‡

Clean and oven-dry two petridish

Cool in a Dessicator

Weigh with filter paper

Rinse pipette with unknown

Transfer 25 mL to 250 mL beaker and dilute with 75 mL 0.1 M HCl

Add 5 drops of Methyl red

Filter through Funnel

Add 15 g of solid urea. Cover with watch glass. Boil for 30 minutes

Add 25 mL of ammonium oxalate. Stir

Add 3 mL of cold water to the beaker

Repeat to transfer all precipitate

Add 10 mL of cold water to rinse

Weigh the petridish. Calculate the weight of Ca and average

Place in a dessicator

Transfer filtered precipitate to petridish. Dry in an oven, 1 2 hrs

‡

Measure 8-9 mL of concentrated HCl with a pipet

Place the HCl to 200 mL distilled water in a 1-L volumetric flask

Mix thoroughly and store in a glassstoppered bottle. Label.

Measure 4-5 mL of 50% NaOH with a pipet

Place the NaOH sol'n to 200 mL of distilled water in a 1-L volumetric flask

Mix and store in a tightly capped polyethylene bottle. Label

Protect the sol'n from the atm

Squeeze the bottle while tightening the cap

Dry a quantity of primary-standard KHP

Weigh individual 0.7-0.8 g duplicate samples of the dried KHP into 250 mL E. flask

Dissolve each in 50-75 mL of distilled water

Calculate the concentration of the NaOH sol'n (M). Get the average M of NaOH

Titrate with base until the pink color of the indicator persists for 30 s

Add 2 drops of phenolphthalein

Place a test tube/ small beaker over the top of the burette with NaOH

Record the initial volumes of acid and base in the burettes to the nearest 0.01 mL

Deliver 25 mL of the acid into a 250-mL E. flask

Rinse the tip of the burette with distilled water from a wash bottle

Carefully add base until faint pink hue that persists 30 s

Again rinse down the walls of the flask

Introduce acid dropwise to discharge color

Add 2 drops of phenolphthalein and a sufficient base to become a definite pink

Record the final burette volumes (nearest 0.01 mL)

Repeat the titration twice

Calculate the M of HCl and average of the 2 trials.

Dry a quantity of unknown sample for 2 hrs at 110ºC

Cool it in a desiccator

Weigh individual 0.200.25-g duplicate samples into 250mL E. flask

Dissolve each in 50 mL distilled water

Determne an indicator correction by titrating 100 mL of 0.05M NaCl and 3 drops indicator.

Boil the sol'n to 2-3 minutes, cool it and complete titration

Titrate with standardized HCl until the color changes from blue to green

Put 3 drops of bromocresol green

Boil briefly, cool, and complete the titration

Subtract any volume needed for the blank from the titration volumes

Calculate the weight of the Na2CO3 in the sample

Compute for the average % Na2CO3

Ask for a liquid sample containing a mixture of bases

Pipette triplicate 25mL aliquot portions of liquid into separate E. flasks

Add 2 drops of phenolphthalein indicator and titrate the sol'n with the standard HCl until a light pink color appear

Record the volume of HCl used

To the same sol'n, add 2 drops of methyl orange indicator and titrate until the color becomes peach

Record the volume of HCl used

From the 2 volumes of HCl, determine the components of the unknown sample as to (NaOH & Na2CO3) or (NaHCO3 & Na2CO3)

Compute the concentration of the two basic components in the unknown mixture

Experiment No. 6
Determination of Ionization Constant of a Weak Acid By Potentiometric Titration

OBJECTIVES
To be familiar with the concepts of potentiometric titration To know the proper techniques in potentiometric titration To determine the ionization constant of a weak acid

PROCEDURES

GRAPHICAL METHOD OF SELECTION OF ENDPOINT
(APPROXIMATION OF THE EQUIVALENCE POINT)

DIFFERENTIAL METHOD OF DETERMINATION OF EQUIVALENCE POINT

1oo mL aliquot (400 mL beaker)

Add 1mL interval at the volume before the sudden change. Record pH.

Change 1mL to 0.5 mL interval during the sudden change. Record the pH.

