AL-Hussein Bin Talal University Science college Chemistry Department Inorganic Chemistry Laboratory Number o e!

periment 2 "reparation o potassium cis-an# transDio!alato#ia$uochromate

Introduction In this experiment we want Preparation of potassium cis-and trans-Dioxalatodiaquochromate(III) ,the metal we use it potassium dichromate, Chromium (symbol Cr and atomic number 24) occurs in the oxidation states 0, +2, +3, and +6 states !lement (0) and di"alent chromium, howe"er, are unstable ,the coordination number o# it Chromium (III)ha"e coordination number 6 (octahedral coordination and in this experiment we want use Cr(III) ha"e coordination number 6 ,and also Cr(III)ha"e coordination number 4 (tetrahedral complex) The physical and chemical property $% is a common inor&anic chemical rea&ent, most commonly used as an oxidi'in& a&ent in "arious laboratory and industrial applications (s with all hexa"alent chromium compounds, it is potentially harm#ul to health and must be handled and disposed o# appropriately It is a crystalline ionic solid with a "ery bri&ht, red%oran&e color ,and potassium dichromate it has a meltin& point(3)*C),boilin& point (+00C(decompose)),speci#ic &ra"ity e,ual (2 6-6),and it is soluble in water ,but insoluble in alcohol , and it is stable under ordinary condition ,the ligand we use in this experiment it water (.2/) and /xalic acid (/xalic acid dehydrate),the #orm #or it

The physical and chemical property :/xalic (cid (also called !thanedioic (cid) is a colorless, crystalline, toxic or&anic compound belon&in& to the #amily o# dicarboxylic acids0 meltin& at 1*- C0 soluble in water, alcohol, and ether It occurs in the #orm o# its metal salts (usually calcium or potassium) in many plants It is commercially manu#actured by heatin& sodium #ormate in the presence o# an al2ali catalyst to #orm sodium oxalate, which should be con"erted to #ree oxalic acid when treated with sul#uric acid /xalic acid is the only possible compound in which two carboxyl &roups are 3oined directly0 #or this reason oxalic acid is one o# the stron&est acids in or&anic compounds 4nli2e other carboxylic acids, oxalic acid (and #ormic acid) is readily oxidi'ed and combine with calcium, iron, sodium, ma&nesium, or potassium to #orm less soluble salts called oxalates /xalic acid and oxalates are use#ul as reducin& a&ents #or photo&raphy, bleachin&, and rust remo"al 5hey are widely used as an puri#yin& a&ent in pharmaceutical industry, precipitatin& a&ent in rare%earth metal processin&, bleachin& a&ent in textile and wood industry, rust%remo"er #or metal treatment, &rindin& a&ent, waste water treatment acid rinse in laundries and remo"in& scale #rom automobile radiators /xalic acid dehydrate ,has a white crystals as a physical state , the meltin& point #or it between (101%102C),the boilin& point #or it (14)%160C),the speci#ic &ra"ity is between (1 6%1 -),it is soluble in water and it is stable under ordinary condition coordination bond #or it0 oxalate ion (ox) /xalate ion is a bidentate li&and e"en thou&h it contains #our / atoms which ha"e lone pairs o# electrons , it is 6identate li&and is 7ewis bases that donate two pairs (8bi8) o# electrons to a metal atom 6identate li&ands are o#ten re#erred to as chelating ligands because they can 8&rab8 a metal atom in two places 5he complexes we preparation it $% the reaction #or cis and trans is :92Cr2/- + -.2C2/4 :6C/2 + 13.2/ +29 Cr(C2/4)2 2.2/ For Cis isomer:- 5he ;hysical and chemical property $%in spectrophotometer methods since in solution the cis isomer absorb much more stron&ly ,that by the color o# it ,it has hi&h dar2 color ,so &i"e much pea2 ,much intensity ,and it is polar ,and the product #or it Cis is 2inetic because it produces hi&h temperature solid state and 2inetic and polar,the color o# complex blac2 Fast reaction

For trans isomer :- the trans is thermodynamic need to temperature to the reaction happened . <olid state and dar2 blue 5hermodynamic and nonpolar ,the color o# complex dar2 blue <low reaction

Calculation :Theoretical yield 92Cr2/- + -.2C2/4 6C/2+13.2/+29Cr(C2/4)2 2.2/ I mol o# 92Cr2/- = 2 mol o# 9Cr(C2/4)2 4 &>2)4 1**6 &>mol = 0 013+)6-1))3 mol o# 92Cr2/?ol o# 9Cr(C2/4)2 2.2/ = 2@ mole o# 92Cr2/?ol o# @? A ?ass o# 9Cr(C2/4)2 2.2/ = =- -+26)46)) & Percentage ield of complex: B yield for Cis = (!ctual mass> Theoretical )@100B = (4 3-6>- -+26)46)))@100B = +6 44B B yield for trans = (0 -44 &>- -+26)46))&)@100B = ) +)66 B Discussion :Chromium "xalate:Chromium /xalate is produced by the reaction o# oxalic acid with a chromium salt Chromium /xalate is a hi&hly speciali'ed product #indin& use in metal treatment and platin& and the pharmaceutical industry !- For cis-Dioxalatodiaquochromate :#- In this experiment #irstly we use powder oxalic acid("xalic acid dihydrate) ,C2/4.2, C2/2(/.)2

