Analytical Chemistry Ii SCH2106 PDF
Analytical Chemistry Ii SCH2106 PDF
Analytical Chemistry Ii SCH2106 PDF
EXPERIMENT 1 (EC202)
A glass/calomel electrode system is convenient for locating the end points in acid-base
titrations. Ordinarily, prior to a series of titrations, the electrode system is standardized by
means of a buffer of known pH.
REAGENTS NEEDED:
Standardized 0.1 N NaOH; Standard buffer solution (pH = 4)
PROCEDURE:
Read in advance the instructions for using the pH – meter. Prepare the instrument for use.
1. Calibrate the electrode system by rinsing the electrodes with water and immersing
them in buffer solution of pH = 4. Follow the instrument instruction for adjusting the
meter to read this pH.
2. Clean a 50-ml burette and rinse it well with distilled water. Rinse the burette with two
5-ml portions of the standard NaOH solution, and then fill the burette to the zero mark.
Record the concentration of the NaOH solution and the initial burette reading.
3. Obtain an unknown acid sample in a labeled 100ml volumetric flask and then dilute it
to exactly 100ml with distilled water. Mix the solution well, rinse your 25-ml pipette
with the solution and transfer a 25-ml aliquot of the sample to a250-ml beaker. Add a
magnetic stirring bar and about 25ml of water.
4. Rinse the electrodes thoroughly and immerse them in the sample solution. Position the
burette so that the reagent can be delivered without splashing. Commence stirring and
measure and record the initial pH.
5. Titrate the solution with standard NaOH solution, measuring and recording the meter
reading and burette volume after each addition of titrant. Introduce fairly large
volumes ( about 2-ml) at the outset. Withhold a succeeding addition until the meter
reading remains constant within 0.05pH unit for at least 30s. In the immediate vicinity
of the equivalence point introduce the reagent in 0.2-ml increments. Continue the
titration 2 to 3 ml beyond the equivalence point, increasing the volume increments as
the pH difference becomes smaller.
Note: During the titration the solution should be stirred moderately with the
magnetic stirrer. Some samples will contain more than one replaceable
hydrogen; be alert for more than one break in the titration curve.
6. Measure the pH of the sample solution, using a dry beaker and dried electrodes.
PRE-LAB QUESTIONS
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1. What is potentiometry?
2. State the uses of potentiometric titrations.
IN YOUR REPORT:
1. Using a short-hand notation give the conventional representation of the cell used.
2. Tabulate all data necessary for the end-point determination.
3. Plot the titration data and determine the end-point or points. Use the derivative
method for end-point determination, as well. Plot the two curves on the same graph
paper using the same horizontal axis.
4. Calculate the quantity of the respective acid (in g) in the sample solution.
5. Calculate the pH of your unknown solution using the calculated concentration (item 4)
and compare the result with the measured pH value. Discuss the result of this
comparison.
6. Evaluate the accuracy of the analysis.
For H3PO4: k1 = 7.11 x 10-3, k2 = 6.34 x 10-8; k3 = 4.2 x 10-13
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NATIONAL UNIVERSITY OF SCIENCE AND TECHNOLOGY
DEPARTMENT OF APPLIED CHEMISTRY, ANALYTICAL CHEMISTRY II SCH2106
SEMESTER ONE
EXPERIMENT 2 (EC205)
Flame photometry is a simple, rapid method for the routine determination of elements that
are easily excited and especially alkali and alkaline earths. The method is based upon the
emission of electromagnetic radiation by atoms after electronic excitation in flames. For
quantitative determination of potassium the emission power P is measured at 767nm.
PROCEDURE
Prepare calibration standards in the range 0 to 10ppm from the standard solution provided.
SAMPLE: Submit a 100ml volumetric flask for your sample. Mark up to the mark up to mark
with distilled water.
Measure the emission of the calibration solutions (three measurements on each). Run the
sample.
NB. The technician/demonstrator will show you how to operate the Flame Photometer.
PRE-LAB QUESTIONS
IN YOUR REPORT:
1. Calculate the concentration (in mgK/cm3) and the quantity (in g K) in your sample.
2. Is it possible, using same conditions, to determine Zn in a solution. Explain your
answer.
