THE UNIVERSITY OF BAMENDA REPUBLIC OF CAMEROON

PEACE – WORK – FATHERLAND

Faculty of Science Department of Chemistry

CHMS4101: ADVANCED CHEMISTRY LABORATORY

The experiments contained in this laboratory manual have been designed to contribute to the student's
understanding of the principles of inorganic chemistry through:

1) The use of some of the modern techniques for the synthesis and investigation of inorganic
compounds. and

2) The gaining of first-hand experience of inorganic compounds. Note that the experiments are not
in some cases specifically tied to particular sections of the lecture course, but rather designed to
augment the lectures in order to provide a broad introductory course in inorganic chemistry.

LABORATORY REPORTS

The format of the written laboratory report will vary slightly from experiment to experiment, but in
general they are expected to contain the following:

a) Purpose: Briefly describe what you plan to do, and why.

b) Procedure: Give a condensed version of what is in the manual. Include the exact weights of
reagents/products you measured.

c) Observations: Describe what happened in your reaction, in some detail.

d) Analysis: If required, report the qualitative tests in the usual way (Test/Observation/Inference).
Include any spectra you recorded and provide interpretations where possible.

e) Discussion: Give an explanation of the steps in the synthesis, and of the observations you made.
Give balanced chemical equations where ever possible. Explain any anomalous (i.e. too low, or
too high) yields from syntheses.

f) Conclusion: Give a very brief summary of your results. This will obviously differ greatly from
experiment to experiment.

g) Post-lab questions: Answer fully all questions posed at the end of the laboratory write-up.

h) References: Include all references used in the laboratory write-up.

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 1

Marking

All laboratory reports are due two days after the end of the experiment. Late reports will be penalized
5% per day except in extenuating circumstances. Each report will be worth 10% of your CA mark, with
the lowest grade being dropped in the final calculation. The final exam will be worth 70% of the grade.

UNDERGRADUATE TEACHING LABORATORY SAFETY REGULATIONS

1) NO STUDENT MAY WORK IN A LABORATORY UNLESS AN INSTRUCTOR IS ON

DUTY.

2) RECOMMENDED EYE PROTECTION MUST BE WORN AT ALL TIMES IN THE

LABORATORY, UNLESS SPECIFICALLY INSTRUCTED OTHERWISE.

3) NO SMOKING, EATING OR DRINKING IS PERMITTED.

4) LABORATORY COATS ARE RECOMMENDED WHILE WORKING IN THE

LABORATORY.

*Regular prescription glasses are an adequate substitute only in the absence of an explosion hazard or
where no hazardous chemicals are being used in the laboratory.

In addition to these four basic rules, the following regulations should be observed:

1. No student may perform an unauthorized experiment.

2. Never leave an experiment in progress unattended.

3. Any chemical which produces toxic vapors must be used in a fume hood.

4. Wipe-up spilled chemicals and bottle `rings' immediately.

5. Never handle or pour flammable liquids near an open flame.

6. Report all accidents to the instructor immediately.

7. Unless given specific permission to the contrary, NEVER pipette a liquid by mouth; Use a
rubber bulb.

8. Keep the sinks clean.

9. At the end of the period, make sure the hood, work area and sink are clean and tidy.

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EXPERIMENT 1: COMPLEX ION COMPOSITION BY JOB'S METHOD (METHOD OF
CONTINUOUS VARIATION)

Introduction

The nickel(II) ion in aqueous solution forms complexes with 1,2- diaminoethane(ethylenediamine)
whose ligand replaces two water molecules in the hydrated complex, i.e. acts as a chelate.

The relative values of k1, k2 and k3 will determine the relative proportions of the complexes. If k3 >>>
k2 >>> k1, then addition of ligand will result in formation of Ni(en)32+. If k3<<< k2<<< k1, then all four
complexes (or three, depending on the absolute magnitude of the constant) will co-exist in appreciable
quantities at equilibrium. The application of Job's Method is limited to situations where one stage
predominates.

In the method, the total molar concentration of nickel(II) plus ligand is kept constant and the ratio
varied from zero to infinity. Initially in a solution containing no nickel(II) ion (ratio = 0), no complex
will be present and the absorbance of the solution is due solely to diaminoethane. As the concentration
of nickel(II) is increased, absorbance will increase (due to formation of complex) until the molar ratio
of nickel(II) to ligand equals the ratio in the complex. Under the Job conditions, i.e. total molar
concentrations of the two species is constant, this represents the maximum possible concentration of
complex. Further increases in nickel(II) concentration (with corresponding decreases in ligand
concentration) will cause a decrease in absorbance until a solution containing no ligand (ratio = 4) has
an absorbance due to nickel(II) ions alone. A plot of absorbance against ratio of molar concentration of
nickel(II) ion to ligand will show a maximum where the ratio represents the composition of the
complex.

While there are several [Ni(en)n]2+ species formed, each has a different colour and, hence absorbs a
different wavelength. By constructing separate Job’s method plots for the absorbance data at each
different wavelength, the different complex ions can be identified.

One last complication is the fact that Ni2+(aq) also absorbs visible light (en is colourless and does not).
Thus, the measured absorbance must be corrected for this fact. The corrected absorbance Y due only to
the complex ion is calculated from the following expression:

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where Ameas is the measured absorbance of a given solution, X is the mole fraction of en in the solution,
and Ani is the measured absorbance of the pure Ni2+(aq) solution at the same wavelength.

Reference

The Job Method outlined above can be justified rigorously, see Synthesis and Technique in

Inorganic Chemistry by R. J. Angelici.

Prelab Assignment

Look up or calculate the molar mass of NiSO4·6H2O. Look up the density and molar mass of
ethylenediamine (you may have to use the IUPAC systematic name of the compound). Calculate the
amounts of solid nickel sulphate hexahydrate and liquid ethylenediamine (volume) necessary to prepare
100 mL of a 0.400 M solution of each.

Procedure

Using solutions of NiSO4·6H2O (0.4 M) and ethylenediamine (0.4 M) prepare solutions having a total
volume of 10 ml in which the mole fraction of ethylenediamine, X, is 0.0, 0.3, 0.4, 0.5,0.6, 0.7, 0.8 and
0.9. Determine the absorbance of each solution at the following wavelengths: 530, 545, 578, 622 and
640 nm.

By appropriate graphical methods, obtain a possible formula to represent the predominant species
present in nickel(II)-1,2-diaminoethane solutions.