2% /xalic acid is the chemical compound, colorless solid is a dicarboxylic acid, Its con3u&ate base, 2nown as oxalate (C2/42%), is a reducing agent. 3%In this experiment we use it as ligand, exactly a chelating agent #or metal cations 4%Ae were crushed the powder oxalic acid("xalic acid dihydrate) that well, to obtain "ery small particle +% (#ter that we &et dichromate, ;otassium dichromate. 6% ;otassium dichromate, 92Cr2/-, is a common inor&anic chemical rea&ent, most commonly used as an oxidi'in& a&ent in "arious laboratory and industrial applications, It is a crystalline ionic solid with a "ery bri&ht, red%oran&e color -% Ae were crushed ;otassium dichromate that well, to obtain "ery small particle *%(#ter that mix them as intimately as possible by &rindin& them &ently to&ether, to product approximately Cellowish oran&e
powder

)% (#ter that we put the Cellowish oran&e powder(the mixture ),on the basin and co"er it ,a#ter that $arm %ery gently 0because the mixture empowerin& suddenly0 soon a "i&orous reaction sets in ,with e%olution of steam and C"&. 5his operation $% '&Cr&"( ) (*&C&"+, -C"& ) #.*&" ) &' Cr/C&"+0&.&*&" 92Cr2/-, happened #or it reduction to product Cr+3,and also e%olution of steam and C"&.,by reducing agent, it is /xalic acid (li&and) 10%(#ter that we were poured ethanol o"er the product we were obtain, For cleanin&, so as not to turn into trans 11%we were put ethanol and stir until the product, is entirely crystalline and &ranular /the product 1purple-blac20. 3- For trans-Dioxalatodiaquochromate :#- In this experiment #irstly we use powder oxalic acid("xalic acid dihydrate) ,C2/4.2, C2/2(/.)2

2% /xalic acid is the chemical compound, colorless solid is a dicarboxylic acid, Its con3u&ate base, 2nown as oxalate (C2/42%), is a reducin& a&ent. 3%In this experiment we use it as li&and, exactly a chelatin& a&ent #or metal cations. +-Dirstly we were prepare two separately solutions, oxalic acid solution and dichromate solution, by usin& boiling $ater 4% 3oiling $ater to speed up the interactions #or the solutions, and we were use water to product trans isomer --(lso we note, when we were do this experiment, a#ter we were add the dichromate solution abo"e oxalic acid solution we co"er the solutions, to reaction proceeds -%6ut this reaction too2 Dor a lon& time, as the solution did not settle ,uic2ly(trans did not settle ,uic2ly)0because the trans isomer has hi&h dissol"ent ,so did not sediment ,uic2ly *%#inally we obtain rose%colored crystals o# the trans isomer 5tructure complex:Chromium $ atomic number 24, wt +2, con#i&uration E(rF3d+4s1 Common states Cr+3 and Cr+6( ie Cr/4%2) Chromium tannin& is between colla&en and Cr+3 6 coordination positions(octahedron) are present, and stereoisomer are possible

#-isomers :cis and trans an octahedral complex, geometrical isomers Cis:- cis bis chelate Trans:-trans bis chelate

it has the d. configuration and it is optically acti%e 1$hich do not ha%e improper relation axis.

:II-5hape

-:III-distortion /ctahedral complexes o# d6 and high -spin d+ ions are often + distorted example #or that CuD2 and ECr(/.2)6F2 so that two metal%li&and bonds(axial) are di##erent len&ths #rom , the remainin& #our (e,uatorial)0</ &' Cr/C&"+0&.&*&" ,cis and trans, an octahedral complex, it . has the d. configuration so no distortion -: 3onding : electron configuration -# Dor Cr$ E(rF 3d+ 4s1 (nd the electronic con#i&uration o# complex (cis and transe)is t&g. eg7 :Point group /& Trans:- trans bis chelate0optically in acti"e G2h Cis :- cis bis chelate0optically acti"e C2" -:splitting and crystal field theory /. In this experiment we use two li&ands ,are /xalate(/H) and water(.2/) as li&and which they e##ect in the splittin&

I%I6r%IEJC<F%ICl%ID%IE/.F%I8ox9- :*&"IEJC<F% IJ.3IenIb;yIphenIECJF% KC/ Ae note #rom this series that 8ox9- :*&" is li&ands increasin& Loct ,and also we use Cr 3+ we note that ha"e hi&h oxidation state (+3) and more stability0 so we /btained lar&e Loct 07ar&e splitting <o we note the electron o# Cr 3+ remained in the bottom (low spin)

+-electron transition:4

(2452(M) and 4(2451(D) transitions

Nuestions $ N1$

N2$ in Cis isomer where it polar the hi&h intensity and the hi&h, molar pea2 N3$we can di#erretiant between cis O trans throu&h the color , Cis blac2 0trans dar2 blue