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NATIONAL UNIVERSITY OF SCIENCE AND TECHNOLOGY
DEPARTMENT OF APPLIED CHEMISTRY, ANALYTICAL CHEMISTRY II SCH2106, SEMESTER ONE
EXPERIMENT 3 (EC204)
SPECTROPHOTOMETRIC DETERMINATION OF CHROMIUM (VI) WITH DIPHENY- CARBAZIDE -
Co(NHNHC6H5)2
A sensitive method for determination of trace amounts of chromium is based upon the formation of
the violet compound between Cr(VI) and diphenylcarbazide. The acidity of the solution is of
importance for the formation of the coloured compound and must be kept constant.
This method is used for determination of chromium in different materials, such as alloys, minerals,
glass, water, organic and biological substances.
REAGENTS NEEDED:
Standard Cr(VI) solution - 6 µg/ml; Diphenylcarbazide solution - 0.15% (w/v);
H2SO4 - 5% (v/v); Dist. Water.
PROCEDURE:
1. (a) Into five 50ml volumetric flasks pipette exactly 2.00, 4.00, 6.00, 8.00 and 10.00 ml of the
standard Cr(VI) solution, containing 6µg Cr/ml.
(b) For each student: clean and label one 50-ml volumetric flask and submit it for the
unknown Cr(VI) solution to be placed in it.
(c) Add 2.00 ml 5% H2SO4 and 5.00 ml 0.15% diphenylecarbazide into each of the volumetric
flasks (including that with the unknown solution), dilute to the mark and mix well.
2 Obtaining an absorption spectrum. Measure and record the absorbance A of the most
concentrated solution at different wavelengths (using water as a blank)
λ, nm 400 420 440 460 480 500 520 530 540 550 560 580 600 620
A
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PRE-LAB QUESTION
1. What is spectrophotometry?
2. Draw a block diagram showing the principle components of a spectrophotometer.
3. Industrial application of the method
IN YOUR REPORT:
1. Briefly describe the principle of the determination of CCr.
2. Enclose all experimental data obtained.
3. Plot A = f(λ) to obtain the absorption spectrum.
4. For the five standard solutions (item 3):
a. Plot A = f(CCr) to obtain the calibration curve. From A measured for your unknown
solution and the calibration curve, ascertain CCr in your unknown solution;
b. Calculate the coefficients a and b in the least square equation of the calibration curve
for the determination of Cr with diphenylcarbazide and using it calculate CCr in your
unknown solution.
5. Using the data obtained for the set of four parallel solutions (item 4):
a. Assess whether the highest and the lowest values of A should be rejected or not;
b. Assess the precision of the measurement.
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NATIONAL UNIVERSITY OF SCIENCE AND TECHNOLOGY
DEPARTMENT OF APPLIED CHEMISTRY, ANALYTICAL CHEMISTRY II SCH 2106, SEMESTER ONE
EXPERIMENT 4
SIMULTANEOUS SPECTROPHOTOMETRIC DETERMINATION OF MANGANESE AND CHROMIUM
The concentration of manganese (II) and chromium (III) in a mixture may be determined by
chemical oxidation of these species to permanganate and dichromate, respectively, followed by
spectrophotometric measurement at two wavelengths. This experiment illustrates the principle of
additivity of absorbance due to two substances, and show how absorbance values at two different
wavelengths are employed to calculate the concentrations of the two desired components.
PART 1
PREPARATION OF STANDARD PERMANGANATE AND DICHROMATE SOLUTIONS AND OBTAINING
THE ABSORPTION SPECTRA
PROCEDURE: Weigh the calculated quantity to the nearest milligram, transfer it into 100-cm3
volumetric flask, dissolve in distilled water, dilute to the mark and mix well.
weight of weighing bottle + K2Cr2O7 _ _ _ _ _ _ _ _ _ _ _ _ _ _ _g
weight of empty weighing bottle _______________g
weight of K2Cr2O7 __ _ _ _ _ _ _ _ _ _ _ _ _ _ _g
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PART II
PREPARATION OF CALIBRATION CURVES AND DETERMINATION OF CONCENTRATIONS OF KMnO4
AND K2Cr2O7 IN AN UNKNOWN MIXTURE
TABLE 1
Data for calibration curve 1
No 1 2 3 4
2-
Vol of stand. Cr2O7 soln, ml 2 4 6 8
CCr, mg/ml
A at λ1
(c) Measure A of the four standard solutions containing KMnO4 and your unknown solution at λ1 and
λ2. Data for the calibration curves 2 { Aλ1 = f(CMn)} and 3 {Aλ2 = f(CMn)} are obtained.