Report

Write a journal-style (formal) report. Include your spectra or spectral data, graphs, and copies of lab
notebook pages. In your discussion, give the formulas of all complexes that you identified. Draw the
structures of each of the complexes; the Ni2+ ion prefers to have a coordination number of six. Discuss
the colours of the solutions and how the wavelength absorbed relates to the colour of the solution.

Post-lab Questions

1. Write structural formulas for the three possible products of reaction of ethylenediamine with
Ni(H2O)62+.

2. What does the absorption spectrum of the ligand, ethylenediamine, look like in the visible
region which you used in this experiment. Assign the absorption maxima you used in this
experiment to individual species in the system, where this is possible.

3. What would happen if the values of K2 and K3 were larger than K1? Could you still use Job's
method?

4. From the observed changes in the spectra and knowledge of the complexes present in the
solutions, what can be said about the relative ligand field strengths of en and H2O?

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 5. A reaction occurs between Co(ClO4)2 and LiNO3 in t-butanol to form a complex of the type
[Co(NO3)n](2-n)+. The following absorbance data at a specific wavelength were collected on
solutions made up in the given concentrations of Co(ClO4)2 and LiNO3:

The LiNO3 does not absorb at this wavelength. Use the same methods as in your experiment to
determine the formula of the likely complex and draw a reasonable structure for it. Carefully consider
the structure of the nitrate ion before you draw the structure of the complex. Note that perchlorate ion
(ClO4-) does not coordinate to the cobalt ion. Question: do you think that nitrate could be a bidentate
ligand?

EXPERIMENT 2: SYNTHESIS OF PENTAAMMINECHLOROCOBALT(III) CHLORIDE

The experiment is based on the following reaction:

2CoCl2 + 2NH4Cl + 8NH3 + H2O2 → 2[Co(NH3)5Cl]Cl2 + 2 H2O

Requirements:

1. Cobalt (II) chloride hexahydrate 2. Hydrogen peroxide 3. Ammonium chloride

4. Hydrochloric acid 5. Ammonia 6. Acetone 7. Silver nitrate 8. Nitric acid 9. Ice cold water

10. Ammonium oxalate

Procedure:

1. Dissolve Cobalt (II) chloride (1.8 g) in water (2.5 ml).

2. In a separate flask make slurry of ammonium chloride (5.6 g) in conc. aqueous ammonia (5.6
ml). Add the cobalt solution to the slurry, and stir well.

3. Add hydrogen peroxide (1.1 ml, 30%) with a dropper very slowly (two drops at a time with
caution) while stirring vigorously.

4. Heat the resulting mixture on the steam bath until thick slurry is obtained. If the slurry shows a
blue tint, either the evaporation is proceeding too fast or the hydrogen peroxide was added too
rapidly.

5. Add hydrochloric acid (3 M, 22.5 ml) and heat at 60°C for 10 min.

6. Cool the solution to room temperature and filter in a Buchner funnel with suction. (Use a highly
retentive paper to prevent the fine crystals from passing through.)

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 7. Wash the product with three 2 ml portions of ice water and then with three 2 ml portions
acetone and dry under suction.

8. Transfer the product plus filter paper to a solution of ammonia (2 M, 68 ml). Warm the
resulting solution on a steam bath (60°C maximum).

9. After the entire solid has dissolved, filter the hot solution with suction.

10. Reheat the filtrate on the steam bath with stirring.

11. At five minutes intervals slowly add hydrochloric acid (12 M) three times portions (17 ml
each).

12. Cool the solution to room temperature and filter.

13. Wash the product with water (2 ml) three times followed by three times washing with acetone
(2 ml).

Tasks

1. Calculate the percent yield.

2. Estimate ionic chloride.

Part B: TEST TUBE EXPERIMENTS

1. Add 2 mL saturated ammonium oxalate solution to 2 mL of a 1% solution of the product. Write

a balanced equation for the reaction.

2. Dissolve a pinch of the product in 2 mL water, add 1 mL 12 M HCl and heat to boiling. Add 1
mL KI solution. Record observed colour changes, if any. What conclusions do you draw about
the lability of Co(NH3)5Cl2+ in strong acid on the basis of your observations? Note that the
following reaction is rapid: 2 Co3+ + 3 I- → 2 Co2+ + I3-

3. Heat a pinch of the product with 2 mL 12 M NaOH and note whether any ammonia is given off.
Describe the changes and write a balanced equation.

4. Heat a pinch of the product in a dry test tube over a Bunsen burner until there is no further
change. Describe the changes and identify the products. Write a balanced equation describing
the chemical change.

5. Heat a pinch of the product in a dry test tube over a Bunsen burner until there is no further
change. Describe the changes and identify the products. Write a balanced equation describing
the chemical change.

Post-lab Questions

1. Draw the structures of the complex synthesized and state its point group.

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 6

 2. What type of isomerism does this complex exhibit? Draw the structures of its isomers and name
them.

3. Draw the structure of the tetraaminecarbonatocobalt(III) cation.

4. What can you determine about the structure of a coordination complex by measuring its
conductance in a solution of known concentration?

5. Predict how many ions would be produced per formula unit of the compound Co(NH3)4(NO2)3,
assuming it is monomeric, and contains an octahedrally coordinated cobalt?

6. Write a balanced equation for the oxidation of Co(II) to Co(III) by hydrogen peroxide. Why is
this oxidation process assisted by the presence of ammonia?

7. Outline a method of analysing [Co(NH3)5Cl]Cl2 for its percentage Cl content that the ionic Cl is
much more reactive than that in the coordination sphere.)

