Apparatus
Check each piece of apparatus, which you find in your locker from the duplicate list
furnished to you by your instructor. Sign your name and submit to your instructor.
The instructor signs the checklists and gives one copy to you for your safekeeping.
Provide your locker with reliable padlock. You are responsible for all the
apparatus issued to you. Towards the end of the semester you have to
replace or give a deposit for any piece which you have lost or broken. If you
have partners, each of you will share equally any loss or breakage of
apparatus kept in your lockers and those borrowed from the stockroom.
General apparatus, e.g., Bunsen burner, thermometer, iron stand, clamps,
etc. and special apparatus may be borrowed from the laboratory attendant.
Borrowing of apparatus from the stockroom should be done during the first
30 minutes of the laboratory period.
You have to provide yourself with the following materials and supplies
besides the apparatus in the laboratory locker and the stockroom:
Group Individual
Padlock with keys Tissue paper Pot holder Lab notebook
Masking/paper Rags Medicine dropper (3-5 pcs) Lab manual
tape
Aspirator Marking pens Rubber tubing (2 ft) Lab gown
Wire gauze Filter paper Marking pen Hand towel
Wash bottle Tray Pair of scissors Mask
Liquid detergent Match Goggles
Stirring rod Test tube holder
Assessment:
Evaluation of the students’ progress will be based on performance laboratory experiments;
written reports of laboratory work and exams. The distribution is as follows:
Safety Reminders
1. All students are required to wear a lab gown during each experiment. This will
be strictly enforced to avoid accidents caused by chemical spills and the like.
2. Safety glasses, goggles or eye shields must be worn during the experiment.
Contact lenses should not be worn.
3. Shorts, skirts, sandals, slippers are not allowed in the laboratory. Secure long hair.
4. Never taste, smell, or touch a chemical solution unless specifically directed
to do so. Individual allergic or sensitivity responses to chemicals cannot be
anticipated. If any chemical comes in contact with any other parts of your
body or clothes, wash thoroughly with plenty of water.
5. Procedures involving the liberation of volatile or toxic flammable materials
shall be performed in a fume hood (e.g., H2S, HCN).
6. Never heat a flask or apparatus that is not opened to the atmosphere.
7. Always pour waste acid, used KMnO4, organic solvents and solutions of
heavy metals into their respective disposal jars, never into the sink.
8. Replace the cover of every container immediately after removal of reagent.
Deposit insoluble refuse such as pieces of paper, wood, glass cork in the
waste basket, never into the sink or on the floor
9. All accidents, injuries, breakages and spillages, no matter how minor, must
be reported immediately to the instructor.
10.Eating, drinking, smoking and playing inside the laboratory are strictly
prohibited. Your hands may be contaminated with “unsafe” chemicals.
11. Unauthorized experiments, including variations of those in the laboratory
manual, are strictly prohibited. If your chemical intuition suggests further
experimentation, consult with your instructor first.
12.Unauthorized person(s) shall not be allowed in the laboratory.
13.Maintain a wholesome, businesslike attitude. Horseplay and other careless
acts are prohibited.
14.The tabletop must be cleared of unnecessary materials. Put all bags and
books in designated areas.
15.Solids, water and other liquids spilled on your tabletop must be cleaned up
as soon as possible
16.No electronic equipment (laptops, ipod, mp3s, cellphone, etc.) will be
switched on while working in the lab.
17. It is imperative that you keep the balance and the immediate area around the balance clean!
Clean-up all chemical spills and excess chemical after each use of the balance. Do not leave
old crumpled papers on the balance table. When the balances are not in use, the balance
should be always turned-off and in the case of the substitution balances the beam arrested,
all weights on zero and the doors closed.
Chemical/Reagents:
0.3 M NaCl
0.1 M Fe(NO3)3.6H2O
1.0 M HCl
Cation exchange resin (Dowex 50)
Phenolphthalein solution
Standard 0.1 N NaOH
Procedure:
Analysis:
(1) +
Generate the H saturated resin by passing about 100 mL of 1 M HCl
through the column at rate of 15 mL per minute. Apply the liquid solution to the
glass wall so as not to disturb the resin. Wash the column free of acid with about
150 mL of water. Use the first few millimeters to wash the glass walls and allow the
water to soak into the resin before continuing the washing.
Pour in 10.0 mL of 0.3 M NaCl and after the solution has soaked in, wash it through with 100 mL
of water at a rate of 3 mL per minute, collecting all eluate. Add 3 drops of phenolphthalein indicator to
the eluate and titrate with standard 0.1 N NaOH. Calculate the theoretical volume of NaOH needed for
the tiration and compare this with your own result. Calculate also milliequivalents of exchangeable
anion per gram of dry resin. Write the exchange equilibrium established between the solid phase and
the solution.