TABLE 2
Data for calibration curves 2 and 3
No 1 2 3 4
-
Vol of stand. MnO4 soln, ml 2 4 6 8
A at λ1
A at λ2
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PRE-LAB QUESTIONS
1. What does the Beer-Lambert Law say?
2. Explain the phenomenon of additivity of absorbance
3. State some applications of the phenomenon
IN YOUR REPORT:
1. Calculate the concentration of the standard solutions of K2Cr2O7 and KMnO4 prepared, in mg
Cr/ml and mg Mn/ml, respectively. Fw(KMnO4) =158, eqw(KMnO4) = fw/5 = 31.6, ArMn = 55.
2. Plot the absorption spectra of K2Cr2O7 and KMnO4 (A versus λ) on the same graph paper.
3. From the data obtained (see Tables 1 ad 2) prepare three calibration curves 1, 2, and 3. Then,
from the measured A values of your unknown solution calculate CCr and CMn in the mixture
(remember that at λ2 only MnO4- absorbs radiation).
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NATIONAL UNIVERSITY OF SCIENCE AND TECHNOLOGY
DEPARTMENT OF APPLIED CHEMISTRY, ANALYTICAL CHEMISTRY II SCH2106, SEMESTER ONE
EXPERIMENT 5 (EC207)
PROCEDURE
Prepare calibration standards in the concentration range 0 to 1ppm Cu2+ from the standard solution
provided, which contains 1ppm Cu2+.
SAMPLE: Submit a 100ml volumetric flask for your sample. Make up to the mark with distilled
water.
The technician/demonstrator will show you how to operate the AAS.
Measure the absorbance of the calibration solutions (three measurements on each) Run the
sample.
Plot the absorbance as a function of concentration and from the calibration curve calculate the
concentration of copper in the sample.
PRE-LAB QUESTIONS
1. Draw a diagram to show the main parts of an atomic-absorption spectrophotometer.
2. What processes occur from the time the solution of the metal ion is presented to the
instrument to the time that a signal is produced?
POST-LAB QUESTIONS
1. Calculate the mean and the relative standard deviation for the absorbance readings of the
calibration standards. Comment on any observed variation.
2. What do you consider to be the greatest sources of uncertainty in the analytical process and
how might these be minimized?
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NATIONAL UNIVERSITY OF SCIENCE AND TECHNOLOGY
DEPARTMENT OF APPLIED CHEMISTRY, ANALYTICAL CHEMISTRY II SCH2106, SEMESTER ONE
EXPERIMENT 6 (PC2101)
The chemicals used in this experiment pose little hazard provided that routine laboratory
precautions are taken and the skin contact is avoided. Any drug allergies should be notified
before the beginning of the experiment.
Paracetamol and aspirin both dissolve in 0.1 M sodium hydroxide solution. Paracetamol ionizes to
give p-acetamido-phenolate ion but aspirin is hydrolysed quantitatively to salicylate ion. The E1%1cm
values for the ions formed from paracetamol and aspirin at the peak absorbances are given below.
Paracetamol Aspirin
E1%1cm(258nm) 721 44.6
E1%1cm(297nm) 244 196.
1%
N.B. The E 1cm value is the absorbance of a 1% solution determined in a 1 cm cell.
Unfortunately, the p-acetamidophenolate ion absorbs more strongly that the salicylate ion even at
the wavelength of the maximum absorbance by the latter; the absorbance peaks are therefore not
resolved when the two ions are present in equal amounts. Nevertheless, good results can be
obtained by application of the simultaneous equations:
A258 = 44.6Ca + 721Cp
A297 = 196Ca + 244Cp
Where A258 and A297 are the measured absorbances of the mixture at the two wavelengths,
and Ca and Cp are the concentrations (%w/v) of aspirin and paracetamol respectively. N.B. The
values given above are for guidance ONLY; you should recalculate these from your experimental
data. Use the λMax values you find experimentally in your calculation.
