE OPERATION OF ELECTRODES un Working Mechanism a REFERENCES 3 to account {4}, namely, that hydrogen ion sensitive glasses responded also to sodium ions at low hydrogen ion and high alkali ion activity (i.e., in alkaline solution). In a most ingenious way, Nikolsky 107 Dipindai dengan CamScanner ips degen camscarnee108 PUNGOR interpreted the phenomenon in terms of ion exchange and introduced the concept of the selectivity coefficient. By this concept most phenomena connected with the selectivity on ion-selective electrodes can be explained. Nikolsky’s results initiated an extensive research with attempts to use inorganic and later on organic ion exchangers as electrode active materials, but without success. Earlier studies on theoretical thin membranes were continued by Teorell [5] and Meyer and Sievers [6], who in their theory attempted to interpret the behavior of practical, thick membranes, in contact on both sides with solutions containing the sort of ion which can produce a membrane potential. This initiated further research and many workers studied the perm-selective properties of ion-selective electrode membranes. As a result, ion transport across thick ion-selective membranes was considered as the basic concept of the theory of ion-selective electrodes. This theory was further elaborated by Eisenmann, Simon, and Buck. In the 1950s I studied the adsorption properties of silver iodide in the laboratory of Professor Schulek. This work later gave me the idea that the chemisorption of iodide ions on silver iodide precipitate could serve as the basis for the operation of an iodide-sensing electrode. Indeed, silver iodide embedded in paraffin became an ideal ion-selective electrode [7]. This electrode was later used to study the origin of the selectivity of precipitate-based ion-selective electrodes, and in the 1960s to show that the defect structure of the crystal only affects the standard potential (Eq) of the electrode. In the mid-1960s Simon and his coworkers [8] began to use complexing agents for preparing ion-selective electrodes with great success. Membranes incorporating large lipophilic molecules produced the expected theoretical response to ion activity changes. 2. THEORY OF ION-SELECTIVE Since a gel layer is formed on a glass surface soaked in an aqueous solution, this approach seemed to be applicable to describe the behaviour of glass. electrodes. 2.2. Nikolsky’s Theory In his ingenious concept Nikolsky [3] explained the effect of interfering ions on the response of ion-selective electrodes in terms of an ion exchange equilibrium. From this consideration came the following: £= + Ting, + Kw) where K is the selectivity coefficient, a, is the activity of the ion to which the electrode responds, and b, is the activity of the interfering ion. In view of the diffusion theories it was assumed that K is affected by the mobilities of the ions in the membrane, thus the potentiometric selectivity, K™ + K, but K™ = m - K, where m is the ratio of the mobilities of the two competing ions in the membrane or a more complicated function (see Eisenmann [9]). K™ is the coefficient to be inserted into the Nikolsky equation. Before the 1960s there was no way to study the physical meaning of the selectivity coefficient in a quantitative manner, but then the Agl-based iodide electrode became an excellent model to study. We investigated the selectivity properties of the electrode in the presence of bromide and chloride ions and found the selectivity coefficients to be the ratio of the solubility products of silver iodide to that of silver bromide and silver chloride, respectively. In addition, the selectivity coefficient did not involve any factor connected with ion transport. Dipindai dengan CamScanner ips degen camscarneeAYER Chemistry Comprehensively Covering the UGC Syllabus) Ae OT Dipindai dengan CamScannerANALYTICAL CHEMISTRY (For Honowrs, Post-Grodwate, BE and B.Tech Students of Various Universities) (COMPREHENSIVELY COVERING THE UGC SYLLABUS) Dr. B. K. SHARMA Reader & Head DEPARTMENT OF CHEMISTRY N.A.S. COLLEGE, MEERUT SPECIMEN $ iio KRISHNA Prakashan Media (P) Ltd. MEERUT *) DELHI Dipindai dengan CamScanner ips degen camscarneeANALYTICAL CHEMISTRY First Edition : 2005 Second Edition : 2006 This book or