8. Outline a method of analysing [Co(NH3)4CO3]NO3 for NH3 and Co content.

EXPERIMNT 3: The Kinetics of Hydrolysis of Pentaamminechlorocobalt(III) Chloride,

[Co(NH3)5Cl]Cl2

In this experiment we will explore the kinetics of hydrolysis of pentaamminechlorocobalt(III) chloride,

[Co(NH3)5Cl]Cl2 in acidic solution. The net equation for the hydrolysis reaction is
[Co(NH3)5Cl]2+ + H2O → [Co(NH3)5(OH2)]3+ + Cl – (1)
Both cobalt complexes in Eq (1) are colored, so we can follow changes in concentration using
spectrophotometry in conjunction with the Beer-Lambert law (commonly known as Beer’s Law). To do
this we need to know the molar absorption coefficient at 550 nm for both [Co(NH3)5Cl]2+ and
[Co(NH3)5(OH2)]3+. Determining these molar absorption coefficients is the purpose of Part A of the
experiment. The wavelength of 550 nm is chosen because at this wavelength the molar absorption
coefficients of the product and the reactant complexes differ the most.
Once sufficient concentration versus time data has been collected, the reaction order in [Co(NH 3)5Cl]2+
and the rate constant k can be determined using either the method of initial rates (Part B, 60oC data) or
the integrated rate equations (Part C, 80oC and 100oC data). The method of initial rates is appropriate
for the 60oC data since at that temperature the reaction is quite slow. The method of initial rates
requires that concentration/time data be collected for the reaction at a number of different initial
concentrations of [Co(NH3)5Cl]2+. In Part B we will run experiments at four different initial
concentrations.
At 80oC and 100oC the reaction is much faster and the reaction quickly proceeds through several half-
lives; thus at these temperatures the integrated rate equations can be used to determine the reaction
order. This method requires only one set of data at each temperature.
Once the rate constant k has been determined at three different temperatures (60oC, 80oC, and 100oC)
an Arrhenius plot can be made of the data. From this plot the Arrhenius parameters are determined.
This is the culmination of Part C.
Since the reaction takes place in acidic solution, we should also establish whether the reaction rate
depends on the concentration of H+. This is the object of Part D.
A. Determination of the Molar Absorption Coefficient ε from a Beer’s Law Plot
The purpose of this experiment is to determine the molar absorption coefficients at 550 nm of the
colored reactant [Co(NH3)5Cl]2+ and the colored product [Co(NH3)5(OH2)]3+. We will begin by

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 7

introducing spectrophotometry and stating Beer’s Law for a single absorbing species. We will then
consider how Beer’s Law is altered when two absorbing species are present.
Spectrophotometry
A simple and accurate method used to determine the concentration of colored solutions is
spectrophotometry. By using a spectrophotometer, such as a Spectronic 20, and the principles of Beer's
Law, it is simple to determine the concentration of an unknown solution from its absorbance.
To define the absorbance A, we first need to define the transmittance T which is the ratio of the
intensity of the light transmitted by a sample I, to the intensity of the light incident on the sample, Io:
I  I 
T ; %T     100%
I0 I0 
If all the light is absorbed by the sample, %T = 0; if no light is absorbed, the %T = 100%. The
absorbance A is defined by the equation
1  I
A  log  log 0 
T   I 
Using this equation, we see that when T = 0.10 (%T = 10%), A = 1.0, and that when T = 1.00 (%T =
100%), A = 0.00. Table 1 shows sets of corresponding values of T, %T, and A. It also gives the
optimum absorbance/transmittance range in which to work.

Table 1. Corresponding values of T, %T, and A.

Transmittance % Transmittance Absorbance
(T) (%T) (A)
0.001 0.1 % 3
0.01 1% 2
0.10 10 % 1

Good range:
0.1 < A < 1
or
80 %T > %T > 10 %T

0.794 79.4 % 0.10

0.977 97.7 0.01
1.00 100 0

Beer’s Law
Beer's Law states
A= lc (2)
where
 Ais the absorbance of the solution at the wavelength λ. It is a dimensionless quantity.
  is the molar absorption coefficient ε (also called the extinction coefficient), for the absorbing
species at the wavelength λ.
 l is the path length of solution through which light must pass (in the cells commonly used l = 1 cm).
 c is the molarity of the absorbing species in the solution.
If Beer’s Law is obeyed, a plot of A versus c for a set of solutions with different concentrations will
Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 8
give a straight line with a y-intercept of zero. The slope of the line gives at the wavelength  at
which the data was collected (since the slope of the line equals l, and l = 1 cm). The units for  are
M-1cm-1.
If at the wavelength is unknown, the first task is to obtain A versus c data for a set of solutions
with different concentrations. is then found by doing a least-squares fit of the data. Then, if the
absorbance of a solution of unknown concentration is measured, Beer’s Law may be used to find the
molar concentration:
A
c 
l 
Beers Law with Two Absorbing Species
In this experiment we cannot assume absorbance is directly proportional to concentration since both a
reactant and a product absorb at 550 nm, and they have different molar absorption coefficients, .
Thus Beer’s Law gives
Atotal,550 = AR,550 + AP,550
= R,550 cR l + P,550 cP l (3)
where
 Atotal,550 is the total absorbance at 550 nm
 R = reactant = [Co(NH3)5Cl]2+
 P = product = [Co(NH3)5(OH2)]3+
 R,550 is the molar absorption coefficient (extinction coefficient) of the reactant (given as 47.5
cm-1M-1 in Ref. 2: you will determine a value experimentally in Part A)
 P,550 is the molar absorption coefficient (extinction coefficient) of the product (given as 25.4
cm-1M-1 in Ref 2 and as 21.0 cm-1M-1 in Ref 1: you will determine a value experimentally in
Part A)
 cR = concentration of R
 cP = concentration of P
 l = cell path length = 1.0 cm
The Eq(1) reaction stoichiometry gives
cR + cP = cR,0 (thus, cP = cR,0 - cR) (4)
where cR,0 is the initial concentration of the cobalt complex. At t = 0, cR = cR,0 and cP = 0 (since no
reactant has reacted to form product). If the reaction goes to completion, cR = 0, and cP = cR,0. At any
stage of the reaction,
(Atotal, 550   P,550 c R,0 )
cR  (5)
( R,550   P,550 )
This equation is derived by combining Eq (3) and Eq (4), and noting that l = 1. You will be asked
demonstrate this in your report (see the Question 1 for Part A)!

Assumptions Specific to Our Reacting System

We will begin by determining the molar absorption coefficients of both the reactant and product at 550
nm by making Beer’s Law plots. Several assumptions must be made. Since the reaction is extremely
slow at 25oC, we can assume to a good approximation that cR = cR,0 and cP = 0. Thus, Eq(3) reduces to
Atotal,550 = AR,550 = 550,R cR,0 l

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and 550,R is found by plotting A versus cR,0 for a set of initial concentrations of
pentaamminechlorocobalt(III) chloride.
To obtain 550,P, we need to run the reaction at 100oC for a long enough time for the reaction to reach
equilibrium. We then assume that at this point (t = ∞) the reaction has gone to completion, so that cP =
cR,0 and cR = 0. Under these conditions, Eq(3) simplifies to
Atotal,550 = AP,550 = 550,P cR,0 l
Thus 550,P may be found from a Beer’s Law plot of A vs. cR,0 for the set of (t = ∞) solutions obtained
from a set of initial concentrations, cR,0.
Procedure for Part A:
Set up a boiling water bath using a 1000 mL beaker and a hot plate.
Make up a liter of 0.10 M HNO3 to use as the solvent in this experiment (concentrated HNO3 is
approximately 15.8 M). Use the 0.10 M HNO3 solution to make up 100.0 mL of 0.0120 M
pentaamminechlorocobalt(III) chloride in 0.10 M HNO3 (the molar mass of [Co(NH3)5Cl]Cl2 is =
250.45 g mol-1). Use this 0.0120 M stock solution and the 0.10 M HNO3 solution to make 2 identical
sets of solutions as listed in Table 2 in large test tubes (15 mm diameter – they should hold 10 mL or
more). Set 1 is for use at 25oC, and Set 2 for use after heating at 100oC.