PROCEDURE:
1. Dissolve about 0.1g of paracetamol (p-acetamidophenol) [accurately weighed] in 0.1M
(0.4%) sodium hydroxide solution, and dilute to 100 ml with 0.1M sodium hydroxide solution. Mix
thoroughly and dilute 10ml of this solution to 100 ml with water in the second volumetric flask. Mix
thoroughly and dilute 10ml of this solution to 100ml with water in a third 100 ml volumetric flask.
i.e. approx 0.10g paracetamol 100ml (in 0.1MNaOH)
10ml 100ml (in distilled water)
10ml 100ml (in distilled water)
3. Plot the spectrum from 230-310 nm of the final diluted paracetamol solutions using 1 cm
silica cells against water as a blank. Wash the caustic soda from the cell immediately after use.
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Then plot the spectra of the aspirin and the tablet mix solutions on the same chart paper used for
paracetamol spectrum.
CALCULATIONS
4. Determine λmax and calculate E1%1cm and ε for paracetamol at its wavelength maximum and
at the λmax for the hydrolysed aspirin (from 5)
5. Determine λmax for aspirin and its E1%1cm and ε at its wavelength maximum and at λmax for
paracetamol. (from 4)
6. From the absorbance of the tablet mix solution at the λmax wavelengths for paracetamol and
aspirin, calculate the composition of the solid tablet using the simultaneous equations similar to
those given above but with factors based on your results.
7. To satisfy yourself, the aspirin was hydrolysed to salicylic acid in this procedure, obtain
spectra of aspirin (dissolved in sodium carbonate solution) and of a sample of salicylic acid
(dissolved in sodium bicarbonate or hydroxide solution).
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NATIONAL UNIVERSITY OF SCIENCE AND TECHNOLOGY
DEPARTMENT OF APPLIED CHEMISTRY, ANALYTICAL CHEMISTRY II SCH 2106, SEMESTER ONE
EXPERIMENT 7 (EC0213)
Read the instrument operating instructions accompanying this script and consult a demonstrator
before starting the experiment.
Acetylene flames are used in atomic absorption. The lighting and extinguishing acetylene/air flames
constitute a considerable hazard; the exact instructions in the experimental text should be followed.
Instruction should also be obtained if it is necessary to handle the hollow-cathode lamp light
sources as these run on high voltages.
The chemicals used in this experiment pose little hazard provided that routine laboratory
precautions are taken to avoid ingestion and skin contact.
1. Aims
(i) Impact bead position Adjust the position of the impact bead(controlled by the
silver knurled knob on the front of the spray chamber) to give the maximum
absorbance.
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(ii) Burner Height – Fuel/Oxidant Ratio. The burner has adjustments for rotation, lateral
and height location. The first two of these have been optimized, but the optimum
height depends on the flame stoichiometry i.e. the fuel/oxidant ratio and is
therefore determined interactively with the flame conditions. Adjust the fuel flow
reading in 5 steps over a range from 17-24 mm (this range is appropriate provided
that the oxidant flow reading is 35). At each step, adjust the burner height control
to minimize the reading on the energy meter. Adjust the gain control to restore the
energy reading to its previous value, auto-zero the instrument and record the
absorbance of the standard. Plot the maximum absorbance vs the fuel flow rate and
select a value of the latter which is a compromise between sensitivity and acetylene
consumption.
(iii) Lamp Current. Prepare calibration curves over the range of 0.5 – 1.5 times the
manufacturer’s recommended lamp current for Ca concentrations in the range 5 –
20 ppm (use 4 standards). Note as the intensity of the lamp varies, you will need to
adjust the gain control to ensure that the blue portion of the scale and then auto –
zero before taking the absorbance readings.
(iv) Slit Width. Select in turn each of the spectrometer band –pass settings, and repeat
the measurements outlined in part (iii). Adjust the gain control as required and
auto-zero before taking the absorbance readings. Tabulate your results.
1) 5 ppm Ca
2) 5 ppm Ca + 50 ppm Al
3) 5 ppm Ca + 50 ppm Al + 500 ppm La
4) 5 ppm Ca + 50 ppm phosphate
5) 5 ppm Ca + 50 ppm phosphate in 0.01 m EDTA
Post-Lab Questions.
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