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1-1 Date Performed: September 18, 2008 Date Submitted: September 29, 2008 I. II. TITLE. Determination of the oxalate in the sample(experiment 8) RESULTS. Standardization of Potassium Permanganate Solution Primary Standard used: Sodium Oxalate O Formula mass of 1 standard: 134.00 g/mol % Purity of 1O standard: 99.8% Trials Weight of Na2C2O4 (g) Corrected Weight Na2C2O4 (g) Final Reading KMnO4 (ml) Initial Reading KMnO4 (ml) Volume KMnO4 used (ml) Corrected Vol. of KMnO4 mL Normality of KMnO4 Ave. Normality of KMnO4 Indicator Blank Trials Final volume KMnO4 (ml) Initial volume KMnO4 (ml) Net Volume KMnO4 (ml) Ave. volume of KMnO4 (ml) Sample Analysis Trials Weight of the sample (g) Final volume KMnO4 (ml) Initial volume KMnO4 (ml) Net Volume KMnO4 (ml) Corrected volume of KMnO4, ml mg Na2C2O4 of unknown % Na2C2O4 of unknown Average % Na2C2O4 of unknown 1 0.5028 39.10 0.1000 39.00 38.90 2 0.5023 38.60 0.1000 38.50 38.40 3 -------1 45.0 44.9 0.1 2 45.1 45.0 0.1 0.1 3 45.2 45.1 0.1 1 0.2862 0.2856 44.80 0.1000 44.70 44.60 2 0.2989 0.2983 47.70 1.700 46.00 45.90 3 0.2856 0.2850 44.60 0.000 44.60 44.50
A. Corrected Mass of Na2C2O4 (g) Masscorrected=M Na2C2O4 * 0.9980 Masscorrected=0.2862 g * 0.9980 Masscorrected=0.2856 g
B. Net Volume KMnO4 Vnet of KMnO4=(Vfinal KMnO4)-(Vinitial KMnO4) Vnet of KMnO4=(44.80 mL)-(0.1000 mL) Vnet of KMnO4=44.70 mL
C. Corrected Vol. of KMnO4
Corrected VolKMnO4= Net VolumeKMnO4 - Ave. volumeKMnO4 in indicator blank Corrected VolKMnO4=44.70 mL-0.1000 mL Corrected VolKMnO4=44.60 mL
D. Normality of KMnO4 NormalityKMnO4=[(corrected weightNa2C2O4/m.wNa2C2O4)] Corrected volumeKMnO4 NormalityKMnO4 =
E. Average NormalityKMnO4 NormalityKMnO4=(0.1005 M + 0.09970 M + 0.1011 M)/3 NormalityKMnO4=0.1004 M
*for the indicator blank
F. Net Volume of KMnO4 Net VolumeKMnO4=45.0 mL - 44.9 mL Net VolumeKMnO4=0.1000 mL
G. Average Volume of KMnO4 Average VolumeKMnO4=(0.1000 mL + 0.1000 mL + 0.1000 mL)/3 Average VolumeKMnO4=0.1000 mL
**for the sample analysis
H. Net volume of KMnO4 Vnet=39.10 mL- 0.1000 mL Vnet=39.00 mL F. Corrected Vol. of KMnO4
Corrected VolKMnO4= Net VolumeKMnO4 - Ave. volumeKMnO4 in indicator blank Corrected VolKMnO4=39.00 mL-0.1000 mL Corrected VolKMnO4=38.90 mL
mg Na2C2O4 of unknown mgNa2C2O4=(corrected volumeKMnO4)(Nave KMnO4)(1 mol KMnO4/ 5 eq KMnO4)x (5 mol Na2C2O4/2 mol KMnO4)(m.w. Na2C2O4) mgNa2C2O4
mgNa2C2O4= J. % oxalate in sample % oxalate in the sample= (mg Na2C2O4/Wsample)*100% % oxalate in the sample =
K. Ave % oxalate in the sample Ave % oxalate=( Ave % oxalate=
The permanganate ion, MnO4-, is a powerful oxidizing agent; it reacts to form Mn2+ ion. MnO + 8H+ +5e- Mn2+ + 4 H2O is the half reaction of Pemanganate to form the Mn 2+ and the one responsible for the color during the endpoint; the Manganese goes from an oxidation state from 7 to 2 thereby saying it has been reduced and is the oxidizing agent in this experiment. Each Permanganate ion will consume 5 electrons to produce the Mn2+ and it has to be done in ACIDIC medium since the presence of H+ marks this type of medium; each MnO4- will also steal 5 electrons in the sense of it being the oxidizing agent; it will oxidize another species and that is the oxalate.
The Oxalate ion is a stable ion, yet it can be oxidized: C2O42- 2 CO2 + 2e-. The C in the oxalate has an oxidation state of +5 while the C in CO2 has an oxidation state of +4; given these oxidation states, each carbon will therefore release 1 electron and each oxalate will release 2 electrons.
o 2MnO4- + 16 H+ + 5 C2O42- 2 Mn+2 + 8 H2O + 10 CO2 (g)
In addition to OXALATE being a strong oxidizing agent, permanganate has another important property; it is a compound with an intense purple color. Even one drop of the titrant is enough to produce a strong pink color. With such property, the titration process just goes by titrating until the solution remains pink. The titration process used DRIED sodium oxalate being the primary standard; it has to be dried since the analyst aims to have a compound in its pure form; and no other contaminants or bound water in them. The procedures encountered required the titer to be heated first in a water bath for 80˚C to 90˚C; of course, water bath is used for the analyst to control the temperature of the system not to exceed that of water even if a thermometer was used. The reaction of permanganate tends to be relatively slow; it can take 30 to 60 seconds; and this would make the titration relatively impractical to perform. However, the reaction is much faster in the presence of a catalyst; a catalyst can never AFFECT the final outcome of the titration process. In this case, Mn 2+ is a good catalyst. So after the first small addition of MnO4-, the reaction will speed up and proceed at a comfortable rate; this is called autocatalysis as Mn2+ is formed in this reaction AUTOMATICALLY. With the facts established on the slowness of this reaction, one way of speeding up the reaction is through heating the reaction and this is what we done asides from the autocatalysis that happened. As experienced by the 2 analysts, there was a hard time reading the buret because of the color of the titrant which is so strong. As read on some sources with a possible solution to this encountered problem in the experiment, sighting across the top of the liquid is one way; of course, It is still important that our eye be level with that of the liquid layer to avoid parallax errors. A blank indicator was used in this experiment to have a corrected and expected volume free from other contaminants. COMMENT: I had problems with the visibility of the grid lines in the buret; the color of the permanganate solution is one hindrance to a sure shot in reading the buret upon taking volume readings. One thing about this experiment was that the permanganate solution was not EXACTLY diluted to 1 L; this is analytical chemistry therefore even in this simple preparation, we could have somehow approximated it would be near a liter. How about before starting the experiment, a kind of story telling where we are told of the applications of this experiment in day to day activities and how we could apply this to our courses; for example, in public health, what could possibly be the applications of this in human systems or maybe in chemical engineering, what could possibly be certain mechanisms we can apply when faced with systems like that.