Table 2. Solutions needed for Set 1 and for Set 2

Solution Concentration mL of 0.012 M mL of 0.10 M
cR,0 stock solution HNO3
1 0.0120 M 5.0 mL 0 mL
2 4.5 mL 0.5 mL
3 4.0 mL 1.0 mL
4 3.5 mL 1.5 mL
5 3.0 mL 2.0 mL
6 2.5 mL 2.5 mL
7 2.0 mL 3.0 mL
8 1.5 mL 3.5 mL
9 1.0 mL 4.0 mL
10 0.5 mL 4.5 mL

Calculate the concentrations of solutions 2 – 10 in the table for use later in your Beer’s Law plots.
Lightly cork your Set 2 test tubes, and place them in the boiling water bath. Be sure that there is
sufficient water in the bath so that the level of solution in the test tubes is below the level of the water
in the bath. This set of solutions will be used to determine the molar absorption coefficient of the
product (550,P) after heating for 40 minutes and then cooling to room temperature.
Since you need to make accurate measurements with your colorimeter make sure your instrument is
properly set up (consult the directions that came with the instrument!!) and check that you are using a
matched set of cells. Use 0.10 M HNO3 as your blank.
Measure the absorbance of each of your Set 1 solutions at 550 nm at room temperature (approximately
25oC) beginning with the most dilute solution (Solution 10) and working backwards to Solution 1. Use
0.10 M HNO3 as your blank. Make a Beer’s law plot as described in the calculation section below. If
the data is poor, repeat the experiment. If a recording UV/Vis spectrophotometer is available, also
obtain the spectrum of Solution 1, Set 1 from 350 nm to 650 nm.
After approximately 40 minutes remove the Set 2 test tubes from the hot water bath, cool the solutions
to room temperature, and measure the absorbance of each Set 2 solution at 550 nm as above. Make a
Beer’s law plot with the Set 2 absorbance data as described in the calculation section below. If the data

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is poor, repeat the experiment. If a recording UV/Vis spectrophotometer is available, also obtain the
spectrum of Solution 1, Set 2 from 350 nm to 650 nm

Calculations for Part A:

NOTE: You will want to use Microsoft Excel for nearly all of these calculations and graphs!
Use your Set 1 absorbance data to make a Beer’s law plot of A versus cR,0 to obtain R. . Recall that
the slope of the line gives at the wavelength  at which the data was collected (since the slope of the
line equals l and l = 1 cm). The units for  are M-1cm-1. If the data is poor, repeat the experiment.
Use your Set 2 absorbance data to make a Beer’s law plot A versus cR,0 to obtain P. If the data is
poor, repeat the experiment.
Questions for Part A:
1. Show how Eq(5) is obtained from Eq(3) and Eq(4). Note that l = 1 cm.
2. What is meant by a “good” Beer’s Law plot? Did you obtain good Beer’s Law plots for both the
reactant and product? Explain why or why not.
3. Why do you think the kinetic experiments in Parts B - D call for measurements at 550 nm? To
answer this question you will need your UV/Vis absorbance data from 350 nm to 650 nm for both
the reactant (Solution 1, Set 1) and the product (Solution 1, Set 2).
4. Give a critical discussion of the results you obtained including sources of error and suggestions for
improvement of the experimental method.

B. Dependence of the Reaction Order on [Co(NH3)5Cl]2+ using the Method of Initial Rates

There are two general methods to determine the rate law from experimental data. The first is the
method of initial rates which is appropriate when the reaction is relatively slow so that the initial rate v0
may be determined as a function of initial concentrations. The second method, which makes use of
integrated rate equations, is applicable when the reaction is sufficiently fast so that concentration
versus time data may be collected over several half-lives. The half-life of a substance is the time needed
for its concentration to fall to one-half its initial concentration.

In Part B we will run the reaction

[Co(NH3)5Cl]2+ + H2O  [Co(NH3)5(OH2)]3+ + Cl –
at 60oC. Since the reaction is relatively slow at this temperature, we will use the method of initial rates.
The reaction is assumed to have a rate law in the form rate = k [A] m[B] n so that the initial rate is given
by

initial rate = vo = k [A]om [B]on (6)

where in our case A = [Co(NH3)5Cl]2+, and B = H2O. The “o” subscripts in Eq(6) indicate “initial” or t
= 0 values. Since water is in large excess, its concentration won’t change appreciably as the reaction
proceeds. Thus [B] = [H2O] = constant, and Eq(6) simplifies to
vo = k' [A]om with k' = k [B]on (7)
where k' is a constant. This equation may be written in logarithmic form:
ln v0  m ln[ A]0  ln k' (8)