any part of this book thereof may not be reproduced in any form without the written permission of the publishers and author. Co-author ; Piyush Sharma Edited by : Manjula Sharma Ankur Sharma LS.B.N. 81-8283-022-2 Book Code No. 298-2 Price : Rs. 250.00 Published by : KRISHNA Prakashan Media (P) Ltd., //, Shivaji Road, Meerut Ph: (0121) 2642946, 2644 Fax: 0121-2645855 C0: 2/11, Ansari Road, Darya Ganj, Delhi-110002 Ph.; (O11) 41563457-459, Fax: 91-11-41563460 Website: www.krishnaprakashan.com e-mail: sk_kpm@yahoo.com ne Pree Abe: ‘Apar Computers, Mayur Vihar, Meerut. Ph: 0121-3296334 Vial Offset Printers, Meerut Ph.: 0121-2641770 Dipindai dengan CamScanner ips degen camscarneeRie ‘ANALYTICAL CHEMISTRY (a) High solubility in lipids. (b) High penetrating action in cells because of higher solubility in lipids, which is about 100 times greater than in water. «(c) Inhibitory action on enzyme systems, and (d) High absorbance in cells. ; In humans, methyl mercury is more toxic than inorganic mercury, because of its greater lipid in the human kidney and exerts its major effect Methyl mercury poisoning leads to permanent of the nervous system. It causes sensory loss in limbs, Joss in hearing and mental retardation, mercury gets retained in the brain for periods of time, The most dangerous has eee she SAY of for moving through the placental barrier and to enter foetal tissues. Higher concentration of mercury causes chromosome damage and interferes severely with the process of heredity. Methyl mercury poisoning also leads to the segregation of chromosomes, chromosome damage in cells, DNA breakage and inhibits cell division. It causes energy defi- ciency in brain cells and disorders in the transmission of nerve impulses. Thus the babies born to mother subjected to methyl mercury poisoning have been reported to suffer from cerebral disorders and convulsions. Alkyl mercury compounds bind to proteins and hamper their normal biological activ- ities. At most severe levels, sour mouth, inflammation of kidneys, chronic irritation of pulmonary tract and malfunction of brain occur. Severe exposure to mercury vapour produces pains and tightness in the chest, difficulty in breathing and coughing followed by headache and sleepless- ness. Muscular tremors are the signs of milder mercury poisoning. Attachment of mercury to cell membranes inhibit active transport of sugars across the membrane and permit the passage of potassium to the membrane. However, extreme toxicity of mercury poisoning was recognised as Minamata disease. Methyl mercury has been found to enter the food chain through plankton and gets concentrated by game fish by a factor of 10* when it passes up the food chain. The major effect of methyl mercury involves neurological disturbances, The most common features of methyl mercury poisoning include. (a) Parasthesias (numbness and tingling). Dipindai dengan CamScanner ips degen camscarneeAccess Article. Published on 115 JUNE 21>. LOwmORUEG On Zt IU aN? 17 -60K. [RQERRIND once ended Cre Comin Aaron 30 Unpned iense, Dalton Transactions ‘Cite thi Daton Tans, 2018, 44 13453) Received 18th May 2015, Accepted 15th June 2015, 0}: 10 20397esa01865) woemncorgiton “Chemiaty, very of Southampton Mighell, Southampton, S017 1, UK mal (etd ae wt Perera Aza-macrocyclic complexes of the Group 1 cations — synthesis, structures and density functional theory study+ John Dyke,” William Levason,* Mark €. Light." David Pugh.” Gil Hanusha Bhakhoa,” Ponnadurai Ramasami? and Lydia Rhyman” ‘The Group 1 complexes, (M(Mes[18laneN)|BA/ (M « LI~Cs: Megl1BlaneNe » 1.4,7,10,13.16-hexamethy 1.47.10,1516-heraazacyclooctadecane; BA" = tetrakis(3.5-bistriluoromethy()-pherylboratel, are ‘obtained in high yield by reaction of the macrocycle with MIBAM'] in anhydrous CHCl solution, and characterised spectroscopicaly (1H, "C('H),’L, #1Na, and "Cs NMR), by microanalysis and, for M = LK. ‘and Rb, by single crystal X-ray analysis. The structures show Ny-coordination to the matat ion: the small onic radius for Li" leads to a puckered conformation. In contrast the K* jon fis well into the Ny plane, with the [BAP] anions abowe and below, leading to two K" species in the asymmetric unt (a hexagons planar [KiMegI18]aneNjI* cation and a TkiMec|18laneN)ie!