(2) Repeat the second paragraph of (1) using 10.0 mL of 0.1 M Fe(NO 3)3
instead of 0.3 M NaCl.
(3) Pass 10.0 mL of 0.10 M NaOH through the column as in (1) and
analyze the eluate. Explain what you observe.
1.b Ion Exchange Separation and Titrimetric Determination of Nickel (II) and Zinc (II)
Chemicals/Reagents:
2 M HCl
Strong-base anion exchange resin such as amberlite CG 400 or its equivalent
6 M NH3
Conc. HCl
Standard 0.01 M EDTA solution
Procedure:
1. Preparation of Ion-Exchange Column.
Insert a wad of glass wool or absorbent cotton at the bottom of a 25-ml burette to retain
the resin particles. Then introduce sufficient strong-base anion-exchange resin to give
a 10 to 15 cm column. Wash the column with about 6 M of NH3, followed by 100 ml of
water and 100 ml of 2 M HCl. At the end of this cycle, the flow should be stopped so
that the liquid level remains about 1 cm above the resin column. At no time should the
liquid level be allowed to drop below the top of the resin.
2. Separation of Nickel (II) and Zinc (II)
2+ 2+
Obtain the unknown, which should contain between 2 and 4 mmol of Ni and Zn , in
a clean 100-ml volumetric flask. Add 16 ml of 12 M HCl, dilute to the mark with distilled
water, and mix well. The resulting solution is approximately 2 M in acid. Transfer 10.00
ml of the diluted unknown onto the column. Place 250-mL conical flask beneath the
column, and slowly drain until the liquid level is nearly above the resin. Rinse the
interior of the column with several 2 to 3-mL portions of the 2 M HCl; lower the liquid
level to just above the resin surface after each washing. Elute the nickel with about 50-
mL of 2 M HCl at a flow rate of 2 to 3 mL per minute. After elution is complete
evaporate the collected liquid just to dryness on a hotplate or steam bath.
Elute the Zn (II) by passing about 100 mL of water through the column, using the
same flow rate; collect the liquid in a 500-mL conical flask.
3. The Titration of Nickel and Zinc with EDTA
(a) Titration of nickel. Evaporate the solution containing the nickel to dryness to
eliminate excess HCl. Avoid overheating; the residual NiCl2 must not be permitted to
decompose to NiO. Dissolve the residue in 100 mL of distilled water, and add 10 to 20 mL
of pH-10 buffer. Add 15 drops of bromopyrogallol indicator or 0.2 g of murexide. Titrate to
the color change (blue to purple for bromopyrogallol, yellow to purple for murexide).
Calculate the weight in milligrams of nickel in the unknown.
(b) Titration of zinc. Add 10 to 20 mL of pH-10 buffer and 1 to 2 drops of
Eriochrome Black T to the eluate. Titrate with standard EDTA solution to a color
change from red to blue.
Calculate the weight in milligrams of zinc in the unknown.
2+
2. SPECTROPHOTOMETRIC DETERMINATION OF Fe IONS USING 1, 10-
PHENANTHROLINE (External calibration method)
Objectives:
Materials:
Apparatus Chemicals
Spectrophotometer/ Filter photometer Ferrous ammonium sulphate hexahdrate
Matched cuvette 1, 10-Phenanthroline
Volumetric flasks (1 L) Hydroxylamine hydrochloride
Volumetric flasks (50 mL) Hydrochloric acid
Graduated pipette, 10 mL Sulfuric acid
Pipettes (5, 10 mL) Acetic acid
Sodium acetate
Preparation of solutions:
Procedure:
Sample preparation
1. Pipette out 1, 2, 3, 5, 10, 15 and 20 mL of the standard ferrous ion solution into a series of
100mL standard flasks labeled from 1 to 7.
2. In another flask, labeled ‘Sample’, take 10 mL of the unknown sample. (Make
2+
sure the approximate Fe concentration is within the calibration curve)
3. To another 100 mL standard flask, labeled ‘Blank’, add about 20 mL of distilled
water to prepare the blank solution.
4. To each of the above flasks (standards, sample and blank) add 1 mL of
hydroxylamine hydrochloride and 5 mL of 1, 10-phenanthroline.
5. Buffer each solution by adding 8 mL of acetic acid / sodium acetate buffer.
6. Allow at least 15 minutes after the addition of the reagents for full color
development (The color once developed is stable for hours).
7. Dilute each solution exactly to 100 mL mark with distilled water and mix well.
8. The standard solutions so obtained correspond to 0.1, 0.2, 0.3, 0.5, 1.0, 1.5
and 2.0 ppm respectively.
9. Record the absorption spectrum for the 2.0 ppm standard solution against the
reagent blank in the range of 400 – 700 nm.
10. Select the wavelength which gives maximum absorbance ( maxλ ).
11. Calculate the molar absorption coefficient ( ε ) of the complex from the
molar concentration and path length of the cuvette. Use the relation A = εbc.
