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Print the entire packet single-sided and bring

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Lab Packet
1120L

Grote 306
Fall 2017

1
CHEMISTRY 1120L SCHEDULE

Fall 2017
DATES ACTIVITY

Aug. 21 NO LAB MEETING

Aug. 28 LAB 1: Safety, Math/Chemistry Review, Notebook Check

Sept. 4 NO LAB LABOR DAY

Sept. 11 LAB 2: Determining the Concentration of a Solution: Beers Law

Sept. 18 LAB 3: Enthalpy Change for a Chemical Reaction

Sept. 25 LAB 4: Complexometric Titration of Magnesium

Oct. 2 LAB 5: Chemical Equilibrium

Oct. 9 EXAM 1

Oct. 16 NO LAB FALL BREAK

Oct. 23 LAB 6: Identification of a Weak Organic Acid

Oct. 30 LAB 7: Qualitative Analysis (Part A)

Nov. 6 LAB 8: Qualitative Analysis (Part B)

Nov. 13 LAB 9: Oxidation States of Uranium

Nov. 20 LAB 10: Rates of Reaction

Nov. 27 EXAM 2**

Quizzes are due on UTCLearn by 11:59:59 p.m. the day before that lab is performed.

**Please Note!! CHEM 1120L (lab only) exam 2 is given during lab time and NOT during the final
exams week.

Unexpected events: It is possible that weather or other events will cause the university to close. If the
university is closed when your lab is scheduled to begin, that days lab will be cancelled. You do not
need to join your class in progress as instructed by the university if the entire lab cannot be attended.
You will be notified by your instructor through UTCLearn what changes in the schedule will occur due to
the event.

2
UTC Department of Chemistry Safety Rules

It is the policy of the Department of Chemistry to provide a safe environment for students and faculty involved in
laboratory work. The chemistry staff will indicate hazards associated with individual assignments and explain the
use of safety equipment available in the laboratories. However, it is the responsibility of each student to be safety
conscious, to recall and observe safety warnings, and to work in such a manner that his or her actions do not result
in injury to any person in the laboratory. The University does not routinely carry insurance for students. If a student
wishes University insurance coverage, he or she should contact the Student Health Services, 205 Maclellan Gym,
425-2266. The following general rules of safety have been adopted by the Department of Chemistry:

(1) Approved chemical splash goggles (not safety glasses) must be worn in laboratories where chemical
work is being done.

(2) Students must conduct themselves in a careful, professional manner in the laboratory.

(3) All warning signs and statements must be obeyed.

(4) All accidents, injuries, and fires must be reported immediately to the laboratory instructor.

(5) Chemicals for disposal must be placed in the appropriate container designated by the lab instructor.

(6) Drink containers are not permitted out on laboratory benches (they must be put away). Eating and
drinking in laboratories is not permitted.

(7) Students, other than laboratory assistants, are not permitted in stock rooms.

(8) Unauthorized experiments are not permitted.

(9) Chemicals and other materials are not to be removed from laboratories without the consent of the
laboratory instructor.

(10) Safe functioning in the laboratory requires concentration. To that end, the use of cell phones, for either
texting or voice communication, or other listening devices such as MP3 players are not permitted during
the laboratory period.

(11) Closed toe shoes (not sandals, flip-flops, etc.) should be worn at all times in the laboratory. Gloves and
lab aprons are available for use in laboratories and may be required for certain experiments in specific
laboratories.

(12) Students should learn the location and operation of fire extinguishers and safety showers.

(13) Students should be aware of the purpose and location of the departments Chemical Hygiene Plan
containing the standard operating procedures (SOP) for the laboratories.

(14) Anyone deliberately violating safety rules may be asked to leave the lab and given a zero for that lab.

MEDICAL EMERGENCY INFORMATION


Any special medical problems that your professor should be aware of: ___________________________________
____________________________________________________________________________________________
Emergency Contact (name & phone number):
_______________________________________________________________

I have read this page and I will observe the departmental safety rules in my laboratory work.
________________________________ _____________________________________ _________________
Print Name Signature Date
3
CHEM 1120L
LAB ATTENDANCE POLICY

Last minute changes and safety instructions will be announced at the beginning of each lab. One point out of 10
possible points will be deducted from your report score if you are late (up to 10 minutes). After 10 minutes,
you will not be allowed to enter the laboratory or complete the assignment. It will be considered an absence.
It will be your responsibility to read the hazards posted on the whiteboard in the lab if you enter after the safety
instructions have been announced. You must have your report sheet stamped by the time clock when entering the
lab (Gr 306, left door, nearest the elevator). There are no laboratory make-up sessions.

One lab absence incurs no penalty, since the lowest report grade is dropped from the final grade calculations. If
you miss more than one lab, you will incur a 16 point penalty (5% of the maximum point total in the class) per lab
session in addition to the points lost for the missed report. For example, if two labs have been missed, then the
result is a lowering of the final course total by 26 total points (8%). Each successive miss will lower the maximum
possible points by an additional 26 points (8%). The table below breaks down how this policy affects your highest
possible percentage based on missed lab meetings.

Absences Penalty Loss of report points Maximum total points possible (%)
0 0 0 330/330 (100%)
1 0 0 330/330 (100%)
2 -16 -10 304/330 (92%)
3 -32 -20 278/330 (84%)
4 -48 -30 252/330 (76%)
5 -64 -40 226/330 (68%)
6 -80 -50 200/330 (60%)

Since lecture and lab are co-requisites, if one is dropped the other should also be dropped. You may speak with
your instructor about exceptions. However, if you fail one and not the other, you can repeat the one you failed
the following semester without repeating the one that you successfully completed (at least a C grade).

I have read this attendance policy and I understand the consequences of missing lab.

_____________________________ ____________________________ _________________


Print Name Signature Date

4
UTC Department of Chemistry Safety Rules

It is the policy of the Department of Chemistry to provide a safe environment for students and faculty involved in
laboratory work. The chemistry staff will indicate hazards associated with individual assignments and explain the
use of safety equipment available in the laboratories. However, it is the responsibility of each student to be safety
conscious, to recall and observe safety warnings, and to work in such a manner that his or her actions do not result
in injury to any person in the laboratory. The University does not routinely carry insurance for students. If a student
wishes University insurance coverage, he or she should contact the Student Health Services, 205 Maclellan Gym,
425-2266. The following general rules of safety have been adopted by the Department of Chemistry:

(1) Approved chemical splash goggles (not safety glasses) must be worn in laboratories where chemical
work is being done.

(2) Students must conduct themselves in a careful, professional manner in the laboratory.

(3) All warning signs and statements must be obeyed.

(4) All accidents, injuries, and fires must be reported immediately to the laboratory instructor.

(5) Chemicals for disposal must be placed in the appropriate container designated by the lab instructor.

(6) Drink containers are not permitted out on laboratory benches (they must be put away). Eating and
drinking in laboratories is not permitted.

(7) Students, other than laboratory assistants, are not permitted in stock rooms.

(8) Unauthorized experiments are not permitted.

(9) Chemicals and other materials are not to be removed from laboratories without the consent of the
laboratory instructor.

(10) Safe functioning in the laboratory requires concentration. To that end, the use of cell phones, for either
texting or voice communication, or other listening devices such as MP3 players are not permitted during
the laboratory period.

(11) Closed toe shoes (not sandals, flip-flops, etc.) should be worn at all times in the laboratory. Gloves and
lab aprons are available for use in laboratories and may be required for certain experiments in specific
laboratories.

(12) Students should learn the location and operation of fire extinguishers and safety showers.

(13) Students should be aware of the purpose and location of the departments Chemical Hygiene Plan
containing the standard operating procedures (SOP) for the laboratories.

(14) Anyone deliberately violating safety rules may be asked to leave the lab and given a zero for that lab.

MEDICAL EMERGENCY INFORMATION


Any special medical problems that your professor should be aware of: ___________________________________
____________________________________________________________________________________________
Emergency Contact (name & phone number):
_______________________________________________________________

I have read this page and I will observe the departmental safety rules in my laboratory work.
________________________________ _____________________________________ _________________
Print Name Signature Date
5
CHEM 1120L
LAB ATTENDANCE POLICY

Last minute changes and safety instructions will be announced at the beginning of each lab. One point out of 10
possible points will be deducted from your report score if you are late (up to 10 minutes). After 10 minutes,
you will not be allowed to enter the laboratory or complete the assignment. It will be considered an absence.
It will be your responsibility to read the hazards posted on the whiteboard in the lab if you enter after the safety
instructions have been announced. You must have your report sheet stamped by the time clock when entering the
lab (Gr 306, left door, nearest the elevator). There are no laboratory make-up sessions.

