synthesis of cobalt complex lab report
Herlt,A.M.Sargeson,J. g;i:nN#7A]pNBnMMb !AWuV`$/& 4VkG>$9%jH}bFag"9xWm&{+$eK'9Mo_E;h/JW[HZARi 'L:%x>w%|%y'YL8%?c|F@Y;JLC\CeY95llzJ30Pp%XzYg(GWj(8]sB*y]G8"{A")P26;[1lSJ?PY#:8;trq.v-|e^4sN D`kyEVp {&g{vOvOi??vO^~x77\>nysCn#x:f1w_w8ojM~Rc@8/D')%1CwEw$8Ce\!}eQ4+~|(E?|/__n_7Z~3 mJf)r{7t>e_e[_l^]{snp8X({t1u>|9^ywTrm2Y1[ak-8bn~t@Q-Tt |dZA>|oi-Fd>}d>ga;R6OG>_bm# [O#f1DZSkL#|WoU;myN.HWH{)C|a{(kbu`89>52 ^;\9;;`V1{r,}P"eX&*ZFQcD+21Z3T.FymZSj%gYK+l1!F)q^_ +*#`g34~qd]bCKik;h_t/[W? The brown complex of cobalt (III) bis-(Iminodiacetato) can only have the trans-fac and the trans-mer isomers. 706 ( g"l]gFd! "D'`*A+"`FL3D2#g^c|F>.RBPL8'= KqZ K# |5MY-iY7KMDzq8V\3FpI8L5I{@v|0]Jk~tR1GdI)gAPO*>T2LvXcr%r~d=zT*#tZu..IWf\-9?>RbcXQFV,L/IK>JvT_ zy*L&>c*b3Mc45^ Educ. The usingUVVisspectrophotometry Snow,J. Thereafter, 5.0 ml of 15% H2O2 was carefully added to the mixture at a rate of 2 ml/hour while stirring. In experiment 7 to 9 you will perform four experiments to determine theunknown x. steroselectivityandwouldnotbepossiblewithoutthepresenceofthemetal oxidation the Co(II) ion might due to the Co(II) complex exchanging ligands, Coordination chemistry 1 werners work and werner's theory, Sigmatropic rearrangement reactions (pericyclic reaction), Aromatic Structures and Chemistry of Benzene, Chapter 06 an overview of organic reactions, Conformational analysis of ethane butane aliphatics, B sc_I_General chemistry U-III(A) Alkane,alkene and alkynes, Preparation of potassium trioxalatoaluminate(III) trihydrate. 5, synthesis of [Co(diNOsar)]3+ During the experiment it reacted very similarly to Iron (III) nitrate and Barium nitrate. Jacewicz, D.; Pranczk, J.; Wyrzykowski, D.; amoj, K.; Chmurzyski, L. Thermal Properties of [Co(En)2Cl2]Cl in Solid State. A strong band appearing at approximately 1730 cm-1 gives the signal for free carboxylic acids. This is done in the introductory section of the manual, the individual lab introductions, and through extension questions requiring research about traditional, more hazardous experimental methods. 5, 2018, pp. This laboratory manual provides a one semester survey of basic analytical laboratory techniques, chemical methods of analysis and approaches to data analysis used in quantitative analytical chemistry. What is the purpose of using H2O2 in the synthesis? showingbothoxidationandreductionpeaksfortheCobaltion(Figure.2). In this experiment [Co(diNOsar)]Br 3 is synthesised from [Co(en) 3 ]Br 3 in the In Inorganic Syntheses; Wiley-Blackwell, 2007; 222225. 0 SargesonandM.R. We will synthesize the unknown compound with concentrated ammonia, Cobalt (II) Chloride Hexahydrate, 30% H2O2, and concentrated HCl. R.J.Geue,T.W. I -s2o.100 Chapter 3 Chemical BondsUWL tnteractive ve.docx. . theNO2groups. TheCVspectraofCo(diNOsar)]Br3and[Co(sepulchrate)]Br3has I.I. Purpose The purpose of this lab is understand how to describes synthesis of the cobalt complex. . shownboth The Brown compound, was the trans-fac isomer whereas the more electronegative groups where on opposite sides, of the central atom, hence, their individual dipole moments cancelled. Inorg. However, when the carboxylic acids are coordinated to cobalt (III) this signal shifts to, a value that is approximately 1630cm -1 . andtheelectrochemistryofthecomplexesusingcircular Acoording, to Lawrence and Rix, 1979 separation of the two isomer by using anion, exchange chromatography elutes the brown compound first. Experiment #9: Synthesis and Percent Cobalt Analysis of a Coordination Compound and Kinetics of Aquation of a Cobalt (III) Coordination Compound. endstream FacilSeynthesoisfaMacrobicycHliecxaamineGobalt(llC[ompleBxaseodn The synthesis of the product and the presence of any undesired byproducts will be verified using mass spectrometry (MS). ,nitromethaneandaqueous Anunderstandingoftherequiredreactionconditionsneededinorderto Reasonsforthelowyieldincludethedifficultyingettingallofthe ,}Tr.6;XAo,p[fY '9rW7f{,mTo "B86"WkYFD@ .% N/ad TheCVspectrumof[Co(sep)]3+ 5 Thereafter, 5 ml of 15% H 2 O 2 was carefully added to the mixture at [ 0 0 612 792 ] >> frIt $Ob`bd`m8$U orderforanewligandssuchaswaterbindtothemetal. to occur. Lack of sodium carbonate may cause incomplete reaction with copper chloride (II) because of low pH (6.0) of the solution [12]. Theseeffectsbringthe assignment. The Cobalt (III) bis-(Iminodiacetato) complex. z5tOG,*PqNWhwb&>Cdiy8D:7X*oqDFMjS4C'O;pjrw>4|/& Journal of Chemical Education . x}IrE$Rnf~7@,4GxcwsqGC]_knnhfgy>>! compoundsshowsthepresenceoftwoabsorbancebands. turned dark blue in pyridine but did not dissolve. PDF) Synthesis of cobalt(III) coordination complex and modifying it to chloropentamminecobalt(III) chloride. Cyclicvoltammetrypart: 3, for the synthesis of [Co(diNOsar)]3+ The Infrared spectra of the brown and violet compounds both had a band at 1623 cm-1 revealing that complexes of cobalt (III) with Iminodiacetic acid were actually formed [3] , see figures 2 ,3 and table 1. Oncethereactivehigh Thereasonforirreversible Co(II)ionwasstabilisedwhilstboundinsidethecage. Analysis of the Cobalt Complexes Collect a uv-vis absorbance spectrum for each complex. Whereas triethylenetetramine coordinates to form a, , symmetry axis, tris (2-aminoethy) amine forms a complex that has a, The purpose of the lab is to synthesize a cobalt (III) that is prepared by using cobalt (II), the, amine, and reagent which convert cobalt(II) to cobalt(III). Figure1/TheCVspectraforthethreecompoundsareattachedwiththe 2, 469 345 9ZfFQ_B}rjH;gM1wyFiMv/1m}eJkk GY]*XR2 The reason for irreversible Chem. Exp 1B cm- Functional group Literature Value (cm- The coordination sphere of electronicnatureoftheCobaltionatthecentreofthecomplexesissimilarin endobj The peroxodisulfate anion, S2O82-, was also observed for its ability to serve as a counterion for precipitation by preparing a copper (II) complex by reacting hydrated copper (II) sulfate with ammonium peroxodisulfate in the presence of pyridine. {|Cy\RLMD]dk:`hk:bC*SBiZsLx11[\(0oP$_ that was formed electrochemicalpropertiesofavarietyofcompoundsincludingmetal Describe any unusual observations and possible reasons for low yield. Since the compound did not react with any of the reagents above and just cations must lose its two valence electrons so that the anions (which have more than an Chem. 4 into a blue-violet colored Co complex and measuring the absorbance in the Spec 20 instrument. The reactivity of the bis (acetylacetonato) copper complex was low due to its exceptional stability. spind7 . Table 2: Table showing the peaks and their possible functional groups that where obtained from the IR spectra of all the bis-(acetylacetonato) copper (iii) complex, Similar to the cobalt complex, a strong band at 1730 cm-1 means that there are free carboxylic acids in the compound. 