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In Eq(8) m and ln k' are constants. Thus Eq(8) has the form of an equation for a straight line y = m x +
b. If we plot ln v0 versus ln[A]0, the slope of the plot gives us the reaction order m, and the y-intercept
is ln k'. Note that in the notation used in this lab, [A]0 = cR,0.
The discussion above demonstrates that if can determine the initial rate vo for different values of cR,0
(with all other concentrations held constant), we can find the reaction order m. In our case we will
determine the initial rate v0 at four different initial concentrations of cR,0 = [Co(NH3)5Cl]2+; the
concentration of B = H2O is constant as outlined above since H2O is in such large excess.
Procedure for Part B:
This experiment is usually a group project. Set up a constant temperature water bath at 60.0oC. For this
you will need a large container full of water, an accurate thermometer, a thermo-regulator/heater, an
additional regulated heater coil, copper tubing for cooling, and assorted rubber tubing. Begin with very
hot water from the tap to speed up the time needed to get to 60.0oC. With Sweet Briar’s equipment,
both heaters must be on to maintain 60.0oC. The heater/regulator should be set to setting B on the back,
and to 60.0oC using the fine adjust setting on the front. Once 60.0oC is reached, you will need to lower
the second heater to approximately level 6.
Fill four 100 mL volumetric flasks with 0.10M HNO3 (concentrated HNO3 is approximately 15.8M).
Immerse the flasks in the hot water bath and let them equilibrate for at least 15 minutes. Check
carefully to insure that the hot water bath is maintaining a constant temperature of 60.0 ± 0.1 oC.
Fill an insulated container with crushed ice, and place small test tubes in the ice to cool. As you take
samples from your reacting mixture, transfer them to these cold test tubes.
Set up the spectrophotometer to record the absorbance at 550 nm. Check that you are using a set of
matched cells. Use 0.10 M HNO3 as your blank.
Weigh out sufficient pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2 (molar mass = 250.45
g) to give 0.0120 M, 0.0100 M, 0.0080 M, and 0.0060 M complex concentration in the 100 mL nitric
acid solutions.
Add the complex to the first (0.0120 M) flask, mix well, record the time of mixing for the flask, and
return the flask immediately to the hot water bath. Take a 3 mL aliquot of the 60oC reaction mixture
immediately after mixing and transfer it to a cold test tube set in the crushed ice. Repeat at roughly 8
minute intervals.
Follow the same procedure for the other flasks. Keep a careful record of the time (to the nearest
minute) at which each aliquot is taken. Continue to take samples for 40 minutes.
Allow the samples to cool for 5 or more minutes on ice, and then measure the absorbance of each
solution at 550 nm. To prevent fogging, you should let each cuvette reach room temperature before
taking a reading. Fogging of the windows will lead to unreliable data. Cuvettes must be clean and dry.
Calculations for Part B:
NOTE: You will want to use Microsoft Excel for nearly all of these calculations and graphs!
Use Eq(5) with your absorbance readings Atotal,550 and the extinction coefficients found in part A to find
cR, the concentration of the reactant [Co(NH3)5Cl]2+ at each time t, for each of the four solutions. Then
graph cR versus t for each of the four initial concentrations cR,0 you studied. Initial rate data should give
linear graphs (or the reaction is too fast for this method, or the data is poor). Do a least squares fit of
each graph to determine the slope and intercept. In each case the initial rate v0 is minus the slope of the
graph:
c
v0   R   (slope of cR versus t plot) (9)
t
Make a table of the four initial concentrations cR,0 and the corresponding initial rates v0. You may need
to get some of these values from other students in the lab.
Use this data and the method described following Eq(8) above to determine the reaction order in
[Co(NH3)5Cl]2+ and the rate constant k'.

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 12

Questions for Part B:
1. What order is the reaction in [Co(NH3)5Cl2+]? In other words, what is m in the equation rate = k'
[Co(NH3)5Cl2+]m ? Justify your answer.
2. What is the rate constant k' for the reaction at 60oC? In other words, what is k' in the equation rate =
k' [Co(NH3)5Cl2+]m ? Justify your answer.
3. Calculate the half-life t1/2 for the reaction. Over how many half-lives did you collect data?
4. Why was the method of initial rates used here rather than the integrated rate equation method?

C. Determination of the Arrhenius Parameters for [Co(NH3)5Cl2+] Hydrolysis

It is well known that reaction rates increase with temperature. This occurs because rate constants k
increase as the temperature increases. It has been found experimentally that rate constant data for many
simple reactions follows the Arrhenius equation
Ea

k  Ae RT
(10)
where
 k is the rate constant for the reaction
 Ea is the activation energy
 A is the pre-exponential factor (also called the frequency factor)
 T is the temperature in Kelvin
 R is the gas constant in energy units
The parameters Ea and A are known as the Arrhenius parameters. Eq(10) may be written in logarithmic
form
E a 1 
ln k    ln A (11)
R T 
The goal of Part C is to determine the Arrhenius parameters for the hydrolysis of
pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2. Concentration cR versus time t data is first
obtained at three different temperatures, 60.0oC, 80.0oC, and 100.0oC. The concentration cR versus time
t data is then analyzed using the integrated rate equation method. You may assume that the reaction is
first-order so that the data is expected to fit the first-order rate equation, ln[A] = - k t + ln[A]0. In the
notation of this experiment, this becomes
ln c R  k' t  lnc R, 0 (12)
Thus a plot of ln cR versus t should give a straight line plot. The slope of the plot is -k', so the rate
constant is found by taking the negative of the slope:
k' = - (slope of first-order graph) (13)

Once the rate constants k' of each run have been determined, the Arrhenius parameters may be found.
Note that in our case k' should be substituted for k in the Arrhenius equation. Since Eq(11) is in y = mx
+ b form, we see that if we determine the rate constant k at a number of different temperatures T, we
can plot lnk versus 1/T and expect a straight line plot. A lnk versus 1/T plot is called an Arrhenius plot.
E
The activation energy Ea can be determined from the slope of the Arrhenius plot (the slope =  a ),
R
and the pre-exponential factor A can be found from the y-intercept of the plot (lnA).
Procedure for Part C:
Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 13
This experiment is usually a group project. The group needs to set up constant temperature water baths
at 60.0oC, 80oC, and near 100oC (i.e., the temperature of a boiling water bath):
 See part B above for the materials necessary for the 60.0oC water bath.
 Our thermo-regulators will not maintain 80oC, so for this temperature you will need to use an
electric heat bath, an additional regulated heater coil, and some sort of stirrer. You will also need to
monitor the temperature and make manual adjustments as required!
 A boiling water bath should give a temperature very close to 100oC; you will need to add boiling
water periodically to keep your reaction flask immersed.
Begin each run by transferring 75.0 mL of 0.10 M HNO3 into a 100 mL volumetric flask (concentrated
HNO3 is approximately 15.8 M). Immerse the flask in the appropriate hot water bath (60.0oC, 80oC, or
near 100oC), and let it equilibrate for at least 15 minutes. Check frequently to insure that the hot water
bath is maintaining a constant temperature.
Set up the spectrophotometer to record the absorbance at 550 nm. Check that you are using a set of
matched cells. Use 0.10 M HNO3 as your blank.
Fill an insulated container with crushed ice, and place small test tubes in the ice to cool. As you take
samples from your reacting mixture, transfer them to these cold test tubes.
Weigh out sufficient pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2 (molar mass = 250.45
g) to give a 0.0120 M complex concentration in the 75.0 mL nitric acid solutions.
Specific directions for 60.0oC, 80.0oC, or 100.0oC runs:
 At 60.0oC: Add the complex to your 60.0oC flask, mix well, record the time of mixing for the flask,
and return the flask immediately to the water bath. Take a 3 mL aliquot of the reaction mixture
immediately after mixing and transfer it to a cold test tube set in the crushed ice. Take samples
every 15 minutes for a total time of 2.5 hours.
 At 80oC: Add the complex to your 80o flask, mix well, record the time of mixing for the flask, and
return the flask immediately to the water bath. Take a 3 mL aliquot of the reaction mixture
immediately after mixing and transfer it to a cold test tube set in the crushed ice. Take samples at
roughly 3 to 5 minute intervals (shorter intervals initially) for a total of 35 to 40 minutes.
 At 100oC: Pour the 75.0 mL of 0.10 M HNO3 at 100oC into a hot beaker. Add the complex, mix,
and return the mixture to the volumetric flask. Return the flask immediately to the water bath, and
record the time of mixing. Take a 3 mL aliquot of the reaction mixture immediately after mixing
and transfer it to a cold test tube set in the crushed ice. Take samples at 2 to 3 minute intervals for a
total of 15 minutes.
Keep a careful record of the time (to the nearest minute) at which each aliquot is taken. Check the
water baths regularly to make sure the temperature is holding reasonably constant at the desired
temperature.
Allow the samples to cool for 5 or more minutes on ice, and then measure the absorbance of each
solution at 550 nm. To prevent fogging, you should let each cuvette reach room temperature before
taking a reading. Fogging of the windows will lead to unreliable data. Cuvettes must be clean and dry.
If the data is poor, repeat the experiment making modifications to allow greater precision in results.

