Andrew Major

Honors Chem 151

Lab Report 2
10/5/2012
Title: Ammonium Decavanadate: Synthesis and Characterization
Purpose: Through a standardized titration of sodium oxalate (Na2C2O4) and potassium permanganate (KMnO4), a
titration of ammonium decavandate hexahydrate [(NH4)6V10O28-6H2O] (synthesized from the reaction of
ammonium metavanadate, acetic acid, and ethanol) with potassium permanganate will allow us to determine its
percent vanadium. This lab focuses on the synthesis of the decavandate, the characterization of the
decavanadate, and the standardization of potassium permanganate. In industry and research, sometimes it is
necessary to synthesize compounds which cannot be obtained naturally or are difficult to store.
Characterization in industry is used to determine unknown properties of unknown compounds. Standardization
is used in industry to give specific, quantitative values of properties of substances which can be used to compare
other substances to.
Procedure:
1. Synthesis of Ammonium Decavanadate Hexahydrate
2. Measure about 1.5 g NH4VO3 (tare weigh boat at balance) into 400 mL beaker.
3. Add 50 mL dH2O.
4. Heat using hot plate to dissolve.
5. Once dissolved, solution should be transparent yellow. It is ok if it does not completely dissolve.
6. Cool beaker containing the metavanadate under tap water.
7. Add 2 mL of 50/50 acetic acid.
8. Place beaker into ice bath until the solution turns orange.
9. Add 75 mL 95% ethanol.
10. Cool beaker, in ice bath, to below 10C for 15 minutes, stirring occasionally.
11. While orange crystals are cooling, obtain 30 mL of ethanol (50 mL beaker) from the hood and place in an
ice bath.
12. Filter bright orange crystals using Buchner funnel.
13. Use ethanol 2x 15 mL washes. Allow to dry under vacuum before removal.
14. Remove Buchner funnel from the side arm flask and invert and tap onto watch glass.
15. Preparation of Potassium Permanganate
16. Measure 1.6 g KMnO4 into a 600 mL beaker.
17. Record the mass of KMnO4.
18. Add 500 mL of dH2O to the beaker and 3 - 4 boiling chips.
19. Cover with large watch glass.
20. Place on hot plate in the hood and allow to boil.
21. Preparation of Sodium Oxalate
22. Weigh approximately 2 g Na2C2O4 using weigh paper.
23. Place in clean weigh vial. Place vial and lid into 400 mL beaker with watch glass and paper with ID.

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Place in drying oven.

Filtering of Potassium Permanganate
Filter KMnO4 solution using Buchner funnel.
As side arm flask fills, pour KMnO4 solution into the amber bottle.
Rinse 600 mL beaker that contained the KMnO4 solution and leave beaker in HCl acid bath until end of
lab.
Clean and rinse side arm flask and buchner funnel after filtration.
Preparing Buret for Titration
Fill buret with dH2O and allow the water to pass through the drain valve to ensure buret is working
properly.
Ensure that sides of the glass sheet with water.
Add 10 mL of KMnO4 solution to the buret and coat the sides of buret walls twirling and rolling buret.
Slowly pour solution into waste beaker at station. KMnO4 solution should also sheet.
Allow some of the solution to pass through the drain valve.
Repeat KMnO4 rinse 2x.
Standardization of KMnO4
Trial 1:
In flask:
0.2xxx grams Na2C2O4
250 mL 0.9 M H2SO4
Add the value calculated for 90% to the flask.
Allow the solution to clear at room temperature.
Once clear, heat flask to 55-60C.
Finish titration at sign of first persisting pink color.
Determine volume of KMnO4 required.
Trial 2
In flask:
0.2xxx grams Na2C2O4
250 mL 0.9 M H2SO4
Add the value calculated for 70% to the flask.
Allow the solution to clear at room temperature.
Once clear, heat flask to 55-60C
Finish titration at sign of first persisting pink color.
Determine volume of KMnO4 required.
Trial 3:
In flask:
0.2xxx grams Na2C2O4
250 mL 0.9 M H2SO4
Add the value calculated for 70% to the flask.
Allow the solution to clear at room temperature.
Once clear, heat flask to 55-60C
Finish titration at sign of first persisting pink color.

63. Determine volume of KMnO4 required.

64. Characterization of Ammonium Decavanadate Hexahydrate
65. 0.3xxx g (NH4)6V10O28-6H2O (record mass before and after transfer using weigh paper at the analytical
balance) into 250 mL flask
66. Do not use a sample size larger than 0.3500 g!
67. Run in duplicate. Be sure to label flasks!
68. Add 40 mL 1.5 M H2SO4 (instead of 20 mL of 3 M H2SO4 and 20 mL of water)
69. Add about 1 g NaHSO3 (measure using weigh paper) and add in hood. Add 50 mL dH2O and a couple of
boiling chips.
70. Swirl and allow the 250 mL flasks to sit 5 about minutes.
71. Then boil for 15 minutes to drive off SO2. Rinse sides of flask with dH2O a couple of times during heating
process.
72. Titrate solution with KMnO4 until it turns a faint orange or dark apple juice colored yellow.
73. Record initial and final buret readings.
Data:
Mass KMnO4: 1.607g
Standardization
Mass NaOx
Initial Volume
Final Volume
Difference of Volume
Molarity of KMnO4