One lab absence incurs no penalty, since the lowest report grade is dropped from the final grade calculations. If
you miss more than one lab, you will incur a 16 point penalty (5% of the maximum point total in the class) per lab
session in addition to the points lost for the missed report. For example, if two labs have been missed, then the
result is a lowering of the final course total by 26 total points (8%). Each successive miss will lower the maximum
possible points by an additional 26 points (8%). The table below breaks down how this policy affects your highest
possible percentage based on missed lab meetings.

Absences Penalty Loss of report points Maximum total points possible (%)
0 0 0 330/330 (100%)
1 0 0 330/330 (100%)
2 -16 -10 304/330 (92%)
3 -32 -20 278/330 (84%)
4 -48 -30 252/330 (76%)
5 -64 -40 226/330 (68%)
6 -80 -50 200/330 (60%)

Since lecture and lab are co-requisites, if one is dropped the other should also be dropped. You may speak with
your instructor about exceptions. However, if you fail one and not the other, you can repeat the one you failed
the following semester without repeating the one that you successfully completed (at least a C grade).

I have read this attendance policy and I understand the consequences of missing lab.

_____________________________ ____________________________ _________________


Print Name Signature Date

6
Forceps

Stirring Rod

Well Plate
Test Tube

Spatula

Dropper

Test Tube Rack

Wash Bottle

Cooling Tile

Buret Clamp

7
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________

LAB REPORT: Math/Chemistry Review Read Appendix 1 in your text if you need help.

REMEMBER: all of your answers must have the correct units where needed.

1. Perform the following calculation, giving the answer in the correct number of significant digits.
-1
(1.145 x 105 g/mol) (0.0035 mol)/(8.57 x 10 g/mL) = ________________________

2. Convert the following amount to kJ.

34.5 J = _________________

3. An experiment calls for 7.57 g of sugar. You have a sugar solution that is 5.00% by weight (for every 100 g of
solution, there are 5.00 g of sugar). How many mL of the sugar solution will be needed to deliver 7.57 g of sugar?
The density of sugar solution is 1.157 g/mL. The molecular weight of sugar is 342 g/mol.

volume of solution = ______________________

4. Solve for x in the following problems:

log (0.056) = x x = __________________

log (X) = -4.67 X = __________________

5. Solve for y in the following problem: 5.3 x 10-9 = (y)(2y)2

y = _____________________

8
6. Solve for t.

ln(A/B) = -kt where A = 1.00 x 10-2 M, B = 1.65 x 10-2 M,

and k = 4.80 x 10-4 s-1

t = ______________

7. What are the names of the following compounds:

HNO3 _______________________ FeCl3 ______________________

Na2SO4 ______________________ SO3 ______________________

8. What are the chemical formulas for the following compounds?

magnesium carbonate _________________ dinitrogen monoxide __________________

sulfuric acid __________________ sodium acetate __________________

copper (II) hydroxide __________________

9. What is the charge on the metal cation in each of the following compounds?

Al(OH)3 _______ CrBr3 _______

KCl _______ BaSO4 _______

10. Calculate how many g of ammonia will be produced from 9.35 g of nitrogen gas and excess hydrogen using
the following equation:

N2(g) + 3 H2(g) 2 NH3(g)

answer ________________________

11. Balance the following reaction and then write the net ionic equation:

AgNO3(aq) + K2CO3(aq) Ag2CO3(s) + KNO3(aq)

net ionic equation:

9
CHEMISTRY 1120L
Determining the Concentration of a Solution: Beers Law
Required reading: p. 351; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Objectives
1. To learn about Beers Law.
2. To use a colorimeter to plot concentration vs. absorbance.
3. To use data collected from the colorimeter to determine an unknown concentration.

Hazards and Disposal


Copper sulfate solutions are toxic. Wear goggles and dispose of all copper sulfate solutions in a waste beaker.

Background
The primary objective of this experiment is to determine the concentration of an unknown copper(II) sulfate solution. You will
use a Vernier Colorimeter (a side view is shown below) to measure the concentration of each solution. In this experiment, red
light from the LED light source will pass through the solution and strike a photocell. A higher concentration of the colored
solution absorbs more light (and transmits less) than a solution of lower concentration. The Colorimeter monitors the light
received by the photocell as percent transmittance which is then converted into absorbance (A = 2 log(% transmittance)) by
LabQuest.

You will prepare five copper(II) sulfate solutions of known concentration (standard solutions). Each solution is transferred to a
small, rectangular cuvette that is placed into the Colorimeter. The amount of light that penetrates the solution and strikes the
photocell is used to compute the absorbance of each solution. When you graph absorbance vs. concentration for the standard
solutions, a direct relationship should result. The direct relationship between absorbance and concentration for a solution is
known as Beers law. LabQuest will plot the absorbance and concentration for each of the known solutions and determine the
best fit line. You will determine the concentration of an unknown CuSO4 solution by measuring its absorbance with the
Colorimeter. With a graph, you could then read the value of the X axis to determine concentration. However, this can be
determined more accurately using the equation for the line generated by LabQuest. The equation for the line is y = mx + b,
where y is absorbance, m is the slope of the line, x is the concentration, and b is the y intercept. The instrument will give
you y, m, and b, and you must calculate x for your unknown.

Part One
Your first task will be to make your standard CuSO4 solutions. Obtain approximately 20 mL of 0.40 M CuSO4 solution and
distilled water in two separate beakers. Label five clean, dry, test tubes 15. Use your 10 mL graduated cylinder to prepare
five standard solutions according to the chart below. Be very accurate with your measurements! Use a dropper to bring the
level of the liquid in the graduated cylinder to the meniscus as precisely as possible. Thoroughly mix each solution carefully
with a stirring rod. Clean and dry the stirring rod between uses. Rinse the graduated cylinder after using it for the CuSO4
solution before using it to measure the water. Calculate the molarity of each new solution and enter the value in the table on
your report sheet. Have these checked for accuracy before continuing with the experiment!

Test tube 0.40 M CuSO4 Distilled H2O


number (mL) (mL)
1 1.0 4.0
2 2.0 3.0
3 3.0 2.0
4 4.0 1.0
5 5.0 0.0

10
Part Two
Your second task will be to set up, calibrate, and use the Colorimeter to measure the absorbance of your samples.

1. Turn on Vernier computer interface. Connect a Colorimeter to Channel 1 of the Vernier computer interface.

2. Touch the mode button with the stylus. Next, click the tab Timed Based and select Events with Entry. Type
Concentration under name and mol/L under units. Click ok to save and start experiment.

3. Calibrate the Colorimeter


a) Prepare a blank by filling a cuvette full with deionized water. Wipe down the smooth sides of the cuvette with a
Kim wipe. Touch the cuvette on only the ridged sides.
b) Place the blank in the cuvette slot of the Colorimeter and close the lid as indicated in the diagram above. Be certain
the smooth sides of the cuvette are lined up with the arrow.
c) Press the < or > button on the Colorimeter to select the wavelength of 635 nm (Red). Press the CAL button until the
red LED begins to flash and then release the CAL button. When the LED stops flashing, the calibration is complete.

4. Now you are ready to collect absorbance-concentration data for the five standard solutions that you prepared. This
time you will store the readings in the LabQuest to produce a graph to determine the concentration of the unknown sample
given to you by your lab assistant.
a) Touch the green button in the bottom left corner of the screen.
b) Using the solution in Test Tube 1, fill the cuvette full. Wipe the outside with a Kimwipe and place in the
Colorimeter. Close the lid on the Colorimeter.
c) When the absorbance reading stabilizes, click the button next to the green start button, type 0.080 in the edit
box, and press the OK key. The data pair should now be plotted on the graph.
d) Discard cuvette contents into the waste beaker. Using the solution in Test Tube 2, fill the cuvette full. Wipe the
outside and place the cuvette in the device and close the lid. When the absorbance stabilizes, click , type
0.16 in the edit box and press the OK key.
e) Repeat the procedure for Test Tubes 3, 4 and 5 by typing 0.24, 0.32, and 0.40 in the edit box.
f) When you have finished testing the standard solutions, click Red button.
g) Click Analyze, Curve Fit, then Absorbance. Click Choose Fit and select Linear. Hit OK.
h) A best-fit linear regression line will be shown for your five data points. Write down m, b, and Correlation values on
your report sheet.
i) Click the X-Y table button on the top right and record the Absorbance Values.
j) When finished, click the top far left button to get back to the absorbance screen.

