SIC 1011
LAB REPORT A2- VOLUMETRIC ANALYSIS
PREPARED FOR: ASSOCIATE PROF. DR. WOI PEI MENG
NAME SUMAYYAH BINTI
LOKMAN
MATRIX NO. 22003285/1
SEMESTER 1
OCCURANCE 1
DATE OF 15th NOVEMBER 2022
EXPERIMENT
TITLE
Volumetric analysis
OBJECTIVES
i) To understand the concept of volumetric analysis
ii) To determine the unknown solution concentration via titration using standardize
solution.
METHODOLOGY
Part A
0.8 to 1.0g of potassium permanganate is
O.3g of sodium oxalate is weighed
weighed and transferred into a 250ml
and transferred into 100ml volumetric
volumetric flask.50ml of distilled water is
flask. 20ml of distilled water is added
added and the volumetric flask is shaken.
followed by 5oml of dilute sulfuric
Distilled water is used to top up to the
acid(2.5M) and distilled water is used
calibration mark. Some of the solution is
to top up to the calibration mark.
poured into a burette.
25ml of sodium oxalate solution is
The molarity is of potassium pipetted into 250-ml conical flask. The
permanganate solution is calculated. solution is heated to 80℃ and the hot
solution is titrated with potassium
permanganate. The process is repeated
2 more times.
10ml of potassium permanganate The beaker is heated to 40℃ and 8ml
solution is transferred into a 400-ml of nitrite solution is added from a
beaker and dilute sulfuric acid (1:5) is burette. The tip of the burette is rinsed
added to the 100-ml mark. with distilled water and the solution is
cooled to room temperature.
The standard iron (ii) ammonium
sulfate solution is poured in a burette
The molarity of nitrite solution is and titrated against nitrite solution. This
calculated. process is repeated 2 more times.
Part B
The burette is filled with sodium 25 ml of potassium iodate solution
thiosulfate solution. About 0.2g of is pipetted into a 250ml conical
potassium iodate solution is flask. 1g of potassium iodate
weighed and dissolved with distilled followed by 5ml of sulfuric acid
water in a 100ml volumetric flask. (1M) is added to the conical flask.
The titration is continued until the
solution turns colorless and the The liberated iodine is titrated with
titration is repeated 2 more times. the thiosulfate solution immediately.
The average molarity of the 100ml of distilled water is added
thiosulfate solution is calculated. when the mixture turns pale yellow
followed by 1 to 2 ml of freshly
prepared starch solution.
10 ml of chlorox solution is pipetted The liberated iodine is titrated with
into a conical flask. 40 ml of distilled the standard thiosulfate solution and
water, 1g of potassium iodide and the titration is repeated 2 more
10ml of sulfuric acid (1 M) is added times. The average concentration of
in the conical flask. hypochlorite in the chlorox is
calculated (expressed in %𝐶𝑙2 .
RESULTS AND CALCULATION
Part A
Table 1: Mass of sodium oxalate and potassium permanganate used
Mass of sodium oxalate (g) 0.3015
Mass of potassium permanganate (g) 0.8806
Table 2: titration of sodium oxalate and potassium permanganate solution
Titration 1 2 3
Initial reading (ml) 5.80 15.90 25.50
Final reading (ml) 15.90 25.50 35.20
Volume of potassium permanganate (ml) 10.10 9.60 9.70
10.10 + 9.60 + 9.70
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑝𝑜𝑡𝑎𝑠𝑠𝑠𝑖𝑢𝑚 𝑝𝑒𝑟𝑚𝑎𝑛𝑔𝑎𝑛𝑎𝑡𝑒 = = 9.8 𝑚𝑙
3
0.3015𝑔
𝑚𝑜𝑙𝑒 𝑜𝑓 𝑠𝑜𝑑𝑖𝑢𝑚 𝑜𝑥𝑎𝑙𝑎𝑡𝑒 = = 2.2502 × 10−3 𝑚𝑜𝑙
133.99 𝑔 𝑚𝑜𝑙 −1
2.2502 × 10−3
𝑚𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑁𝑎2 𝐶2 𝑂4 = = 0.0225 M
0.1𝑙
𝑀𝐾𝑀𝑛𝑂4 × 9.8 2
=
0.0225 × 25 5
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝐾𝑚𝑛𝑂4 = 0.02296 ≈ 0.0230𝑀