Trial 1
.254g
43.7mL
44.2mL
34.1mL
0.0222M

Trial 2
.250g
36.2mL
43.7mL
33.2mL
0.0225M

Trial 3
.251g
27.0mL
35.2mL
34.0mL
0.0220M

Trial 1
0.3001g
1.0mL
24.0mL
23.0mL
0.1301g
43.3%
0.2%

Trial 2
0.3003g
24.0mL
47.0mL
23.0mL
0.1301g
43.3%
0.2%

Average

Average Molarity: 0.0222M

Characterization
Mass of Decavanadate
Initial Volume
Final Volume
Difference of Volume
Mass of Vanadium
%V
%Error

Calculations:
Balancing the Oxidation-Reduction Reaction:
V10O286- + H2SO3 VO2+ + HSO4V10O286- + H2SO3 10VO2+ + HSO4V10O286- + H2SO3 10VO2+ + HSO4- + 17H2O

43.3%
0.2%

V10O286- + H2SO3 + 33H+ 10VO2+ + HSO4- + 17H2O

V10O286- + H2SO3 + 33H+ + 8e- 10VO2+ + HSO4- + 17H2O
VO2+ + MnO4- VO2+ + Mn2+
VO2+ + MnO4- VO2+ + Mn2+ + 3H2O
VO2+ + MnO4- + 6H+ VO2+ + Mn2+ + 3H2O
VO2+ + MnO4- + 6H+ + 4e- VO2+ + Mn2+ + 3H2O
Two Halves:
1 X [V10O286- + H2SO3 + 33H+ + 8e- 10VO2+ + HSO4- + 17H2O]
2 X [VO2+ + MnO4- + 6H+ + 4e- VO2+ + Mn2+ + 3H2O] (to balance the number of electrons)
V10O286- + H2SO3 + 33H+ + 8e- + 2VO2+ + 2Mn2+ + 6H2O 10VO2+ + HSO4- + 17H2O + 2VO2+ + 2MnO4- + 12H+ + 8eV10O286- + H2SO3 + 21H+ + 2VO2+ + 2Mn2+ 12VO2+ + HSO4- + 11H2O + 2MnO4Standardization of Potassium Permanganate Theoretical:
Mass KMnO4 / MM KMnO4 X 2L-1 = Molarity KMnO4
1.607g / 158.05mol/g X 2L-1 = .0203M KMnO4
Mass NaOx / MM NaOx X Mole Ration2/5) / Molarity KMnO4 = L KMnO4
Trial 1:
(.254g / 134g/mol X 2/5) / .0203M = .0373L
.0373L X 90% = .0336L
Trial 2:
(.250g / 134g/mol X 2/5) / .0203M = .0368L
.0368L X 70% = .0257L
Trial 3:
(.251g / 134g/mol X 2/5) / .0203M = .0369L
.0369L X 70% = .0258L
Standardization of Potassium Permanganate Actual:
Mass NaOx / MM NaOx X Mole Ratio(2/5) / L KMnO4 = Molarity KMnO4
Trial 1:
(.254g / 134g/mol X 2/5) / .0341L = .0222M
Trial 2:
(.250g / 134g/mol X 2/5) / .0332L = .0225M
Trial 3:
(.251g / 134g/mol X 2/5) / .0340L = .0220M
Average Molarity: .0222M
Characterization of Mass of Vanadium:
L KMnO4 used in titration X Average Molarity KMnO4 X MM Vanadium (54.9415g/mol) X Mole Ratio (5)
Trial 1:
.0230L X .0222M X 50.9415g/mol X 5 = .1301g

Trial 2:
.0230L X .0222M X 50.9451g/mol X 5 = .1301g
Conclusions: In this lab, standardization of a solution of potassium permanganate allowed us to characterize an
unknown solution of decavanadate and determine its percent vanadium by mass. This lab focused on the
synthesis of the decavandate, the characterization of the decavanadate, and the standardization of potassium
permanganate. Our three trials revealed that our potassium permanganate had an average molarity of .0222M
with individual values of .0222M, .0220M, and .0225M. These standardized values were fairly precise with less
than 2% variation on either side of the average value. Possible sources of error in the standardization process
include incomplete filtration of the potassium permanganate, although it is more likely that error arose in the
titration process itself, most likely in the realm of over titrating the solution or improper distinction of a
persisting pink color. When characterizing the decavandate, both trials, and thusly the average came to be
43.3% vanadium by mass. Since both trials yielded the same result, our precision was perfect but when
compared with the theoretical value our accuracy was also very good with a .2% margin of error. Sources of
error in characterization of the decavandate are largely a part of knowing when the solution has been
completely titrated without going over the point where it is complete. Overall, however, our results proved to
be both precise and accurate despite the difficulty associated with titrations.