12. Measure the absorbance for all the standard solutions at the wavelength of
maximum absorption and record the readings. Determine the calibration curve.
13. Measure and record the absorbance for the ‘Sample.’ Determine the
concentration of the sample solution. Calculate the standard deviation for results
obtained from the calibration curve (a)using your sample and (b) the mean of all
measurement done by the whole class.
14. Calculate the mg Iron present in the tablet by accounting for the dilution factor.
3. SPECTROPHOTOMETRIC DETERMINATION OF Fe2+ IONS USING 1, 10-
PHENANTHROLINE (Standard addition method)
Objectives:
Procedure:
Chemical /Reagents:
KMnO4 0.25 H2SO4
K2Cr2O7
Procedure:
Prepare and standardize a 0.01 M solution of KMnO 4. Then using a measuring pipette,
place 0.5-, 1.00-, 3.00-, and 4.00-mL portions into five 100-mL volumetric flasks numbered
1to 5. Dilute the solution in each flask to the mark with 0.25 M H2SO4.
Using the wavelengths that give the maximum absorption as obtained from (c),
measure the absorbances of the standard solutions at each wavelength. Plot
absorbance vs. concentration for each ion at the two wavelengths and calculate
the molar absorptivity for each substance at each wavelength. If the pathlength id
not known, simply calculate b for each wavelength.
(e) Analysis of the Mixture
Mix a known amount of KMnO 4 and K2Cr2O7 in a 100 ml volumetric flask.
Measure the absorbance at the chosen wavelengths. Calculate the concentration
2-
of MnO4- and the Cr2O7 in this solution. Using t-test, determine if the measured
concentration does not differ from the known value.
5. Analysis of Ethanol in
Rum Objective:
Materials:
Apparatus Chemicals
FTIR with ATR accessory Unknown solution: Vodka sample
Volumetric flasks (10 mL) (~40% ethanol by volume)
Pipettes (1, 2, 5 mL) Pure ethanol (100%, 200-proof)
Procedure:
measurements Objective:
Materials:
Calcium standards:
Samples:
3 mg/L Ca solution
3mg/L Ca solution with 10mg/L P
3mg/L Ca solution with 10 mg/L P, 2000 mg/L Cs
3mg/L Ca solution with 10mg/L P, 2000mg/L Cs,
2000mg/L LaCl3 3 mg/L Ca solution with 100 mg/L Al
3mg/L Ca solution with 100 mg Al/L, 2000mg/L EDTA
Procedure:
1. Determine the absorbance of the calcium standards and samples using the
following schemes.
Ca Standard
1 mg/L
2 mg/L
3 mg/L
5 mg/L
Ca standard+ Cs
1 mg/L
2 mg/L
3 mg/L
5 mg/L
Discussion:
Objectives:
1. To illustrate the types of titration curves obtained with a strong acid and
weak acid against a strong base.
2. To determine the equivalence point of an acid-base titration by graphical methods.
3. To determine the pKa of a weak acid
Chemical/Apparatus:
Approximately 0.1 M HCl
Approximately 0.1 M NaOH
Potassium acid phthalate (KHP)
Burette (50 mL)
Beakers (250 mL)
pH-meter
Magnetic stirrer
Procedure:
Pipette a 25.00 mL of about 0.1 N HCl into 250-mL beaker and dilute the solution to
about 100 mL with distilled water. Place the beaker with solution and spin bar on
magnetic stir plate. Insert and adjust the electrodes into the solution, being sure that
they dip about ½ inch below the surface and the spin bar rotates uniformly without hitting
them. Set up a burette containing about 0.1 NaOH with the tip touching the side of the
beaker to avoid spattering. Measure and record the pH of the solution before the
addition of the titrant. Then add from the burette about 5 mL of the base solution and
again measure the pH. Record this value as well as the burette reading at this point.
Proceed in this manner to record the pH and burette readings after the addition of about 10, 15, and
20 mL of titrant. Then add the titrant in about 1-mL intervals until the equivalent point is almost
reached. Then add the titrant in 0.1-ml intervals until the equivalence point is passed. It will be
evident when this point is reached because of the large change in pH that occurs. Finally, record two
additional readings at about 5 and 10 mL of excess titrant.
Weigh to the nearest 0.1 mg, approximately 0.60 g of standard potassium acid phthalate.
Dissolve the sample in about 100-mL of distilled water and titrate with the sodium hydroxide
solution. Measure the pH at different increments of titrant as in part (a).
Plot the titration data in the same manner as above and compare the curves
obtained for the weak acid and with those obtained for the strong acid. Justify
the selection of the phenolphthalein as the indicator in titrimetric method of
analysis. Determine the pKa of KHP.
8. Ion-Selective Electrode Determination of Fluoride Ion