Calculations for Part C:

NOTE: You will want to use Microsoft Excel for nearly all of these calculations and graphs
For each of your runs, use Eq(5) with your absorbance readings Atotal, 550 and the molar absorption
coefficients found in part A to find cR, the concentration of the reactant [Co(NH3)5Cl]2+ at each time t.
Those working at 100oC may find that the absorbance becomes essentially constant towards the end of
the run. At this point the reaction has reached completion and cR  0.0 . Do not include the points for
which cR  0.0 in your data fits.

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 14

Next make first-order plots (ln cR versus t ) of your cR versus t data, and determine k' for each run from
your least squares fit. See the discussion following Eq(12) for the method.
Also make second-order plots (1/cR versus t) of your data for use in answering the questions below.
Note: In the notation of this experiment, the second-order integrated rate equation is

1 1
 k' t  (14)
cR c R,0

Make a table of the three temperatures T (in Kelvin) and the corresponding first-order rate constants k'.
You will need to get some of these values from other students in the lab. Your goal in this section is to

determine the Arrhenius parameters for the reaction. Make an Arrhenius plot and determine the
Arrhenius parameters, A (the pre-exponential factor) and Ea (the activation energy) for the reaction.
See Eq(11) and the discussion following Eq(13) for the method.
Questions for Part C:
1. Answer this question only for the data you actually collected (runs at 60.0oC, 80.0oC, or 100.0oC).
(a) Does your data indicate that the reaction is first order in concentration of [Co(NH3)5Cl]2+? To
answer this question you need to compare the quality of your first-order and second-order least-squares
fits. Does your data give a better fit to the first-order or the second-order integrated rate equation? The
better fit should have an R2 value closer to 1. Also, the initial concentration cR,0 calculated from the y-
intercept should be close to the initial concentration used in your runs. Explain your reasoning.
(b) What is the rate constant k’ and the half-life t1/2 for the reaction at your temperature? Over how
many half-lives did your collect data?
(c) Is the reaction sufficiently fast so that fits to the integrated rate equations are meaningful? Explain
your reasoning.

2. What are the Arrhenius parameters, A (the pre-exponential factor) and Ea (the activation energy), for
the reaction? Be sure to affix appropriate units.

D. Dependence of the Reaction Order on [H+] using the Method of Initial Rates

Procedure for Part D:

Set up a constant temperature water bath at 60.0oC. For this you will need a large container full of
water, an accurate thermometer, a thermoregulator/heater, an additional regulated heater, copper tubing
for cooling, and assorted rubber tubing. Begin with very hot water from the tap to speed up the time
needed to get to 60.0oC.
Fill two 100 mL volumetric flasks with 0.10M and 0.30M HNO3, respectively (concentrated HNO3 is
approximately 15.9M). Immerse the flasks in the hot water bath and let them equilibrate for at least 15
minutes. Check carefully to insure that the hot water bath is maintaining a constant temperature of
60.0 ± 0.1 oC.
Fill an insulated container with crushed ice, and place small test tubes in the ice to cool. As you take
samples from your reacting mixture, transfer them to these cold test tubes.
Set up the spectrophotometer to record the absorbance at 550 nm. Use 0.10 M HNO3 as your blank.
Weigh out sufficient pentaamminechlorocobalt(III) chloride, [Co(NH3)5Cl]Cl2 (molar mass = 250.45
g) to give 0.0120 M complex concentration in the 100 mL nitric acid solutions. Add the complex to the
flasks, mix well, record the time of mixing, and return the flasks to the hot water bath.

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 15

Take a 3 mL aliquot of each reaction mixture immediately after mixing and transfer it to a cold test tube
set in the crushed ice. Repeat at roughly 15 minute intervals. Keep a careful record of the time (to the
nearest minute) at which each aliquot is taken. Continue to take samples for 2 or more hours.
Allow the samples to cool for 5 or more minutes on ice, and then measure the absorbance of each
solution at 550 nm. To prevent fogging, you should let each cuvette reach room temperature before
taking a reading. Fogging of the windows will lead to unreliable data. Cuvettes must be clean and dry.
Calculations for Part D:
Use Eq(5) with your absorbance readings Atotal, 550 and the molar absorption coefficients found in part A
to find cR, the concentration of the reactant [Co(NH3)5Cl]2+ at each time t, for each of the four
solutions. Assume that the reaction is first order in the concentration of the complex ion,
[Co(NH3)5Cl2+], and that [H+] is constant since it is not consumed in the reaction. Thus the rate law
should have the form, rate = k [complex][H+]n = kobs [complex] where kobs = k [H+]n. Your goal is to
determine the value of n (n = 0, 1, 2 or whatever) by determining the dependence of kobs on [H+].
Begin by making appropriate first-order plots of ln[complex] = ln(cR) versus t for both your [H+] =
0.10 M and [H+] = 0.30 M runs. Obtain kobs from each plot. Finally use these results and your H+
concentrations to determine n in kobs = k [H+]n.
Questions for Part D:
1. Does your data at each of the fixed (0.10M and at 0.30M) nitric acid concentrations indicate that the
reaction is first order in concentration of [Co(NH3)5Cl]2+? Is the reaction sufficiently fast that you can
answer this question with your data? Explain your reasoning.
2. What order is the reaction in [H+]? In other words, what is n in the equation rate = k
[Co(NH3)5Cl2+]m [H+]n (where m is presumed to be 1)? Justify your answer.
3. What is the rate constant k for the reaction? In other words, what is k in the equation rate = k
[Co(NH3)5Cl2+]m [H+]n? Justify your answer.

