lab report4 - Synthesis of Iron()-Oxalate Complex, and...

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Synthesis of Iron( )-Oxalate Complex, and Analysis for Oxalate and Iron Content of Complex 11/17/09 Aerin Noh Section : B05 TA :  Pavan J. Dalal
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Abstract: In this experiment, an Iron ( ) oxalate coordination complex was synthesized and analyzed to determine the empirical formula of K w [Fe x (C 2 O 4 ) y ] ∙z H 2 O . An oxidation-redox titration was performed to determine the oxalate concentration and spectrophotometry was used to find the concentration of iron within the unknown solution. From part4A, at first, yellow precipitation, then dark yellow precipitation, then brownish solid/solution, and then green crystal were produced.”observations omit from abstract” After leaving in the dark for few days, small, oblong-shaped, emerald green, salt-like crystals, and 1.1918g of crystals were produced. The empirical formula of the iron-oxalate compound turned out to be K 3 [Fe (C 2 O 4 ) 3 ] ∙3 H 2 O , where w=3, x=1, y=3, and z=3. This means that the ration of Fe: K: C 2 O 4: H 2 O is 1:3:3:3. (The exact ratio between mmol of oxalate and mmol of iron was 3.06: 1.00, which gave the approximation of a 3:1 ratio, and the exact ratio between mmol of water and iron was 3.21: 1.00, which gave the approximation of 3:1 ratio). Through titration, the weight percentage of oxalate was found to be 53.60 ± 1.50%, which could be converted into mmol per 100.0g of complex, meaning that 608.9 ± 17.2mmol of oxalate were present. Through spectrophotometry, Beer’s Law calibration equation was derived to be y = 10930x – 0.0102, which was then used to find the concentration of Iron ( ) in the solution, and thus, the weight percentage of Iron ( ) – a value of 11.1 ± 1.4%. This can be converted to mmol of Iron ( ) in 100mL sample which value was 0.206 ± 0.028. This, too, could also be converted to mmol per 100.0g of complex, giving a value of 199 ± 26mmol of iron preset. The initial mass of the Fe (NH 4 )( SO 4 ) 2 H 2 O compound was 1.2088g , which made 1.1918g of crystal product. Thus, determining that the complex is K 3 [Fe (C 2 O 4 ) 3 ] ∙3 H 2 O , the percent of yield of the iron-oxalate complex was found to be 78.72%.
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Introduction: The purpose of this experiment is to synthesize a coordination complex of Iron ( ) oxalate complex (in experiment 4A), which will then be analyzed quantitatively to determine its composition of oxalate (in experiment 4B) and Iron (in experiment 4C), by means of, oxidation- reduction titration and spectrophotometry, respectively. The complex ion is inside a coordination compound and is made up of both a metal ion and ligands. The metal ion usually carries a +2 or +3 charge, and is usually electron deficient, which means it is a Lewis acid that accepts electrons. Ligands donate electron pairs to the empty d-orbirtals of the metal ion, which makes them good Lewis bases. They can bind to many sites on the central metal ion. Ligands that bond to the metal ion in only one place are called
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This note was uploaded on 11/27/2010 for the course CHEM6BL 589023 taught by Professor Bernoilles during the Spring '10 term at UCSD.

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lab report4 - Synthesis of Iron()-Oxalate Complex, and...

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