7, TheCVspectrumfor[Co(diNOsar)]3+ 3 0 obj presence of formaldehyde, nitromethane and sodium carbonate. We use concentrated H. MUKHANBETOVA NAZIRA EXPERIMENTAL LABORATORY MANUAL on discipline ANALYTICAL CHEMISTRY CHEMICAL METHODS OF ANALYSIS: TITRIMETRY and GRAVIMETRY (part 1) for the students of technical specialities, Food Analysis Laboratory Manual Second Edition, Analytical Chemistry for Technicians Third Edition, EXPERIMENTAL LABORATORY MANUAL by discip 1, EXPERIMENTAL LABORATORY MANUAL by discipline GENERAL CHEMISTRY for students of technical specialties Astana 2015 2, Vogel's TEXTBOOK OF QUANTITATIVE CHEMICAL ANALYSIS 5th ed - G H Jeffery, Standard Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated Lime 1, PRECISE ADVANCED LEVEL CHEMISTRY PRACTICAL GUIDE, A manual on analytical techniques A. 2 0 obj 2. The mixture was cooled down The synthesis of the coordination complex trans- dichloro bis (ethylenediamine)cobalt(III) chloride is a classic experiment and can provide an opportunity for inclusion of diverse concepts if additional activities are incorporated. 36.7%wasobtainedforthe[Co(diNOsar)]Br3.Theelectrochemicalproperties The solution was cooled in an ice bath and the product crystallised. Course Hero is not sponsored or endorsed by any college or university. Synthesise[Co(diNOsar]3+ This same ability, coupled with its strong oxidizing ability allowed for stabilization of the unusual oxidation state of 2+ for silver which was observed by preparing an analogous silver (II) complex by reacting silver (I) nitrate with ammonium peroxodisulfate in the presence of pyridine. couplingtoeachother. A infrared spectra of the product was then obtained. ofCo(diNOsar)]Br3,[Co(en)3]Br3and[Co(sepulchrate)]Br3wereinvestigated The other molecule is named pentaamminechlorocobalt (III) chloride. << /Length 1 0 R /Filter /FlateDecode >> The minimum amount of NH 3 was used to neutralize acetyl acetone. productcrystallizingoutofsolution. fromclassicalcomplexes. Description This is a two-week lab in which students synthesize and then characterize three Werner cobalt complexes using IR, UV/VIS and computer calculations using Spartan. dissolved in some, it can be conclude that this compound is highly stable due to its low x\s_G. 0oN @ Ea]?0;IS)$nJ;>Z-Nvo]y?-R_?~P,8O] o_g t:Gd8~$2_/-)7|CN&x!Ox2*#<3kN(L|VgS>Mq3~FJw[?, qhq,)\7E0%IE_`jw)Qcbyo~yW+Tv_RYeCe[aF0Ov!O+q\,PQ#\VknU%q_yOws%I6>ORYvBhB5: es.P)/[\Z|hCR^^/Mqn+Mq*/_*/P#57k@x3'BsyxG|z,J\`& ck/W~' Fyar_FZR6e{y=' z/WjPyU\N5 &gCpye?~WQK2*SNj(Nf>gT@{ ^*zP*ki&:[& GX*=1 V\E?r4F\! Amer. When viewed under a microscopic both compounds were similar to tiny pieces of broken, glass. stream 4Ix#{zwAj}Q=8m endobj IR spectra for the three products were, This experiment initially involved the synthesis of an iron (III) oxalate complex with the general, Cobalt Complex Project-Synthesis Lab Report, The compounds of the transition metals react with negative ions and/ or neutral molecules to form transition metal complexes. There are three possible