EXPERIMENT 4: PREPARATION AND ANALYSIS OF POTASSIUM TRIOXALATO

FERRATE(III) TRIHYDRATE K3[FE(C2O4)3]·3H2O

Step One: Preparation of Ferrous Oxalate

Weigh the vial containing the sample of ferrous ammonium sulphate, (NH4)2SO4·FeSO4·6H2O.
Transfer the ferrous ammonium sulphate to a beaker containing 25 mL of warm water acidified with 1
mL dilute 3 M H2SO4. Dry the vial and weigh the empty vial. Record the mass of ferrous ammonium
sulphate used. To this solution add 25 mL of oxalic acid solution (5 g/50 mL). Cautiously heat the
solution to boiling on a hot plate, continuously stirring the solution to avoid bumping. Remove and
then allow the precipitate to settle. Decant and discard the clear supernatant liquid (avoid loss of
precipitate). Stir the remaining precipitate with 25 mL of hot water, the solubility of FeC2O4·2H2O is
0.022 g/100 mL in cold water and 0.026 g/100 mL in hot water. Decant and discard the wash liquid.
Add 25 mL of hot water to the precipitate and stir, then filter by suction using a small Büchner funnel
and wash the precipitate thoroughly with small portions (10-20 mL) of hot water. Finally rinse with 20
mL of acetone. Weigh the final product.

Step Two: Preparation of K3[Fe(C2O4)3]·3H2O

Suspend the washed and dried ferrous oxalate in 30 mL of warm solution containing 3.5 g of potassium
oxalate (K2C2O4·H2O). Place this solution in an ice bath and add slowly with continuous stirring 7-10
mL of 30% H2O2 in very small portions, then heat the mixture to boiling and dissolve the precipitate by
Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 16
adding in one portion 7 mL of a solution of oxalic acid (containing 2.5 g/25 mL). A further 3 mL is
then added drop by drop using an eye dropper (an excess of oxalic acid is to be avoided). The liquid
should be near the boiling point while these additions are being made.

Filter through a Büchner funnel. Transfer the hot solution to a clean beaker and while still hot, add to
the filtrate 15 mL of 95% ethanol and re-dissolve any precipitated crystals by gently heating. Then
store the solution in a dark cupboard for crystallization.

After crystallization has occurred, filter with suction and wash the product on the filter paper with 20
mL of an equi-volume mixture of ethanol and water and finally with 20 mL of acetone. Draw air
through the precipitate for several minutes. Weigh the dry crystals. K3[Fe(C2O4)3]·3H2O is highly
photosensitive. The bright green crystals on exposure soon become covered with a yellow powder of
ferrous oxalate.

Oxidation - Reduction Titration

Potassium permanganate (KMnO4) is commonly used as an oxidizing agent and can be reduced in
different ways, depending on the H+ concentration of the reaction mixture. In neutral or basic solutions
a mixture of products may result, chiefly solid MnO2 and green manganate ion, MnO42–. In acid
solution, however, the reduction goes by one course only, the half-reaction being:

Preparation of a 0.02 M KMnO4 Solution

Weigh out approximately 1.2 - 1.40 g of potassium permanganate and add it to approximately 350 mL
of boiled distilled water in a 600 mL beaker. Stir the solution well to dissolve all the crystals. Cover the
solution with a watch glass and keep the solution near the boiling point for 20 minutes. Allow the
solution to cool slightly, and then filter the solution through a non-reducing filter (glass wool) placed in
the neck of a short stemmed funnel. The KMnO4 solution can be stored in a plastic bottle.

Standardization of KMnO4 Solution

Note 1: The MnO4– / C2O42- reaction is slow at room temperature and hence the titration is carried
out at elevated temperatures. Even at higher temperatures the reaction starts slowly, but the rate
increases as Manganous (Mn2+) ion, which acts as a catalyst, is formed. Since the Mn2+ ion is a
product of the reaction itself, the reaction is called "autocatalytic".

Note 2: With deeply coloured solutions like permanganate, it may be necessary to read the top of the
meniscus since it is difficult to see the bottom of it. Weigh accurately, to the nearest tenth of a
milligram, three samples each in the range 0.18 - 0.22 g of sodium oxalate (Na2C2O4) into clean 250

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 17

mL Erlenmeyer flasks. To each sample add 60 mL of water and 10 mL of 3 M (dilute) sulphuric acid.
Titrate each solution as follows. Heat the contents of the Erlenmeyer flask to 80 - 90°C, but not over
90°C. (Do warm all trials at the same time). Rinse the thermometer with 1 to 2 mL of distilled water
and remove and titrate the hot solution with the KMnO4 solution. Add several mL of KMnO4 solution
slowly to initiate the reaction then larger portions may be added until the endpoint is approached. Then
slow the addition of titrant to avoid overshooting the faint pink endpoint. The solution should be
swirled while additions are being made. The reaction is represented by the following reactants and
products in acid solution.

Balance the equation and calculate the molarity of your permanganate solution.

Characterization of the Green Crystals

A. % H20 in the green crystals

Weigh 0.7-1.0 g (±0.0001g) of the complex salt into a pre-weighed evaporating dish. Label or mark the
dish so you can identify it and place the evaporating dish and complex salt in an oven set at 110°C for
approximately 45 minutes. Cool the dish and contents and weigh to the nearest ±0.1 mg. Calculate the
% H20 in the crystals. Use the dried crystals for part C.