5. Determine the absorbance value of the unknown CuSO4 solution.


a) Obtain about 5 mL of the unknown CuSO4 solution in another clean, dry, test tube. Record the number of the
unknown in your data table.
b) Fill the cuvette full with the sample. Wipe the outside and place in the Colorimeter. Close the lid of the
Colorimeter. Important: The reading in the meter is live, so it is not necessary to click Collect to read the
absorbance value.
c) Read the absorbance value displayed in the meter. When the displayed value stabilizes, record it as Tube 6 in your
data table.
d) Calculate the unknown concentration by plugging in the absorbance value into your equation from the standard curve.

6. Before leaving, have your TA initial your report near the time stamp after showing that your cuvette is rinsed, empty, and
back in the colorimeter.

11
CHEMISTRY 1120L Name ____________________________

Partner __________________________
Desk # ___________________________
LAB REPORT: DETERMINING THE CONCENTRATION OF A SOLUTION: BEERS LAW

Show setup on all calculations


Part Two

Absorbance readings of the five CuSO4 standard solutions and the unknown.

Tube Concentration (mol/L) Absorbance

6 Unknown number ____ (y value)

Line equation: y = mx + b

m value __________
b value __________
Correlation value __________ (not part of equation but an indicator of how well the data fit the line; should be >0.9)

Calculation to determine x (concentration):

Unknown concentration: _______________

Experiment adapted from Advanced Chemistry with Vernier by Jack Randall.

12
CHEMISTRY 1120L
ENTHALPY CHANGE FOR A CHEMICAL REACTION
Required reading: pp. 387-392, 402-404; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Objectives
1. To study the changes in heat energy that accompany chemical reactions
2. To calculate enthalpies of reaction experimentally and theoretically

Hazards and Disposal


HCl, NaOH, and bleach (NaClO) are contact hazards. Avoid eye and skin contact. Dispose of all solutions in the sinks by
diluting with large volumes of water.

Part One
Your first task will be to determine the experimental and theoretical enthalpies of reaction for the following equation:

HCl + NaOH NaCl + H2O


Hf (kJ mol-1) -166.4 -469.4 -407.1 -285.9

1. Obtain one Styrofoam cup and a thermometer for your calorimeter

2. Measure out 50.0 mL of 2.00 M HCl (1.03 g mL-1) and place in the calorimeter. Measure out 50.0 mL of 2.00 M NaOH
(1.05 g mL-1) and place in a beaker.

3. Record the initial temperature of the HCl. Quickly pour in the NaOH, stirring with the thermometer. Record the
temperature every 10 seconds until it levels off or begins to decrease. Find the greatest difference in temperature between
the initial and final (highest) temperature (t).

4. Calculate the mass of HCl solution and the mass of NaOH solution used in the reaction from the volumes and the given
densities.

5. Calculate the heat absorbed by the solution the same way it was done in Figure 10.9, p. 396-397. Use 4.184 J / g C for
the specific heat of the solution and the total mass from above.

6. Determine the moles of HCl used in the reaction from the volume and molarity.

7. To find the experimental enthalpy of this reaction you must calculate the heat produced (how will this differ from the heat
absorbed?) per mole of reactant. Since the volume and molarity of both reactants are the same you can use either. Using
the results of your calculations above, find the heat produced by the reaction, the experimental H, per mole of HCl. Be
sure to have the proper sign.

8. Using Example 10.8, p. 403, as an example, calculate the theoretical H for the reaction using the enthalpies of formation
above.

9. Calculate the % error between the experimental and theoretical values of H.

(Difference between the two values/ theoretical) x 100

13
Part Two
You will determine the experimental and theoretical enthalpies of reaction as you did above for the following equation:

NaClO + Na2SO3 NaCl + Na2SO4


Hf (kJ mol-1) -346 -1104 -407 -1388

Specific heat of solution: 4.18 J / g- C Density of bleach: 1.07 g mL-1


Density of Na2SO3 solution: 1.01 g mL-1

1. Rinse and dry your calorimeter and thermometer.

2. Measure 50.0 mL of bleach and 50.0 mL of 0.500 M sodium sulfite as before, mix, and take temperature readings every ten
seconds.

3. Calculate the mass of bleach and the mass of Na2SO3 solution used in the reaction from the volumes and given densities.

4. Using the information above, calculate the heat absorbed by the solution.

5. Bleach is only 8.25% NaClO by weight. Using the grams of bleach found above, determine how many grams of NaClO
were used.

6. This time the moles of each reactant are not equal. Find the number of moles of each reactant and determine which is the
limiting reactant.

7. Using the results of your calculations above, find the heat produced by the reaction, the experimental H, per mole of the
limiting reactant. Be sure to have the proper sign.

8. Calculate the theoretical H using the enthalpies of formation above.

9. Calculate the % error between the experimental and theoretical values of H.

14
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: ENTHALPY

Show setup on all calculations


Part One
1. Initial temperature ____________
2. Temperatures at 10 second intervals
________ ________ ________ ________ ________
________ ________ ________ ________ ________
3. Change in temperature (maximum t) ____________
4. Mass of HCl solution ____________
(calculations)

5. Mass of NaOH solution ____________


(calculations)

6. Total mass ____________


7. Heat absorbed by the solution ____________
(calculations: heat absorbed = mass x spec. ht. x t)

8. Moles of HCl used ____________


(calculations)

9. Heat produced by the reaction per mole of HCl (H) ____________


(calculations)

10. Theoretical H ____________


(calculations)

11. % error ____________


(calculations)

Part Two
12. Initial temperature ____________
13. Temperatures at 10 second intervals
________ ________ ________ ________ ________
________ ________ ________ ________ ________
14. Change in temperature (maximum t) ____________
15. Mass of bleach solution ____________
(calculations)

16. Mass of Na2SO3 solution ____________


(calculations)

17. Total mass ____________


18. Heat absorbed by the solution ____________
(calculations: heat absorbed = mass x spec. ht. x t)

15
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: ENTHALPY (cont.)

19. Mass of NaClO used ____________


(calculations)

20. Moles of NaClO used ____________


(calculations)

21. Moles of Na2SO3 used ____________


(calculations)

22. Limiting reactant ____________


23. Heat produced by the reaction per mole of limiting reactant, H ____________
(calculations)

24. Theoretical H ____________


(calculations)

25. % error ____________


(calculations)

26. What do you think caused the error in the experimental values of H? Use complete sentences and be specific.

16
CHEMISTRY 1120L
COMPLEXOMETRIC TITRATION OF MAGNESIUM
Required reading: pp. 931-935, 945; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Bring a water sample to class (preferably an interesting one, not just tap water)

Objectives
1. To study titrations involving EDTA, ethylenediaminetetraacetic acid
2. To use an EDTA titration to determine the concentration of magnesium in an unknown
3. To measure water hardness using an EDTA titration

Hazards and Disposal


The pH=10 buffer solutions are NH /NH Cl solutions so they are contact hazards. The Eriochrome Black T indicator is
3 4
prepared in triethanolamine which makes it a contact hazard. Should you get either of these solutions on you, wash them off
immediately with soap and water. Dispose of all solutions in the sinks when finished. Dilute with large volumes of water.

Background
Hard water is water that contains a large number of metal ions, principally Mg2+, Ca2+, and Fe3+. All of these ions can be
titrated with EDTA in basic solution. The pH plays a critical role in determining how the EDTA will bind to a given metal.
The reaction between Mg2+ and EDTA4 - is shown by the equation:
Mg2+ + EDTA4 - MgEDTA2

Notice that the Mg and the EDTA react in a 1:1 ratio. Metal ions such as Fe(III) form very stable complexes with EDTA and
will be complexed by EDTA even at acidic pH values. Mg(II) forms less stable complexes with EDTA and will be complexed
by it only at fairly basic pH values. Therefore, it is necessary to buffer all of the solutions used in the experiment to a pH of
10. The pH of a solution is a factor that can be used to selectively titrate metal ions with EDTA. The indicator used for the
titration is Eriochrome Black T which, like EDTA, acts as a coordinating ligand. The structures of Eriochrome Black T and its
magnesium complex are shown below.

