LABORATORY ASSIGNMENT

SKA 3013-ANALYTICAL CHEMISTRY

SEMESTER 2 2019/2020

PART A

GROUP MEMBERS :

NAME MATRIC NUMBER

1. NABILA HUSNA BINTI MOHD KHAZAID D20181083131
2. SITI NUR ATIKAH BINTI JUSOF D20181083150

GROUP :C

LECTURER : DR. MAZLINA BINTI MUSA

LAB1 : GRAVIMETRIC ANALYSIS

1. State the sample number of chloride used by student. Why the number is important?

= Chloride 345. Because these are unknown salts with different percentages of
chloride by mass. The sample number need to be recorded. So, lab of our TA can give
accepted percentage of chloride in the salts and make sure get the right number.

2. State the solution contained in beaker and graduated cylinder.

= Beaker: 0.1g to 0.15g sample salts + 100mL water + 6M nitric acid, HNO3

Graduated cylinder: 0.1M silver nitrate, AgNO3

3. What can you observe after 2 minutes the solution was heated?

= There are some clumps on the bottom of the solution but the supernatant liquid still
very cloudy

4. Name the technique was used by Alice to transfer the solution into the crucible during
filtration?

= Decantation technique

5. Name the chemical was added into the crucible to ensure no more silver is present in the
sample.

= Hydrochloric acid, HCl

LAB 2: LIQUID-LIQUID EXTRACTION

1. What kind of substance was added into the beaker before the water boiled?

= 75mL of distilled water and a few boiling stones.

2. How many sachet/s of tea were added into boiled water?

= Two sachets tea

3. How the researcher squeezed the tea sachet after boiled?

= By squeezing the tea sachet between two watch glasses

4. Name the chemical was added into the tea solution after cooled? How much it is used.

= 1g of sodium carbonate (Na2CO3)

5. Write the chemical equation for reaction tannins between sodium carbonate.

= ArOH + Na2CO3 ArONa + NaHCO3

6. How many layers of solution can you observed from this experiment?

= 2 layers of solution

7. Name the apparatus used by researcher to separate the layers?

= Separatory funnel

8. What is the purpose of dichloromethane added into the tea solution?

= To extract caffeine from an aqueous extract of tea leaves because caffeine is more
soluble in dichloromethane than in water.

9. What was a drying agent used in this experiment?

= Anhydrous sodium sulphate (Na2SO4)

10. How did the researcher determines the solution is dry when after drying agent was
introduced?

= There is no water left in the solution because sodium sulfite is an insoluble

inorganic that will absorb water

11. How the researcher purified the caffeine?

= By putting the solution in the water bath and by using vacuum filtration

LAB 3: STANDARDIZATION OF SODIUM HYDROXIDE

1. Name the primary standard used in this experiment to standardize sodium hydroxide?
How many grams it was used?
= Potassium hydrogen phthalate. 0.919 g was used.

2. State the indicator added into the primary standard solution?

= Phenolphthalein.

3. What was colour appeared at equivalent point in this experiment?

= Pink colour will appear.

4. What is difference between equivalent and end points?

Equivalent point End point

It gives the point where reaction It does not give the point where
ends. reaction ends.
Not always indicated by the color Always indicated by the color
change of the reaction mixture. change of the reaction mixture.

The point at which an equivalent The point which the reaction is

or stoichiometric amount of titrant observed to be completed.
is added to the analyte.

5. What is the concentration of sodium hydroxide was tested in this experiment?

= Concentration of NaOH: 0.200 M

6. Write the equation of reaction?

NaOH (aq) + KHC8H4O4 (aq) → KNaC8H4O4 (aq) + H2O (l)

7. State the initial & final volume of sodium hydroxide in the burette.

= Initial: 0.60 mL

Final: 23.15 mL

8. What was the total volume of sodium hydroxide was used in this experiment?

Total volume of NaOH used = 23.15 mL – 0.60 mL

 = 22.55 mL

9. Why primary standard used to standardize acid or base?

= Primary standard are often used to make standard solution, solution with a
precisely concentration. In this experiment KHP is used as a primary standard, it does
not absorb water or carbon dioxide thus it does not change the mass.

10. What is the pH of the solution at the end point?

= The pH of the solution is 7 which is neutral.

11. A 50.00 mL aliquot of 0.100 M HCl is titrated with 0.100 M NaOH. Calculate the pH of the
solution after addition of 0, 5, 10, 25, 30, 45, 50, 65, 75, 90 and 100 mL of NaOH. Show the
calculation works. Draw the titration curve of strong acid-strong base titration and determine
the pH at equivalent point of the solution.
Volume of NaOH
pH
added (mL)
0.00 1.000
5.00 3.606
10.00 3.620
25.00 3.727
30.00 3.796
45.00 4.323
50.00 7.000
65.00 10.237
75.00 10.495
90.00 10.748
100.00 10.875
 HCl and NaOH Titration Curve of pH vs Volume of NaOH Added

11

10

7
7

6
pH

1
0 10 20 30 40 50 60 70 80 90 100

Volume of NaOH added (mL)

LAB 4: DETERMINATION OF CAFFEINE IN BEVERAGES USING HIGH PERFORMANCE
LIQUID CHROMATOGRAPHY (HPLC)

1. Name the drinks that have been analysed by the student using HPLC.

= Coffee, tea, diet soda and regular soda.

2. Why pure caffeine was used in the analysis?

= In order to identify there is indeed caffeine in a samples and also as a pure standard
to compare with the other samples.

3. How many percent of sample dilution has been prepared by the student?

= 20% dilution.

4. Which part of the instrument the sample was injected?

= Injection port.

5. Name the first sample was injected into the instrument?

= Pure Caffeine.

6. State the size of the syringe was used by student to inject the sample into the instrument?

= 100 µl.

7. How long the sample was scanned by HPLC?

= 2-5 minutes.

8. Specify the caffeine’s time for all drinks appear on the graph.

= 5 minute.
9. What is a composition of mobile phase used in the experiment to analyse caffeine in the
sample?

= Aqueous component.