B. % of Oxalate in the green crystals using Potassium Permanganate

Proceed with the prepared salt complex. Weigh out 3 samples of the complex salt in the weight range
of 0.18 - 0.22 g (on the analytical balance) into clean 250 mL Erlenmeyer flasks. Dissolve each sample
in 60 mL H2O, 10 mL of 3 M (dilute) sulphuric acid and heat each sample to 80-90°C but not over 90°
and titrate with standardized potassium permanganate until the first appearance of a faint permanent
pink colour occurs. Calculate the percent oxalate in the complex salt.

C. % of Iron in the green crystals

This procedure should be carried out in the fume hood until the final step. To the evaporating dish and
dried crystals, add cautiously approximately 3 mL concentrated H2SO4 (sulphuric acid) and cover with
a watch glass. In the fume hood, using a hotplate, gently heat the dish and contents for several minutes
until the bubbling resulting from the decomposition of the oxalate ion ceases rather abruptly. Allow the
evaporating dish and contents to cool in the hood. Then pour the colourless (anhydrous) ferric sulphate
from the dish into an Erlenmeyer flask and rinse the watch glass. Add approximately 25 mL of distilled
H2O to the Erlenmeyer flask and heat the flask and contents to boiling. The milky solution will
gradually turn to a clear pale yellow solution. Then add small portions of zinc dust and continue to
cautiously heat the flask until the yellow colour disappears from the solution. Heat for approximately 1
minute beyond this point. The hot mixture is filtered through #1 Whatman paper into a clean flask and
rinsed to achieve complete transfer. This solution is then titrated with standardized KMnO4solution

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 18

until a faint pink/orange endpoint appears. The % Fe in the green crystals can then be calculated. Use
the original mass of the green crystals before they were dried in the oven.

Data Sheet

1. Step one: Preparation of Ferrous oxalate

Mass of Ferrous ammonium sulphate·hexahydrate used ________ g

Mass of 250mL beaker _________ g

2. Step two: Preparation of Potassium trioxalato ferrate (III) trihydrate

Mass of ferrous oxalate·dihydrate used to start the reaction _________ g

Mass of Potassium Tris-oxalatoferrate (III) trihydrate produced _______ g (Green Crystals)

Part B: Standardization of the prepared KMnO4 solution

Trial #1 Trial #2 Trial #3 Trial #4

Mass Na2C2O4 & container (g) ___________ ___________ ___________ ____________

Mass container (g) ___________ ___________ ___________ ____________

Mass of Na2C2O4 used (g) ___________ ___________ ___________ ____________

Initial Volume KMnO4 ___________ ___________ ___________ ____________

Final Volume KMnO4 ___________ ___________ ___________ ____________

Volume of KMnO4 used (mL) __________ ___________ __________ ____________

Molarity of KMnO4 _________M, _________ M, _________M, _________M

Average Molarity of KMnO4 __________ M

Analysis of the of Potassium trioxalato ferrate (III) trihydrate

A. % H2O in the Green Crystals:

Mass of the evaporating dish _____________g

Mass of green crystals & the evaporating dish before heating _____________g

Mass of green crystals before heating _____________g

Mass of green crystals & the evaporating dish after heating _____________g

Mass of green crystals after heating _____________g

B. % oxalate ion in the Green Crystals:

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 19

 Trial #1 Trial #2 Trial #3 Trial #4

Mass crystals & container (g) ___________ ___________ ___________ ____________

Mass container (g) ___________ ___________ ___________ ____________

Mass green crystals used (g) ___________ ___________ ___________ ____________

Initial Volume KMnO4 ___________ ___________ ___________ ____________

Final Volume KMnO4 ___________ ___________ ___________ ____________

Volume of KMnO4 used (mL) __________ ___________ ___________ ____________

C. % of Iron in the Green Crystals:

Mass of green crystals before heating ______________g

Initial Volume KMnO4 ___________ mL

Final Volume KMnO4 ___________ mL

Volume of KMnO4 used (mL) ___________ mL

Show example calculations on the back of the report sheets or append separate sheets.

Theoretical Yield (Show your work): Using your experimental mass of starting material for each
calculation.

Per Cent Yield (Show your work):

Balanced titration and reaction equations for: Fe3+ & Zn; MnO4- & C2O42-; and Fe2+ & MnO4- .

Molarity of KMnO4:

Average Molarity of KMnO4 = __________ M.

Experimental weight % of C2O42- in the prepared green crystals:

Average weight % of C2O42-

Experimental weight % of Fe in the prepared green crystals:

Experimental weight % H2O in the prepared green crystals:

Experimental weight % K in the prepared green crystals:

Formula Weight % of Fe, H2O, C2O42-, K in K3[Fe(C2O4)3]·3H2O:

% Deviationof the Experimental weight % values compared to Formula Weight % values:

Conclusions:

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 20

Pre-Lab Questions

1. Write the chemical formula of potassium permanganate.

2. A mixture of 5.00 g of H2(g) and 10.00 g 02(g) is ignited. Water forms according to the following
reaction: 2H2 (g) + O2 (g) → H2O (g) Which is the limiting reagent? How much water will be
produced?

3. Name this compound: K3[Fe(C2O4)3]·3H2O

4. Write the chemical formula for ferrous oxalate dihydrate.

5. Describe the proper procedure for diluting 18 M concentrated sulphuric acid to prepare 100 mL of 3
M sulphuric acid.

6. A solution of potassium permanganate was prepared by dissolving 21.08 g of KMnO4 in water and
diluting to a total volume of 800mL. What is the molarity of the prepared solution?

7. Is oxalic acid a liquid or a solid under normal laboratory conditions?

8. Is oxidation or reduction occurring in the following reaction? Indicate why.

MnO4- + 8 H+ + 5 e– → Mn2+ + 4 H2O

9. DDT (dichlorodiphenyltrichloroethane) is an insectide banned in Canada because it is hazardous to

fish, birds and humans. The reaction for its preparation is;

2 C6H5Cl (chlorobenzene) + C2HOCl3 (chloral) → C14H9Cl5 (DDT) + H2O

If 450 g of chlorobenzene reacts with 899 g of chloral calculate (a) the theoretical yield of DDT in
grams and (b) the % yield if 650 g of DDT is actually isolated.

10. What colour change occurs at the endpoint of the permanganate - oxalate reaction?

11. Why should potassium permanganate be handled carefully?

12. What is the catalyst used in the permanganate - oxalate reaction?

13. What is the colour of ferrous oxalate?

14. What colour are the crystals of K3[Fe(C2O4)3]·3H2O?

15. Why are you analysing the crystals of K3[Fe(C2O4)3]·3H2O?

Dr. MBOM D. YUFANYI UBa Lectures October 2016 Page 21