Prepare graph 2, plotting the change in pH/V vs ave. V

Prepare graph 1, plotting the pH vs the NaoH used

Add 1mL of the titrant after the sudden change in pH. Record pH.

Determine the volume of titrant used to reach equivalence point and conc. of unknown

Determine volume for the 50% neutralization and pKa of unknown

LEARNINGS AND INSIGHTS 
Through potentiometric titration, one can determine the ionization constant of a weak acid  Use of pH meter

Dry 2.0 g of primarystandard-grade CaCO3

Weigh duplicate samples of 0.2-0.25 g of the dry CaCO3

Transfer it to a 250 mL e.flask

To each sample, add 5 mL of concentrated HCl sol'n , then 50 mL of distilled water

To the flask, add 5 drops of Eriochrome Black T indicator and titrate with 0.005 M EDTA

Pippette 25 mL aliquot portion of the CaCO3 sol'n to a 250 mL e.flask and add 10 mL of NH3 buffer

Tranfer the cooled sol'n to a 500 mL v.flask and dilute

Boil for 5 minutes

Calculate the molarity of EDTA sol'n

Then, the average of the EDTA concentration

Pipette triplicate 50 mL aliquot portions of the water sample into a 250 e.flask

Add 10 mL NH3 to each sample

Add 5 drops of EBT indicator and titrate with the 0.005 M EDTA until clear blue color appears

Calculate the water hardness as ppm CaCO3

Repeat the titration with the remaining samples

Dry 1.0 g of primarystandard Na2C2O4 at 110ºC for 1 hr. cool it in a desiccator

Weigh duplicate samples of 0.2-0.3 g into 400 mL beakers

Dissolve each in 250 mL of 1 M H2SO4

Do a blank titration with 1M H2SO4 with KMnO4

Reheat if the temperature drops below 60ºC

Heat each sol'n to 8090ºC and titrate with KMnO4 while stirring with a thermometer

Correct the titration data by subtracting the volume obtain from blank titration

Calculate the concentration of the KMnO4 sol'n

Determine the molarity of the KMnO4 sol'n

Dry the unknown for 1-2 hrs

Weigh 0.25-0.30 g duplicate samples in 250 mL beakers

Add 10 mL concentrated HCl dropwise

Add 10 mL of water to each sample and cover with a watch glass

Add 5 drops of saturated bromine water and boil gently for 5 minutes

Dilute each sample solution to about 50 mL, heat to boiling, and add 100 mL of hot 6% (w/v) (NH4)2C2O4 sol'n

Add 3 to 4 drops of methyl red, and precipitate CaC2O4 by slowly adding a 6 M NH3 sol'n

Allow the sol'n to stand for no more than 30 min and then filter

Continue until the sol'n becomes the intermediate yelloworange color of the indicator.

When the indicator starts to change color, add the NH3 at a rate of one drop every 3-4 sec

Wash the precipitates with several 10-ml portions of cold water

Rinse the outside of the crucibles to remove residual (NH4)2C2O4

Return them to beakers where the CaC2O4 was formed

Add 100 mL of water and 50 mL of 3 M H2SO4 to each of the beakers containing the precipitated CaC2O4 and crucible

Heat to 80-90ºC, and titrate with 0.02 m KMnO4 sol'n

Report the percentage of CaO in the unknown

The temperature should be greater than 60ºC throughout the titration; reheat if necessary

EXPERIMENT NO. 12

OBJECTIVES
‡ To be familiar with the Oxidation/Reduction Titration. ‡ To determine the Ascorbic Acid Content of Vitamin C tablets using the standard Potassium Bromate (KBrO3) Solution.

Schematic Diagram
‡ ‡ ‡ ‡ ‡ ‡ ‡ ‡ 3 5 g Vitamin C Pulverize 0.04 0.05 sample (250mL Erlenmeyer Flask) Dissolve (50mL 1.5M H2SO4) 5g KBr Titrate w/ KBrO3 (Faint yellow) 3 g KI & 5mL starch indicator Back titrate (Na2SO3)

Learnings/Insights
‡ Using Iodometric Method, one can calculate the ascorbic acid content of Vitamin C ‡ Balancing Redox Reactions ‡ Redox Titration

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