bis- type geometric isomers of Cobalt that can be synthesized in, this experiment. Analysis of the other cobalt complexes e. [Co, (IDA) dien +], where dien = diethylenediamine, revealed that IDA favoured the facial (fac), complex to that of the meridional one since the trans-mer isomer was less stable than the. The The reaction mole ratio of sodium carbonate to copper chloride (II) was controlled from 1.08 to 1.68. The neutralized solution was then added carefully to CuSO4.5H2O in 50 ml dH2O. University Science Books, 1996, pp 13-17. The precipitate was filtered with suction and was washed repeatedly with water acetone and a small amount od ether. Its formula is written [Co (NH3)5Cl]Cl2. This was because Cis isomer (or violet compound) had a higher affinity for the resin due to its dipole, all the more electronegative groups were on the same side of the central atom. The crystals were then observed under a microscope. Thisindicatesthatinthetwocomplexesthecobaltionis endobj Aims Noticied a slight color change to dark purple. Copper sulfate: 3 .05g 1 mol249 reactantg 11 molmol reactantproduct 1 mol265 productg = 3, Acetyl acetone: 2 .45g 1 mol100 reactantg 11 molmol reactantproduct 1 mol265 productg = 3, Therefore copper sulfate is the limiting reagent, = 74 % for the Bis-(Acetylacetonato) copper (III) complex, Table 2: Table showing the peaks and their possible functional groups that where obtained %PDF-1.6 % When the obtained product was mixed with chloroform there was no reaction. All three syntheses begin with cobalt (II) nitrate hexahydrate, which is oxidized to Co (III) using hydrogen peroxide in the presence of ammonia. Moreover, unknown 3 reacted similar to Barium nitrate when it was tested against ammonium chloride and sulfuric acid. 36.7% was obtained for the [Co(diNOsar)]Br 3 .The electrochemical properties A handout called "The Cobalt Complex Project-Synthesis" was given by the instructor. 3167 NH 3 (N-H gHgL5][:)iv?/]ie-vi=h~pQ%RRUcx D/rTSTL[. constituteandAABBspinsystem. alsoshowsbothoxidationand When the obtained product was mixed with chloroform there was no reaction. Snow,J. TheUVVisspectraofall insidethecageeventhoughitisnotconsideredtobethermodynamically THE PREPARATION , ANALYSIS AND REACTION OF AN ETHANEDIOATE (OXALATE) COMPLEX photo chemistry of ligand in coordination compound, 17 - Reactions of Aromatic Compounds - Wade 7th. radiochemistry. . Figure 1: Possible structures of the cobalt (III) bis-(Iminodiacetato) complex, Bis(acetylacetonato) copper(II) is a complex that results from the coordination of copper with acetyl acetonato anions. TrisIEthylenediaminelGolUbaltfl,JChemicalEducation,62,9,804806. ka*>suzKo-~PjE_a-zTv@W2e T&KB$C^?a WawVn , !in.N0dK3Oz[nv+j1E,zoj_*nai.GS6)Q.; The crystal turned dark blue in pyridine but did not dissolve. v[9a_*#HQ&1*"4lSV)7)+,%#kpHL|=RtE`6RcM||HEl>t) H,hun7lx.-d byusingcyclicvoltammetry. reversible oxidation of the Co(II) ion to Co(III) ion. The stereochemistry of the brown compound is actually the trans-fac and that of the violet compound is actually cis. Cobalt salts react with solutions containing chloride ion, and ammonia to produce different complexes containing cobalt, ammonia, and chlorine. Please put it in the container provided, as directed by your instructor.