-BAr)” anion’, with long axlat Ko-F intr= {actions}. The Rb" jon sits above the Ng plane, with two long axial Rb F interactions In one cation and two ong, mutually cis Rb-F interactions in the other. The unusual sandwich cations. IM(Mestacni:!* (M = Na, : distorted octahedral, Ne donor set) and hall-sandwich cations [LiiMestacrtth (distorted tetrahedron. NO donor set, [LMeycycen)(OH;I". and INalMe,cyclenithf|* both distorted square pyramids with [NO donor sets) were also prepared (Metacn = 1.4,7-trimethy\-1.4,7-tiazacyelononane, Megcycien 14,7.10-tetramethy\-1,47.10-tetraazacyclododecane). Density functional theory (OFT) calculations, using the BP86 and BSLYP functionals, show that the accessibility of the (M(Mestacn);!* sandwich cations ‘depends strongly on the M" ionic radius. such that tis sufficiently lage to avoid stenc clashing between the Me groups of the two rings, and small enough to avoid very acute N=M-N chelate angles. The caleu- lations also show that coordination to the Group 1 cation involves significant donation of electron density {rom the p-orbitals on the N atoms of the macrocycl, rather than purely electrostatic interactions lam (14,8, btetrar including structural characterisation of the sandwich cation salt, [No(Me,tacn),[BAr"] (BAP = tetrakis3,5-bistrifuoro- methyl)phenyl)borate) and [Na(Me,cyclam)(thf)[BAr’], con- taining tetradentate coordination of the 2 The reparation of several *amputaonal Chemistry Group, Department of Chamitry, Faulty of ene, ndversy of Maurin, Red BOE, Mauris 1 ectranie supplementary formation (ES!) wallble: Xe ereaographie Parameters and ef ies for the compen reported (Table $1), ertallographe ita i EP format, together with fal DPT computsional detail using bth the PSG and MILYP functionals Tables 52-530, Fig SI-S5} CCDC 1081099-105110, for ESL and cystallgaphic data in CHF or other electronic format we DOL Hesarnesdo1ses) Ths urls © The Royal Socety of Chem 2015 id we attributed this unusual behav- four to the low lattice energy of No(BAt"), coupled with the hhigh solubility of the (BAr"]- salts in non-competitive, very ‘weakly coordinating solvents, such as CHCl, and toluene. Neutral diamines (eg. N,N,N,N'tetramethylethyt- {enediamine) are often used as complexation agents to increase the reactivity of alky! lithiums? and to increase the solubility of aston Tans, 2015, 44, 13855-15866 | 13853 Dipindai dengan CamScanner ips degen camscarneeg $ Aaticle. Published on 18 June 2015. Downloaded on 26/10/201 ‘Ths atcle Hcensed under a Creative Cammonn Atibution 3.0 Unported Licence a Earler wo = ccles are more stable towards electrides compared to the ana- ogous crown ethers." Other than the two Na’-aza macrocyclic complexes that we reported," four examples involving Me,tacr coordinated to lithium are known: two lithiurbased elec trides, a BzLi complex with Mestaen and a lithium enolate stabilised by Me,tacn.” Two sodium complexes with Me,tacn and Me,eyclen (1,4,7rimethyl-t4,7,10-tetraazacyelododecane) ‘were structurally characteised."” No examples of neutral tri- and tetraaza macroeycles are known for K’, Rb’, or Cs' and there are very few examples with the Nemethylated aza ana- logue of 18-crown-6, Me,{18}aneN, (1,4,7,10,13,16-hexamethy!- 14,7,10,13,16-hexaazacyelooctadccane)."* The enya struc- tures of two electrides, [k(Me,[18}aneN,)}’Na~ and [Cs{Me,[18} aneN,]'Na", were determined by Dye and coworkers," who also reported NMR spectroscopic evidence for [Rb(Me,[18} aneN,)J'Na", [Cs(Me{ts]aneN,)]", [Ca(Mes{1s}aneN,):|", and two [Cx(Meq[18}aneN,)rown)}" complexes." We report here the first systematic study of the synthesis, spectroscopic, and structural characterisation of Group 1 cation (Li to Cs') complexes involving tr, tetra: and hexa-aza rmacrocycles. Density functional theory (DFT) with the BPE6 and BSLYP funetionals has been used to investigate the elec- tronic structure and bonding present in the resulting cations. Experimental All preparations were carried out under a dry dinitrogen atmos- phere using standard Schlenk and glove bax techniques. [Li(tht) [BAe] and NafBar]}2thf were synthesised using a slight modification of the literature procedure." The lithium salt was isolated as [Li(OH.),J{BAP’, which can be converted to the thf adduct by stiring in thf for 16 h over 4 A molecular sieves. Filtration and removal of solvents affords the thf adduct. Crude Na{BAr"} was recrystallised from thf/mhexane, resulting in the isolation of Na[BAr"}2thf. K[BAr'), Rb[BAr"), and Cs{BAP] were synthesised via cation exchange of Na[BAr"}2thf in water at 95 °C with excess (5 mol. equiv.) NOs, RDNO,, oF CsNO,, respectively.” Mestacn was syn- thesised by a literature procedure."