Table 3: titration of standard iron (ii) ammonium sulfate and nitrite solution
Titration 1 2 3
Initial reading (ml) 0.00 11.65 23.45
Final reading (ml) 11.65 23.45 35.00
Volume of iron (ii) ammonium sulfate 11.65 11.80 11.55
(ml)
concentration of (𝑁𝐻4 )2 𝐹𝑒(𝑆𝑂4 )2 ⋅ 6𝐻2 𝑂 = 0.0106𝑀
11.65 + 11.80 + 11.55
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑖𝑟𝑜𝑛 (𝑖𝑖)𝑎𝑚𝑚𝑜𝑛𝑖𝑢𝑚 𝑠𝑢𝑙𝑓𝑎𝑡𝑒 = = 11.67 𝑚𝑙
3
𝑀𝑀𝑛𝑂4 × 𝑉𝑀𝑛𝑂4 𝑎
2+ 2+
=
𝑀𝐹𝑒 × 𝑉𝐹𝑒 𝑏
0.0230 × 𝑉𝑀𝑛𝑂4 2
=
0.0106 × 11.67 10
𝑉𝑀𝑛𝑂4 = 1.0757 𝑚𝑙 (𝑙𝑒𝑓𝑡𝑜𝑣𝑒𝑟)
10ml - 1.0757ml = 8.9243 ml (excess, react with nitrite)≈ 8.92𝑚𝑙
𝑀𝑁𝑂2− × 𝑉𝑁𝑂2− 5
=
𝑀𝑀𝑛𝑂4 × 𝑉𝑀𝑛𝑂4 2
𝑀𝑁𝑂2− × 8 5
=
0.0230 × 8.92 2
𝑀𝑁𝑂2− = 0.0641𝑀
Part B
Mass of sodium thiosulfate= 0.2079g
Mass of potassium iodide=1.0048g
Table 4: titration of sodium thiosulfate and potassium iodate
Titration 1 2 3
Initial reading (ml) 0.00 12.60 25.10
Final reading (ml) 12.60 25.10 24.90
Volume of sodium thiosulfate (ml) 12.60 12.50 12.40
Table 5: Titration of sodium thiosulfate solution and chlorox solution
Titration 1 2 3
Initial reading (ml) 1.90 25.40 0.00
Final reading (ml) 25.40 48.80 23.90
Volume of sodium thiosulfate (ml) 23.50 23.40 23.90
DISCUSSION
Volumetric analysis is a widely used quantitative analytical technique. As the name implies,
the volume of a solution which concentration is known is measured and then used to calculate
the concentration of the analyte. In the presence of an indicator, the reagent of unknown
concentration combines with a chemical of unknown concentration to reveal the end-point. It
marks the point at which the reaction has completed. The amount of reagent and solution is
determined by the volume and concentration of the reagent used in the titration. Moreover, the
mole fraction of the equation is used to calculate how much unknown chemical is present in
t h e s p e c i f i e d v o l u m e o f t h e s o l u t i o n .
Based on the result, the molarity of potassium permanganate is 0.0230M. The leftover volume
of potassium permanganate is 1.0757ml which is used to react with iron (II) ammonium sulfate.
The equivalence point of titration can be determined when the amount of titrant added is
enough to neutralize the analyte solution, where the number of moles of base is equal to number
o f m o l e s o f a c i d .
The source of error in this experiment includes end point error which Is caused by overshooting.
Other than that, misreading the volumes can also contribute in error in this experiment.
SAFETY PRECAUTIONS
1. After adding the indicator and with the addition of each drop of solution from the
burette, the flask should be thoroughly shook.
2. Towards the end, the solution is added drop by drop and swirl to avoid errors
3. Remove the funnel immediately after filling the burette to avoid running over it.
4. Make sure that the stop cock does not leak.
QUESTIONS
1. Acid base indicator is a chemical substance that change color with Ph. It is used to
determine wether the aqueous solution is acidic, basic or neutral.
2. The equivalence point of a titration is determined by observing the point when the
indicator change color. It is the point where number of moles of acid is equal to the
number of moles of base.
REFERENCE
1. Admin. (2022, July 27). Volumetric analysis - procedures and basic principles of
analysis. BYJUS. Retrieved December 11, 2022, from
https://byjus.com/chemistry/volumetric-analysis/
2. Yousuf, D. J. (2013, May 23). Precautions in gravimetric & volumetric analysis
presented by: Dar Jaffer Yousuf Aem-Ma ppt download. SlidePlayer. Retrieved
December 11, 2022, from https://slideplayer.com/slide/10787558/