OH
OH
HO3S N=N

O 2N
Eriochrome Black T Indicator

-
O Mg

O
-
O3S N=N

O2N
Red Mg-Eriochrome Black T Complex

Since the indicator is a triprotic acid, it exists in varying degrees in the forms of H3In, H2In-, HIn2-, and In3-. The In3- form is a
good coordinating ligand and complexes with magnesium to form MgIn-. The color of the complex MgIn- is wine-red while
the color of the form of the indicator present at a pH of 10 is blue. At a pH of 10 the indicator is in the HIn2- form. Upon
addition of the indicator to a magnesium solution, a red solution forms as a result of the formation of MgIn-. Because the
EDTA forms a more stable complex with the magnesium, it begins to displace the indicator from the magnesium as more and
more EDTA is added during the titration. At the endpoint, the EDTA completely displaces all of the indicator from the
magnesium. The indicator then forms the blue HIn2- which is the endpoint of the titration. This red to blue color change
serves as the endpoint of the titration.
17
Submit a clean 125 mL Erlenmeyer flask with your name and that of your partner to your TA. Proceed with Part One
while the unknowns are being poured into the beakers.

Part One
Your first task will be to determine the relative hardness of your water sample. Note that the titration does not determine the
concentrations of the individual ions, but the total number of ions present. After the water samples have been titrated,
comparisons can be made to see whose water is the hardest or softest.

1. Obtain a buret and 75 mL of standard EDTA solution. Rinse the buret with water followed by two 5-10 mL portions of the
EDTA solution, and then fill it with the EDTA solution.

2. Measure 100 mL of the water sample using a graduated cylinder. Pour the water into a 250 mL Erlenmeyer flask. Add 10
mL of buffer solution (pH=10), 30 mL of distilled water, and 2 drops of Eriochrome Black T indicator. Mix well.

3. Titrate the water sample slowly with the EDTA solution. If your water sample is very soft, it may take less than 1 mL to
reach your endpoint. Be careful not to overshoot your endpoint. The endpoint for the titration is a color change from red to
blue, NOT red to purple. Be certain to record the initial and final volumes of the EDTA solution and the molarity of the
EDTA solution. After calculating the molarity of metal ions in your solution, write it on the board along with where it
came from so it can be compared to the results of other students.

Part Two
1. Obtain the unknown water sample (5.00 mL) prepared for you by your TA. Add 10 mL of buffer solution, 30 mL of
distilled water, and two drops of indicator as before. Mix well.

2. Titrate the solution slowly using the standard EDTA solution. Be certain to record the initial and final volumes of the
EDTA solution and the molarity of the EDTA solution.

3. Repeat using a second sample of your Mg unknown.

18
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: COMPLEXOMETRIC TITRATION

Show setup on all calculations


Part One
1. Molarity of EDTA solution ____________
2. Final volume reading of EDTA buret ____________
Initial volume reading of EDTA buret ____________
Volume of EDTA used ____________
3. Moles of EDTA required ____________
(calculations)

4. Total number of moles of metal ions in sample ____________


5. Molarity of metal ions in sample ____________
(calculations)

Part Two
Unknown Number ____________
1st Sample 2nd Sample
6. Final volume reading of EDTA buret ____________ ____________
Initial volume reading of EDTA buret ____________ ____________
Volume of EDTA used ____________ ____________

7. Moles of EDTA required ____________ ____________


(calculations)

8. Molarity of Mg in unknown ____________ ____________


(calculations)

Average ____________

9. What are some of the experimental errors that a student might make in performing this experiment? Use complete
sentences and be specific.

19
CHEMISTRY 1120L
CHEMICAL EQUILIBRIUM
Required reading: pp. 605-607, 635-640; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Objectives
1. To study chemical equilibrium.
2. To learn how changes in concentration affect chemical equilibrium.
3. To learn how changes in temperature affect chemical equilibrium.

Hazards and Disposal


HCl is a contact hazard. If you get it on your hands, wash it off with lots of soap and water. HCl also has an irritating vapor
so keep HCl solutions under the hood as much as possible. Place stoppers in your test tubes when working with HCl at your
desk.

Background
Consider a chemical system which is at equilibrium: w A + x B y C + z D

A state of chemical equilibrium is said to exist when the rates of the forward and reverse reaction are the same. The
equilibrium expression for the above equilibrium is:

[C] y [D] z
K=
[A] w [B] x

Le Chatelier's Principle states that a system in equilibrium reacts to a stress in such a way as to counteract the stress and
establish a new equilibrium state. In the experiment you will examine two types of stresses that chemists place on systems at
equilibrium: changes in concentration and changes in temperature.

Part One
Your first task will be to determine the effect of changes in concentration on equilibrium. Work in pairs. Do not be afraid of
making an incorrect prediction since you will not be penalized for incorrect predictions. If your prediction does not agree with
your observation, try to understand why it does not. Be certain to stir solutions well when additions are made. Dispose of
your solutions by pouring them into the sink and rinsing them down with lots of water.

Iron(III) Chloride/Ammonium Thiocyanate System


1. Pour 1 mL of iron(III) chloride solution and 1 mL of ammonium thiocyanate solution into a 100 mL beaker containing 40
mL of water. What is observed? An equilibrium has been established between the iron(III) chloride and the ammonium
thiocyanate according to the equation

FeCl3 + 3 NH4SCN 3 NH4Cl + Fe(SCN)3


yellow blood-red

Fill five test tubes about 1/4 full with the red solution. The first tube will serve as a control for the experiment. Use the
deepness of the red color in the first tube as a comparison to see if equilibrium changes occurred. The color of the control
tube should not be so dark so that you cannot see through it. Be certain to mix the solutions well after each addition.

2. Predict what would happen if more FeCl3 were added. Test your prediction by adding 2 mL of FeCl3 solution to the second
test tube. Record your observations. How have the relative amounts of NH4SCN, NH4Cl, and Fe(SCN)3 changed? Use
arrows ( or ) to indicate increase or decrease.

3. Predict what would happen if more NH4SCN is added and test your prediction by adding 2 mL of ammonium thiocyanate
to the third tube. Has the equilibrium shifted to the left or to the right ( or )?

4. Predict what would happen if more NH4Cl was added. Test your prediction by adding 0.20 grams of ammonium chloride
to the fourth tube. Record your observations. How have the relative amounts of FeCl3, NH4SCN, and Fe(SCN)3 changed?
Clean up any ammonium chloride spills on or near the balance!

20
5. Sodium monohydrogen phosphate, Na2HPO4, will react with FeCl3 to form the ion FeHPO4+ and sodium chloride. The ion
FeHPO4+ is colorless. Predict what would happen if Na2HPO4 is added. Test your prediction by adding 0.10 grams of
Na2HPO4 to the fifth tube. Record your observations. Has the equilibrium shifted to the right or to the left?

Cobalt(II) Chloride/Hydrochloric Acid System


6. Pour 5 drops of 0.2 M CoCl2 solution (made in concentrated HCl) into a test tube. The solution has already been prepared
for you. When it is open, keep this solution under a hood or in a test tube with a cork. An equilibrium is established
between the complex ion, Co(H2O)62+, and HCl as illustrated below:

Co(H2O)62+ + 4 Cl- CoCl42- + 6 H2O


pink blue

The solution is presently in concentrated HCl so the blue CoCl42- ion predominates. Predict the results of adding water to
the test tube. Test your prediction by adding 1 mL of water and mixing thoroughly. Record your observations. How have
the relative amounts of Co(H2O)62+, Cl-, and CoCl42- changed?

7. Predict the results of adding more HCl to the system. Test your predictions by adding 2 mL of concentrated HCl to the
tube and mixing thoroughly. Record your observations. Has the equilibrium shifted to the right or to the left?

Part Two
You will determine the effects of temperature changes upon chemical equilibrium.

1. Mix 6 mL of 0.2 M CoCl2 solution (made in concentrated HCl) and 4 mL of water in a 50 mL beaker. The mixture should
be purple in color, intermediate between the blue and pink extremes observed in the previous part of the experiment. If the
color of the solution is not purple, adjust the color by adding more water or CoCl2 solution dropwise. If you notice HCl
fumes, place a watch glass over the beaker.

