February 1 -February 4, 2010

The preliminary report on the synthesis and yield of Potassium Tris(oxaloto)ferrate(III) Trihydrate is due the week of Feb. 8th
This week you will complete experiments 12-090, 13-079 and 14-067:
The prepared K3[Fe(C2O4 )3]*3H2O should be filtered using a Buchner funnel and washed with 50% ethanol. The product should be covered with aluminum foil and vacuum dried for at least 30 minutes. While the product is drying the you can prepare the standard series for experiment 13079. You will work in pairs to prepare the standard series. Plastic disposable transfer pipets (not burets) will be used to make their solutions. Each pair of students only need to use 2 mL 10% hydroxylamine hydrochloride, 15 mL 1,10 phenanthroline and 15 mL 2 M acetate buffer, pH 4.6. These are sufficient amounts to prepare both the shared standard series and your individual solutions. The solutions are somewhat expensive and we would like to cut down on needless waste. After preparation of the standard series, you should weigh your small amber bottle (without the cap), transfer your sample of K3[Fe(C2O4 )3 ]*3H2O the amber bottle and then reweigh the bottle. Cap up the bottle to protect your sample from decomposition. You should

then calculate the percent yield of your product and check your calculations with your lab instructor. You can then prepare your sample of K3 [Fe(C2O4)3]*3H2 O H2O for colorimetric analysis and then analyze the standard series and your individual sample. For experiment 13-079, you will need to generate a plot of the curve for your standard iron series. You can use Excel to generate a standard graph. Your lab manual has a section on using Excel to generate graphs. Before you leave lab you must generate your standard curve, find (remember Beer's Law?). You may bring a laptop computer to lab this week or if you want to use the PC's in the lab, bring a floppy disk to store your data.

The Preliminary Report :

Guidelines for writing a scientific report are found on pages 42 - 44 of the lab manual. Helpful Hints (perhaps): This PDF file includes some shortcuts for producing subscripts,
superscripts and symbols in MS Word.

Calculations for preliminary report should include limiting reagent, theoretical

yield, experimental yield and % yield. Moles of each reagent used should be calculated. The literature molecular weights should be used (Aldrich is a good source of information and a copy is available in the in the lab and the science library). The limiting reagent should be determined and the theoretical yield (in moles and grams) should be calculated. [Fe(NH4)2(SO4)2]*6H2O (ammonium iron (II) sulfate hexahydrate) H2C2O42*2H2O (oxalic acid dihydrate) K2C2O4*H2O (potassium oxalate monohydrate) H2C2O42*2H2O: (you used different amounts in each part of the experiment) 6 % H2O2 (hydrogen peroxide): 6% w/v = w/17 mL, w = 17 mL x 0.06 g/mL. Once you have weight of H2O2 you can determine moles. Once the theoretical yield is calculated, you can calculate your % yield : (experimental yield/theoretical yield) x 100%

Calculations for 13-079: Determination of iron content of your coordination compound:

Calculate the molarity of the initial stock solution of [Fe(NH4)2(SO4)2]*6H2O. Calculate the molarity of the diluted stock solution (50.0 mL volumetric). Calculate the concentration of Fe3+ for each solution of the standard curve and make a plot of the concentration of iron (xaxis) vs. absorbance at (y-axis). Draw the best straight line through your points and use your graph (see example below). Using your standard curve, calculate the concentration of Fe3+ in your coordination compound samples which were diluted 1:100. You can read the [Fe3+] directly from the graph or solve the equation for the line using Beer's law: A= lc, where, A = absorbance, l =

= molar absorptivity and c = concentration. The slope of the line is simply equal to l, and since l = 1.00 cm, the slope of the line equals . Once you have solved for , you can use the absorbance of your sample to determine [Fe3+] of the
path length (1 cm in this case), sample. Using the determined concentration and the volume of sample analyzed, calculate the mass of Fe3+ present in your original solution of coordination compound. Using the mass of iron present in the original solution, and the mass of coordination compound weighed out, calculate the percent iron by weight in your coordination compound: (Mass Fe in your sample/Mass of sample) x 100% = % of Fe in your sample. Calculate the average percent iron in your coordination compound and the standard deviation of your measurements. Does the average percent iron in your compound compare favorably with the percent iron in potassium trisoxalatoferrate(III) trihydrate?

Example of a Standard Curve:

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Last Updated: 1/5/10