* Me,eyclen was obtained by methylation of eyelen (Sigma) using formic acid/formal- dehyde."* Meg{18]aneN, (Sigma) was used as received. CH.Cl ‘was dried by distillation from CaHt;, toluene distilled from Na, and mhexane distilled from Na/K alloy. "H and “O("H4} NMR spectra were recorded in CD.Cl; solution at 298 K using a Bruker AV 1-400 spectrometer and are referenced to the residual CHCl, resonance. “Li, ’Na, and "Cs NMR spectra ‘were obtained on a Bruker AV 11-100 spectrometer at 298 K (unless otherwise stated) and referenced to a 0.1 mol dm” solution of LiCl, NaCl, of CsNO, in D,O, respectively. Micro- analyses were undertaken at London Metropolitan University. 35884 | ton Tone, 2015.44 15853-15966 View Ate Oia Dalton Transactions Xray crystallography Crystals were obtained as deseribed below. Details of the ery tallographie data collection and refinement are in Table SI} Diffractometer: Rigaku AFC12 goniometer equipped with an enhanced sensitivity (HG) Seturn724+ detector mounted at the window of an FR-E* SuperBright molybdenum rotating anode senerator (i, = 0.71073 A) with VHP Varimax optics (70 ym focus). Cell determination and data collection: CrystalClear-SM Expert 3.1 827, data reduction, cell refinement, and absorption correction: CrystalClearSM Expert 2.1 29." Structure soli: tion and refinement were carried out using WinGX and soft ware packages within."” Disorder in the CF groups of the [BAe] anions was present in all of the structures, whieh is often observed in compounds containing [BAr"]"," and this ‘was satisfactorily modelled using DFIX, DELU, and SIMU restraints. Positional disorder was also present in the “CH,CH,- linkers of the macrocycle in [Na(Me,eyclen}tht)} [war] and was modelled similarly. Two locations for the water molecule in [Li(Me,cyelen)(H,0)JBAe] were observed, with the combined electron density consistent with one fully-occur pied water molecule. Attempts to model this as other moieties (€- methoxide) were unsuccessful. H-atoms were placed in _geometrically-assigned positions with C-H distances of 0.95 A (CH), 0.98 A (CH), oF 0.99 A (CH,) and refined using a riding ‘model with Use(H) = 1.2Uqq(C) (CH, CH) 0F 1.5Upq(C) (CHs)- tenClfer was used to prepare material for publication."” CCDC reference numbers 1051099-1051108 contain crystallographic data in CHF format. Preparations [H(Mefrs}anen gwar}. [Li(th) [BAP] — (100mg, 0.09 mmol) was suspended in CHCl, (5 mL) and a solution of Meq{as}aneN, (31 mg, 0.09 mmol) in CHCl, (2 mL) was added. The reaction was stirred for 4 h then the product was precipitated by the addition of mhexane (20 mL). Crystals were obtained by layering a concentrated CH,Cl, solution of the product with hexane, White solid. Yield: 97 mg, 89%. Required for CottsdBPadLINe C, 49.51; H, 449; N, 6.93. Found: C, 49.52; H, 4.58; N, 6.9486, 'H NMR (298 K, CDCl, 6 = 7.73 ((SH), 5, BAP H2/6), 7.57 ([4H), 5, BAP HY), 2.46 (and, brs, NCH), 229 (8H), 5, NMe). NCf'Ht} NMR (298 K, CD.CL,}: 5 = 162.37 (C, q, Jen = 49.9 Hz, BAL" C1), 135.40 (CH, Bar! C2/6), 129.49 (C, qq, “Jew = 315, 2.9 Hz, BAP C3/5), 125.20 (C, 4, Je-y * 272 Hz, CF), 118.06 (CH, septet, Your = 40 He, BAP C4), 56.62 (NCH,), 45.24 (NMe). "Li (298 K, €D.C1,}: 6» -0.30. [Na(Me,{18}aneN,)[8A"). Prepared similarly using ‘a{iae"} 2th (100 mg, 0.10 mmol) and Me,(18]aneNy (34 mg, 0.10 mmol). Colourless erystals were obtained by layering a concentrated CHCl, solution of the product with mhesane, Yield: 59 mg, 44%. Required for CyoHl BP NuNa: C, 48.97; H, 4.43; N, 6.84. Found: C, 48.96; H, 435; N, 6.78. "HNMR (298 K, CD,CL,}: 5= 7.73 (HH), s, BAP” 2/6), 7.57 ([A], 5, BAP HA), 2.54 ([12H}), v br s, NCH,), 2.26 (30H), brs, NMe + NCH,). SC{!H} NMR (298 K, CD,CL}: 5 = 162.85 (C, qJo-n = 49.9 Hi, Ti jouna it © Te Roja Socety of Cherrisny 2015 Dipindai dengan CamScanner ips degen camscarneeDipindai dengan CamScanner