2. Distribute the volume of the solution evenly among three test tubes. The first tube will serve as a control. Place the second
tube in an ice bath for 10 minutes. Place the third tube in a beaker of water at 60 for five minutes. Record your
observations after this time period. Is this an endothermic or exothermic reaction in the forward direction?

21
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: CHEMICAL EQUILIBRIUM

Part One
Iron(III) Chloride/Ammonium Thiocyanate System
1. Observation of mixing FeCl3 and NH4SCN:

2. Predicted color from adding more FeCl3: ____________________________


Experimental observation: _____________________________________
Change in relative amounts of species ( or ):

NH4SCN: __________ NH4Cl: ___________ Fe(SCN)3: ____________

3. Predicted color from adding more NH4SCN: _________________________


Experimental observation: ____________________________________
Shift in equilibrium ( or ): ________________________________________

4. Predicted color from adding more NH4Cl: ___________________________


Experimental observation: _____________________________________
Change in relative amounts of species ( or ):
FeCl3: __________ NH4SCN: ___________ Fe(SCN)3: ____________

5. Predicted color from adding Na2HPO4: _____________________________


Experimental observation: ____________________________________
Shift in equilibrium ( or ): _________________________________________

Cobalt(II) Chloride/Hydrochloric Acid System


6. Predicted color from adding water: _______________________________
Experimental observation: ____________________________________
Change in relative amounts of species ( or ):
Co(H2O)62+: __________ Cl-: ___________ CoCl42-: ____________

7. Predicted color from adding HCl: _________________________________


Experimental observation: _____________________________________
Shift in equilibrium ( or ): _________________________________________

Part Two
8. Experimental observations:
Color of tube at 60: _________________________
Color of tube at 0: ______________________________
Endothermic or exothermic reaction? _______________________________

22
CHEMISTRY 1120L
IDENTIFICATION OF A WEAK ORGANIC ACID
Required reading: pp. 672, 678-679, 729-730; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Objectives
1. To learn how to use a pH meter.
2. To become familiar with the principles of weak acid-base ionization.
3. To be able to calculate the equivalent weight and Ka of a weak acid from a titration with a strong base and use that to
identify the acid.

Hazards and Disposal


Several of the acid unknowns are corrosive. Do Not Handle Them!!! In case of skin contact wash immediately with
volumes of water. NaOH solutions are corrosive and particularly dangerous to the eyes. Wipe up any NaOH spills
immediately. Dispose of waste solutions down the sinks with large volumes of water.

Background
The purpose of the experiment is to identify a weak acid by finding its equivalent weight and dissociation constant. The
experiment introduces the student to an important laboratory instrument, the pH meter. A series of weak organic acids along
with their ionization constants and molar mass are given in the table below. Your unknown will be one of the organic acids
listed there. Since all of the acids are monoprotic acids, the equivalent weight and molar mass of the acids are the same.
For a weak acid, HA + H2O H3O+ + A-
The equilibrium constant for the equation can then be written as Ka = [H3O+] [A-] / [HA]
As more and more NaOH is added to HA during the titration, the concentration of HA decreases and the concentration of A-
increases. The acid is being neutralized by the addition of the base NaOH to form the strong electrolyte NaA. The reaction
equation is
HA + Na+ + OH- H2O + Na+ + A-
Note that the sodium ion acts as a spectator ion. The half-way point in the titration is the point where exactly of the initial
amount of HA has been neutralized. If one mole of HA is initially present, and mole of NaOH is added, only mole of HA
remains. The concentrations of HA and A- are both equal to mole. By substituting into the Ka expression, we can see that at
the half-way point (equal concentrations of HA and A-), Ka = [H3O+]. Thus, pKa = pH at the halfway point. See the graph for
such a titration on p. 730 in your text.

Acid Ka Molar Mass


Acetic acid 1.8 x 10-5 60.05
Barbituric acid 9.8 x 10-5 128.09
Bromoacetic acid 2.0 x 10-3 138.95
Butyric acid 1.5 x 10-5 88.12
Chloroacetic acid 1.4 x 10-3 94.50
Lactic acid 8.4 x 10-4 90.08
Potassium Hydrogen Phthalate 3.9 x 10-6 204.23
Salicylic acid 1.0 x 10-3 138.12
Sulfanilic acid 5.9 x 10-4 173.19

23
Part One
Your first task will be to determine the amount of NaOH required to neutralize your unknown acid that will be assigned to
you. Work in pairs. All solutions may be disposed of in the sink.

1. Clean a buret by rinsing it with distilled water. Get about 50 mL of NaOH in a beaker. Rinse the buret with two 5 mL
portions of the standardized NaOH solution. Be certain to record the molarity of the NaOH solution and your unknown
number. After rinsing the buret fill the buret with the NaOH solution.

2. Weigh out exactly 0.100 grams of the acid unknown in a plastic weigh boat. Record the weight. Use the same weigh boat
for all weight measurements in the experiment. Be certain to clean the balances and balance area when you are finished.
Transfer the acid sample completely into a 400 mL beaker. Add 100 mL of distilled water and stir to partially dissolve
your unknown. It is not necessary to dissolve all of your unknown before beginning the titration. However, all of your
unknown should have dissolved by the endpoint of the titration. Add one or two drops of phenolphthalein indicator.

3. Be certain to record the initial and final readings of the buret to the nearest 0.01 mL. Titrate the acid sample until a
phenolphthalein endpoint is obtained. Be certain to stir the solution during the titration. Repeat the titration using exactly
the same amount of acid unknown.

4. Using volume and molarity, calculate the moles of NaOH used to completely neutralize the acid (and the moles of acid
titrated).

5. Calculate the molar mass of the acid from the grams and number of moles used.

Part Two

1. Calibrate the pH sensor and leave in the pH 4.00 (or 4.01) buffer
a. Turn on and place electrode in pH 4.00 buffer
b. Select Sensor, calibrate, Ch 1 pH
c. Check box saying 1 pt calibration, then calibrate now
d. Type in 4.00 and keep, then OK
e. Should show 4.00 or very close

2. From the average of your two titrations determine the volume of NaOH needed to neutralize one-half of the acid (volume of
NaOH at the half-way point). Add this volume of NaOH solution to a third sample of acid weighing exactly the same as
the first two. Add 100 mL of water and stir as before. You are now ready to measure the pH of the half-neutralized
solution.

3. Now that you know the pH of the half-neutralized solution, you know the pka of the acid. Since the pKa = -log (Ka), then
the Ka = 10-pKa.

4. Using the molar mass and Ka, determine which acid in the list is your unknown. If both calculations do not match one acid,
which calculation do you believe to be the most likely to be correct?

24
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: IDENTIFICATION OF A WEAK ACID

Show setup on all calculations


Part One
1. Unknown number _______________

Molarity of NaOH solution _______________

1st Determination 2nd Determination


2. Weight of unknown acid _______________ _______________

3. Final volume NaOH solution _______________ _______________

Initial volume NaOH solution _______________ _______________

Total volume used _______________ _______________

Average volume of NaOH solution _______________

4. Moles of NaOH used _____________


(calculations)

5. Moles of acid _____________


6. Molar mass of acid _____________
(calculations)

Show setup on all calculations


Part Two
7. Volume of NaOH needed to neutralize of acid _____________
8. pH of half-neutralized acid solution _____________
9. pKa of acid _____________
10. Ka of acid _____________
(calculations)

11. Identity of unknown _____________

12. Which method, Part One titration/molar mass, or Part Two pH meter/Ka, gives more
reliable results and why?

25
CHEMISTRY 1120L
QUALITATIVE ANALYSIS
Required reading: pp. 324-325, 749-756, 931-932; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Objectives
1. To practice careful laboratory manipulation, critical observation, and logical interpretation of results.
2. To learn some descriptive inorganic chemistry.
3. To illustrate certain principles covered in lecture including ionic equilibria, solubility, and coordination chemistry.

Hazards and Disposal


Concentrated solutions of acids and bases are extremely corrosive. Always keep HCl and ammonia solutions under the hood
as much as possible since these solutions have irritating vapors. The mercury(I) test solution has been prepared in dilute acid
so exercise caution when using this test solution. Ethanol is used in the preparation of DMG solutions and is extremely
flammable. When using the centrifuge make certain that it is balanced. All solutions which contain metal ions should be
poured into the specially labeled waste containers. Assume all ion solutions are contact hazards.

Background
The "classical" course in qualitative analysis consisted of analyzing for 25 metal ions and 12 anions. Nowadays modern
analytical procedures and instrumentation such as polarography, specific ion electrodes, and atomic absorption have replaced
the older classical methods in the laboratories of the research chemist. The modern methods are not only faster and more
reliable, but they also are capable of giving a more quantitative analysis for each particular ion. Although qualitative analysis
of inorganic materials is rarely performed by research chemists, a reduced qualitative analysis scheme is useful in illustrating
some important principles. The qualitative analysis scheme that you are going to perform has been reduced to only 6 cations,
which are separated into three groups: Group I Insoluble Chlorides (Ag+, Hg22+); Group II Insoluble Hydroxides (Fe3+,
Mn2+); and Group III Complexed Ammines (Cu2+, Ni2+).

While it is fairly easy to devise tests for specific ions, devising tests for specific ions present in mixtures of other ions is much
more difficult. Classification of metal ions into groups enhances their separation and characterization. The classification of
ions is based upon similar chemical properties, such as solubility and the ability to form complex ions.

Group I -- The Insoluble Chlorides


Most metal chlorides are soluble, but silver(I) and mercury(I), as well as lead(II), form chlorides that are not. Note that
mercury(I) exists as a dimer, Hg22+. This cation contains two mercury(I) ions connected by a mercury-mercury bond. All of
the Group I cations form insoluble chlorides in the presence of dilute HCl. This distinguishing property separates the Group I
cations from all the other possible ions.

Silver(I) and mercury(I) chlorides can be separated on the basis of complex ion formation. In the presence of excess
ammonia, silver ions form a soluble complex ion, [Ag(NH3)2]+, while mercury(I) cannot complex the ammonia and remains
insoluble as HgNH2Cl.

Group II -- The Insoluble Hydroxides


Most metal hydroxides, with the exception of the alkali metals, ammonium, and some of the alkaline earth metals, are
insoluble, and they demonstrate a wide range of insolubility, as seen through their solubility product constants, Ksp.

The separation of Group II metal hydroxides, which precipitate from solution upon the addition of ammonia, from Group III
complexed ammines, which do not precipitate from weaker basic solutions such as ammonia, is accomplished by adjusting the
acidity of the solutions (and, thus, the hydroxide ion concentration) so that only the less soluble Group II metal hydroxides
precipitate. Even though Cu2+ and Ni2+ have smaller solubility product constants than does Mn2+ and Fe3+, they do not
precipitate as hydroxides because of the ease with which they form complex ammines with ammonia. Since Mn2+ and Fe3+ do
not form a complex ammine upon the addition of ammonia, they are able to form an insoluble hydroxide instead.

Iron(III) is detected by the addition of thiocyanate ion to form a blood-red complex ion (as was seen in Lab 5). Detection of
manganese is accomplished when the hydroxide is dissolved in HNO3 and oxidized to the purple MnO4- by sodium bismuthate
(NaBiO3).

Group III -- The Complexed Ammines


26
The Group III ions have remained in solution during the entire scheme due to their formation of complex ammines upon the
addition of ammonia. Cu(II) and Ni(II) ions both form complex ammines, which are soluble, when NH3 is added. Formation
of the deep blue complex ammine upon addition of NH3 confirms Cu(II). In basic solution nickel(II) complexes with
dimethylglyoxime, DMG, to form a pink precipitate.

Laboratory Procedure
You must work individually on your unknown. All glassware used in the experiment must be thoroughly rinsed with deionized
water to avoid contamination. Be sure to mix all solutions thoroughly when you add reagents to your test tubes. There are
several check points in the known solutions where the lab assistant must examine your solutions and initial your report sheet.
Use the flowchart to assist in the identification of the unknown.

(Qualitative Analysis, part A; in pairs) - Preliminary Experiments on Known Solutions

Insoluble Chlorides (numbers in parentheses refer to the line on the answer sheet)
1. Put 5 drops of 0.1 M Ag+ solution and 5 drops of 0.1 M Hg22+ solution into one test tube. Add 5 drops of water and 1 drop
of 3 M HCl solution. What happens when HCl is added to the test tube (1)? Write net ionic equations for the two chemical
reactions (2).

2. To the same tube from step 1, add 1 mL (about 20 drops) of 6 M NH3. Mix the solution very well by using a finger
vortex or a stirring rod. Record your observation (3). Centrifuge the tube (be sure to place a balancing tube with water at the
same level opposite it in the centrifuge). A gray/black solid is indicative of mercury (see flow chart). Pour the centrifugate
(liquid) into another tube. To that tube, carefully add, drop by drop, 6 M HNO3. Be certain to mix thoroughly. Continue the
addition until the solution is acidic to litmus or pH paper. A white solid is indicative of silver (see flow chart). Record your
observations (4).

Insoluble Hydroxides
1. Put 10 drops each of 0.1 M test solutions of Fe3+ and Mn2+, along with 1 mL of H2O, into one test tube. Add 2 drops of 6
M HNO3 then 1 mL of 6 M NH3 to the tube. The solution should be slightly basic. Note the color and texture of the
precipitate that forms (5). Centrifuge and discard the centrifugate.

2. To the solid, add 10 drops of 1 M NaOH, mix, and centrifuge. Discard the centrifugate (also called supernatant the liquid
above the solid). Next add 2 mL of H2O, then 6M HNO3 until acidic. Pour half of the sample into another test tube.

3. Into one of the tubes, add 5 drops of potassium thiocyanate solution (KSCN). Record your observations (6). Show the
tube to the lab assistant for approval (7). This blood-red solution is the test for iron (see flow chart).

4. Into the other tube, add 2 more drops of 6 M HNO3. Add a micro-spatula full of NaBiO3, stir, and centrifuge. Record
your observations (8). This purple supernatant confirms the presence of Mn(II).

Complexed Ammines
1. Put 10 drops of 0.1 M Cu2+ into a test tube and 10 drop of 0.1 M Ni2+ test solution into a different test tube. Add 1 mL of
H2O to each test tube. Add 6 M NH3 to each until basic. Record your observations (9). A deep blue liquid indicates Cu2+.
Add 10 drops of dimethylglyoxime solution (DMG) to the Ni2+ tube. Record your observations (10). Show your tubes to the
lab assistant for approval (11).

27
(Qualitative Analysis, part B; individually) - Analysis of the Unknown Solution

Obtain an unknown solution and record its appearance and NUMBER on your report sheet. Mix the solution well and pour
about 2 ml into a test tube for analysis. Construct a flowchart as you proceed with the analysis.

Group I -- The Acid Chloride Group


Add 3 M HCl drop by drop to the unknown solution until it just registers acidity to litmus. Add five drops excess. If your
unknown solution is already acidic, just add five drops of 3 M HCl. If a precipitate is observed, label the test tube (A), and
then place it in a centrifuge along with a similar test tube containing water to serve as a counterbalance. Centrifuge for about
30 seconds, then decant the clear centrifugate into a test tube labeled (B). Wash solid (A) with 1 ml of water plus five drops of
3 M HCl, centrifuge, and then discard the centrifugate. If (A) is not white or appears gelatinous rather than crystalline, Group
II or Group III cations may be present. The washing step should be repeated to remove these contaminants.

Add 10 drops of 6 M NH3 to (A), stir, and centrifuge. If a dark gray or black precipitate remains, mercury(I) is present. If
silver is confirmed later, a small amount of black residue at this point might be due to metallic silver, formed by the
photochemical decomposition of AgCl. Transfer the centrifugate to a test tube labeled (A1), then cautiously add 6 M HNO3,
drop by drop with stirring, until the solution is acidic. Formation of a white precipitate confirms the presence of silver(I).

Group II -- The Hydroxide Group


Add 3 drops of 6 M HNO3 then 20 drops of 6 M NH3 to the solution in test tube (B) and stir. Centrifuge and decant the
centrifugate into a test tube labeled (C). Add 10 drops of 1 M NaOH to solid (B) and stir. Centrifuge and discard the
centrifugate.

To the solid in tube (B) add 2 mL of H2O then add 6 M HNO3 dropwise until acidic. Transfer half of the solution to a test tube
labeled (B1). To the solution in (B) add 5 drops of KSCN. Formation of a blood-red solution confirms the presence of
Fe(III). To the solution in (B1) add 2 drops more 6 M HNO3, 1 micro-spatula full of NaBiO3, and centrifuge. The formation
of a purple supernatant confirms the presence of Mn(II).

Group III -- The Complexed Ammine Group


To the solution in tube (C) add 6 M NH3 until it is basic, then add 5 drops excess. If the solution in (C) is deep blue,
copper(II) is present. Remember from Part A that nickel will form a very pale blue. The next step will confirm if there is
nickel present.

Add five drops of dimethylglyoxime (DMG) solution to (C), centrifuge and decant. Appearance of a pink precipitate confirms
the presence of nickel(II).

28
Unknown
Qualitative Analysis Flowchart

Add 3M HCl

(A) Precipitate (B) Clear Solution


Group I Groups II and III

Add 6M NH3 Add 6M HNO3


and 6M NH3

(A) Gray (A1) Clear


Precipitate Solution
Hg22+
{HgNH2Cl} (C) Clear Solution
Add 6M HNO3 (B) Precipitate Group III
Group II

Add 6M NH3
White Precipitate
Ag+ {AgCl} Add 1M NaOH

Blue Solution
Cu2+ {Cu(NH3)42+} Add DMG
(B) Dark Precipitate Solution
Discard

Pink Precipitate
Ni2+ {Ni(DMG)2}
(B) Add H2O and 6M HNO3

(B) Add KSCN (B1) Add 6M HNO3


and NaBiO3

Red Solution
Fe3+ {Fe(CNS)63-} Purple Solution
Mn2+ {MnO4-}

29
CHEMISTRY 1120L Name ____________________________

Partner __________________________
Desk # ___________________________
LAB REPORT: QUALITATIVE ANALYSIS (part A)

Insoluble Chlorides
1. What happens when HCl is added to the tube?

2. Write the net ionic equations for the two reactions (part of the silver equation is done for you).
Ag+ + Cl-

Hg22+ +

3. What is observed when ammonia is added to the test tube?

4. What is observed when the silver solution is acidified?

Insoluble Hydroxides
5. What is the color and texture of the precipitates?

6. What is observed when thiocyanate is added to the iron?

7. Assistant's approval _________________

8. What is observed when NaBiO3 is added to the Mn(II) solution?

Complexed Ammines
9. What is observed when excess NH3 is added to the Cu(II) and Ni(II) solutions?

10. What is observed when the DMG solution is added to the Ni(II) solution?

11. Assistant's approval _________________

30
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: QUALITATIVE ANALYSIS (part B)

UNKNOWN NUMBER _________________________

Appearance of Unknown: ___________________________________________________________________________

Cations Present: __________________________________________________________________________________

Unknown # _______

Add 3 M HCl

(A) Ppt (Group I)


(B) Clear Solution (Groups II, III)

31
CHEMISTRY 1120L
OXIDATION STATES OF URANIUM
Required reading: pp. 334-335, 338-339, 769-772; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Objectives
1. To learn about the principles of oxidation and reduction.
2. To observe some of the chemistry of the element uranium.
3. To use an oxidation-reduction titration to identify an unknown oxidation state of an element and write the balanced
chemical equation for the oxidation-reduction reaction.

Hazards and Disposal


All of the solutions used in the experiment are acidified with dilute sulfuric acid. Exercise caution when working with
them. Sulfuric acid is a contact hazard. When diluting acid solutions, ALWAYS ADD ACID TO WATER. The
permanganate solution is a powerful oxidizing agent. All uranium salts are toxic. When using the pipet, do not pipet by
mouth!! Return waste zinc amalgam to the specially labeled waste container. Do not throw the amalgam into the sinks or
waster containers. All solutions used in the experiment may be flushed down the sinks with large volumes of water.

Background
The known oxidation states of the element uranium are +6, +5, +4, and +3. In the +6 and +5 states, the uranium exists as the
oxo-ions, UO22+ and UO2+. In this experiment the uranyl ion, UO22+, is used as the salt, uranyl acetate dihydrate,
UO2(C2H3O2)2 . 2 H2O. Note that in the uranyl ion the uranium is in the +6 oxidation state, the most common and most stable
oxidation state for uranium. Metals in high oxidation states must be stabilized by electronegative atoms such as oxygen or
fluorine. This is why metals in oxidation states larger than +4 will usually be found in oxo- or fluoro-ions.

In the experiment you will use a zinc-mercury amalgam (Zn in diagram above) to reduce the uranium from the +6 oxidation
state (in UO22+) to a lower one. A zinc-mercury amalgam consists of zinc metal with a mercury coating. The mercury coating
is necessary to prevent the reaction of zinc with hydrogen ions which are present in the acidic solutions used in the
experiment. The lower oxidation state of uranium obtained in this step is not stable with respect to air oxidation. The zinc-
reduced uranium solution is stirred to complete the oxidation to a more stable intermediate oxidation state. Then, this
intermediate oxidation state of uranium is oxidized back to the +6 oxidation state by titrating with potassium permanganate,
KMnO4.

Part One
Your first task will be to reduce the uranium from the 6+ state to the unknown m+ state using zinc. This will then be oxidized
to the n+ state with oxygen from the air. All solutions may be poured into the sink. The used zinc must be placed in the waste
bottle! No zinc in the sink! Work in pairs.

1. Prepare 200 mL of a 1 M H2SO4 solution by diluting the correct amount of 5 M H2SO4 to 200 mL with water. Be sure to
add acid to water. This is the solution you will use for the washes below!

2. Place one scoop of the zinc-mercury amalgam (about the size of a nickel) in your Florence flask. Add 25 mL of 1 M
H2SO4. Swirl the flask for a few minutes and then decant the acid solution into a beaker for disposal. Repeat the washing
process with another 25 mL portion of the acid and decant.

3. Draw out a sample of 0.100 M uranyl acetate dihydrate, UO2(C2H3O2)2 . 2 H2O, using a 10.00 mL pipet. DO NOT PIPET
BY MOUTH!! Be sure you have watched the video on using volumetric glassware.

4. Add the uranium solution to the zinc and swirl for five minutes. Note the color of the uranyl acetate solution before and
after it is added to the zinc. Decant the uranium solution into a 250 mL Erlenmeyer flask. Wash the zinc four times with
32
25 mL portions of 1 M H2SO4, decanting each washing into the flask that contains the uranium solution. The washings
should remove all traces of the uranium solution from the zinc. The idea is to get every last mole of uranium into the 250
mL flask but do not allow the zinc to pass into the flask with the uranium.

5. Stir the uranium solution for five minutes with a stirring rod. The stirring rod allows oxygen to oxidize the lower oxidation
state of uranium to a more stable intermediate oxidation state. Note the color of the intermediate oxidation state of the
uranium.

Part Two
Your second task will be to determine the amount of potassium permanganate solution needed to oxidize the intermediate
compound to the 6+ state (UO22+). From this data you will be able to determine the n+ state and then predict the m+ state.

1. Titrate the intermediate uranium solution with a standardized KMnO4 solution. Rinse and fill your buret with the KMnO4
solution. Be certain to record the initial and final volumes of the KMnO4 solution during the titration. The endpoint of the
titration is when a faint pink color (not peach) is obtained, and the color lasts for thirty seconds or more. Be sure to note
the colors of the different oxidation states of the manganese. Record the molarities of the permanganate and the uranium
solutions. When you have completed the titration, empty the solutions into the sink and wash your buret thoroughly to
remove any permanganate.

In any red-ox titration, at the equivalence point, the number of equivalents of oxidant (oxidizing agent) is equal to the number
of equivalents of reductant (reducing agent). This relationship is illustrated in the equation below.

# of equivalents REDUCTANT = # of equivalents OXIDANT

Since the manganese gained five electrons in the titration:


MnO4- + 5 e- Mn2+
So # of equivalents Mn = # of moles Mn x 5

The uranium lost electrons in the titration. We know it began as n+ and ended as 6+:
Un+ UO22+ + (6-n) e-
So # of equivalents U = # of moles U x (6-n)

Thus at the equivalence point, # of moles Mn x 5 = # of moles U x (6-n).


2. Solve the equation for n and make an educated guess about m.

3. Write the half reactions and balanced overall equation for the permanganate/uranium reaction (above equations).

4. Write the half reactions and balanced overall equation for the uranium ion with the lower oxidation state (Um+) and O2. The
uranium is oxidized to n+ and the oxygen is reduced to water.

33
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: OXIDATION STATES OF URANIUM

Part One
1. To prepare 200 mL of 1 M H2SO4 you will dilute ______________ mL of 5 M H2SO4 to 200 mL with ________ mL of
water.
2. Volume of uranyl acetate dihydrate used _____________
3. Color of uranyl acetate solution (+6 oxidation state) _____________
+
4. Color of reduced uranium solution (lower oxidation state, m ) _____________
+
5. Color of air-oxidized uranium solution (intermediate state, n ) _____________

Show setup on all calculations


Part Two
6. Final volume reading, KMnO4 _____________
Initial volume reading, KMnO4 _____________
Total volume used, KMnO4 _____________
7. Color of manganese solution; +7 oxidation state _____________
Color of manganese solution; +2 oxidation state _____________
8. Molarity of KMnO4 solution _____________
Moles of KMnO4 used _____________
(calculations)

9. Molarity of uranyl acetate solution _____________


Moles of uranium used _____________
(calculations)

10. Identity of intermediate oxidation state _____________


(calculations)

11. Probable identity of lower oxidation state _____________


12. Balanced chemical equation (including half reactions) for permanganate titration:

13. Balanced chemical equation (including half reactions) for air oxidation:

34
CHEMISTRY 1120L
RATES OF REACTION
Required reading: pp. 815-820, 827-831, 855-858; Chemistry: Atoms First, Burdge & Overby, 2nd edition

Objectives
1. To study the effects that changes in concentration, catalysts, and temperature have on the rate of chemical reactions.
2. To learn how to determine the order of a chemical reaction.
3. To be able to construct a potential energy vs. reaction coordinate diagram for a reaction.

Hazards and Disposal


The dilute hydrogen peroxide solutions used in the experiment are mild contact hazards due to the oxidizing ability of
hydrogen peroxide. The other compounds used in the experiment are not particularly hazardous provided normal precautions
are taken. You may dispose of all waste solutions in the sinks. Use deionized water from the containers at the front of the
lab for all the experiments.

Background
The study of the rate of chemical reactions is called kinetics. Your text explains the factors that govern the rate of a chemical
reaction and how to determine the rate law.
Rate = k [A]n
The value for the rate constant, k, and the order of the reaction with respect to A, n, must be determined experimentally. The
order of the reaction is usually a small integer (0, 1, or 2). In the experiment you will determine the order of a reaction with
respect to one of the reactants. The reaction is the classic iodine clock reaction and proceeds by a series of steps.
IO%$ + 3 HSO$ I
%
Step 1: %
+ 3 SO)% ( + 3 H+ (slow)
Step 2: 5 I% + 6 H+ + IO%
$ 3 H2O + 3 I2 (fast)
Step 3: I2 + HSO%
$ + H2O 2 I% + SO)%
( + 3 H+ (faster)

When all of the bisulfite has been depleted, I2 reacts with the starch to produce a dark blue complex. You will determine the
rate of reaction by monitoring the time that it takes for the dark blue color of the starch-iodine complex to appear. Monitoring
changes in chemical or physical properties (such as color) with time provides experimental means for determining rates of
reactions.

Temperature and the presence of a catalyst are two factors that control the rate of reaction. A (positive) catalyst impacts a
reaction by providing an alternate pathway or mechanism by which the reaction can proceed. The influence of temperature
and catalysts will be studied using the cobalt(II) catalyzed oxidation of tartaric acid with hydrogen peroxide. Tartaric acid,
H2C4H4O6, is formed in aqueous solutions from the dissolution of sodium potassium tartrate. The chemical reaction is:
H2C4H4O6 (aq) + 5 H2O2 (aq) CoCl
2 8 H2O (l) + 4 CO2 (g)

The rate of reaction is measured by the time that it takes for the pink color of the cobalt(II) to reappear. The appearance of the
green intermediate complex is due to the formation of the green cobalt(III)-tartrate complex.

Part One
Your first task will be to determine the order of the clock reaction with respect to [IO%
$ ]. Work in pairs. Use a watch or wall
clock to record times. Rinse glassware thoroughly between runs to avoid contamination. Make accurate volume
measurements when using the graduated cylinders.

1. Using the specially labeled 50 mL graduated cylinder, carefully measure 20 mL of sodium bisulfite-starch solution and pour
the solution into a 50 mL beaker. Similarly, measure 20 mL of potassium iodate solution using the specially labeled 50 mL
graduated cylinder and pour into a second beaker. Measure all of your volumes accurately! Record the volumes of both
solutions. Record the temperature of the solutions. Add the potassium iodate solution to the bisulfite-starch solution and
stir thoroughly. Read the time when the solutions are mixed and carefully measure the time between the initial mixing and
the appearance of the dark blue starch-iodine complex. Record the time of reaction.

35
2. Thoroughly rinse and clean your glassware. Slight amounts of solution remaining can interfere with subsequent
determinations. Repeat the experiment using 20 mL of sodium bisulfite-starch solution and only 10 mL of the iodate
solution. Add 10 mL of deionized water to bring the total volume to 20 mL. Note that you have used only half as much
iodate as you did before. Before mixing make certain that the temperatures of the two beakers were the same as they were
previously. Record the temperature and volumes for this run. Again, measure the time that it takes for the dark blue color
to appear.

3. Repeat the experiment for a third time using 5 mL of iodate solution and 15 mL of water and the 20 mL of sodium bisulfate-
starch solution. Make certain that the temperatures of your solutions are the same as they were before. Record your
temperature, volumes used, and time of reaction. Calculate an approximation of rate by taking 1/time to get sec-1.

4. What is the order of the reaction with respect to IO%


$?

Part Two
You will determine the effects of temperature and a catalyst upon the rates of the tartaric acid reaction above.

1. Using a 100 mL or 150 mL beaker, mix 30 mL of sodium potassium tartrate solution and 10 mL of 6 % hydrogen peroxide
solution. Heat the solution to 55 using a hotplate. Remove the beaker from the heat and place it on a mat. What changes,
if any, do you observe?

2. Quickly add 3 mL of cobalt chloride solution. Record the temperature of the solution at the time of the addition.
Immediately begin timing the reaction. Record the temperature of the solution and the number of seconds until the pink
color of the cobalt(II) returns. Cite three observations (things you can see) that indicate that a chemical reaction has
indeed taken place. Why did the reaction not take place until the cobalt was added?

3. Dispose of your solutions in the sink. Thoroughly clean the beaker and mix a second 30 mL portion of sodium potassium
tartrate solution and a second 10 mL portion of 6 % hydrogen peroxide in the beaker.

4. Heat the solution to 65 C. Add 3 mL of cobalt chloride solution and record the temperature of the solution before and
after, and the amount of time that it takes for the pink color to return. From comparisons of the reaction time at 65 C and
55 C, how do temperature increases affect rates of reaction?

5. Construct two potential energy vs. reaction coordinate diagrams, one for a theoretical uncatalyzed reaction and one for the
cobalt(II) catalyzed reaction. Be sure to label the following on your diagrams. Some things should be different and some
should stay the same. Be sure to make it clear what changes and what does not in your drawing. See page 855 in your text.

R -- the location of the energy for the reactants


P -- the location of the energy for the products
I -- the location of the green intermediate complex
Ea -- the activation energy (relative value)
H -- the change in enthalpy (relative value)

36
CHEMISTRY 1120L Name ____________________________
Partner __________________________
Desk # ___________________________
LAB REPORT: RATES OF REACTION

Part One
NaHSO3(mL) KIO3(mL) H2O(mL) Time(sec) Rate(sec-1) Temp(C)
1. __________ __________ __________ __________ __________ __________
2. __________ __________ __________ __________ __________ __________
3. __________ __________ __________ __________ __________ __________
4. Order of reaction with respect to iodate: _______________
Part Two
5. Observations after heating mixture:

6. Addition of Co catalyst: Temp: 55C

7. Pink color returns: Temp: _____________ Time: __________

8. Observations after addition of catalyst:


a. b. c.

9. Addition of Co catalyst: Temp: 65C

10. Pink color returns: Temp: _____________ Time: __________

11. Why does the reaction not take place until the cobalt is added? Use complete sentences.

12. How do temperature changes affect rates of reaction? Use complete sentences.

13. Potential energy vs. reaction coordinate diagrams:

Uncatalyzed reaction Catalyzed reaction

37