COMPOUND TYPE OF CHEMICAL EQUATIONS AND CALCULATIONS ASSAY PROCEDURE AND REASONS FOR

TITRATION AND IMPORTANT STEPS

REACTION

Analyte: Sodium Type of Half - Reaction: Assay Procedure

Hypochlorite Solution
Molecular Formula: NaOCl
Molecular Weight: 74.44
g/mol
Indicator Used: Starch TS
Color
Transition/Endpoint: Blue-
black to light greenish blue
solution
Official Requirement:
Sodium Hypochlorite Solution
contains not less than 4.0
percent and not more than 6.0
percent, by weight of sodium
hypochlorite.
Analysts:
Gonzales
Reyes
Oloroso
Codorniz
Valles
Titration: Iodome Reaction between hypochlorite and iodide Dilute the 3 g NaOCl solution with 50 ml of water,
try OA: and add 2 g of potassium and 10 ml of 6N acetic
Type of 2e- + 2H+ + OCl- > Cl- + H2O acid . titrate the liberated iodine with 0.1 N sodium
Reaction: Redox RA: thiosulfate VS, adding 3 ml of starch as the
reaction 2I- >I2 + 2e- endpoint is approached. Perform blank
OA: Sodium Net Ionic Equation: determination and make any necessary correction
Hypochlorite 2H+ + 2I- + OCl-> I2 + Cl- + H2O Reason/s For Important Steps:
RA: Potassium Reaction between iodine and thiosulfate  Use iodine flask when performing
Iodide and Sodium OA: iodometry/iodimetry type of assay to prevent
Thiosulfate 2e- + I2 > 2I- the escape of iodine which will be reacted
RA: with the titrant.
Titrant/s: 0.1 N 2S2O32-> S4O62- + 2e-  Loosen the stopper when adding the titrant
Sodium Net Ionic Equation: in to the analyte. Don’t fully open the flask
Thiosulfate VS I2 + 2S2O32- >2I- + S4O62 as it may cause the iodine to escape.
Special Factor: 2  The sample solution is diluted before
Conditions: Wea Explanation: The oxidation state of the chloride in the hypochlorite ion is titration to convert the sodium hypochlorite
kly acidic. +1, gaining electrons in the reaction in the reaction, and is reduced to -1 to hypochlorous acid, because
(same for sodium thiosulfate, losing two (2) electrons). The factor is hypochlorous acid is the who react with
determined by the number of electrons gained/loss in the reaction, potassium iodide.
therefore the factor is two (2).  Addition of potassium iodide to liberate
Pre- Lab Computations: iodine.
Wt. = 0.1 N x 30 ml x 74.44 g/mo/1000 x 2 = 0.1116 g NaClO  Addition of acetic acid because it is a weak
0.1116/ (5g/100g) = 2.2332 g NaClO solution acid and starch TS is sensitive in highly
*5% = From USP, OR of NaClO solution acidic medium. And if you add strong acids
Post - lab computations: Cl2 and O2 will liberate.
 Add the starch TS when the solution imparts
a pale light yellow solution.
 Do not add starch TS at the
beginning as it may give undesirable
results.
Analyte: Potassium
permanganate
Molecular Formula: KMnO4
Molecular Weight: 158.034
g/mol
Indicator Used: no indicator
used since potassium
permanganate is a self
indicating substance.
Color
Transition/Endpoint: colorle
ss to faint pink
Official Requirement:
NLT
Analysts:
Mojica, Maria Madel
Type of Half - Reaction STANDARDIZATION:
Titration: Indirect OA: Dissolve about 3.3g of Potassium Permanganate in
titration RA: 1000 ml of water in a flask, and boil the solution for
Type of Net Ionic Equation: about 15 minutes. Insert the stopper in the flask,
Reaction: Reducti 2MnO4- + 16 H+ + 5C2O42- → 2Mn2+ + 8H2O + 10CO2 allow it to stand for at least 2 days, and filter
on-Oxidation Factor: through a fine-prosperity, sintered-glass crucible. If
Reaction Pre-lab computation: necessary, the bottom of the sintered-glass crucible
Titrant Used: 0.1 Post-lab computation: may be lined with a pledget of glass wool.
N Potassium Standardize the solution as follows.
permanganate
Requirement: ASSAY PROCEDURE:
Analyte should be Accurately weigh about 200 mg of Sodium Oxalate,
at 70 C - 80 C. dried according to the instructions on its label, and
OA: potassium dissolve it in 250 ml of water. Add 7 ml of sulfuric
Permanganate acid, heat to about 70 C, and then slowly add the
RA: sodium permanganate solution from a buret, with constant
oxalate stirring, until a pale pink color, which persists for 15
seconds, is produced. The temperature at the
conclusion of the titration should be not less than
60 C. Calculate the normality. Each 6.700 mg of
sodium Oxalate is equivalent to 1 ml of 0.1 N
potassium Permanganate.
Since potassium permanganate is reduced on
contact with organic substance such as rubber, the
solution must be handled in apparatus entirely of
glass of other suitably inert material. It should be
frequently restandardized. Store in glass-
stoppered, amber-colored bottles.
REASONS FOR IMPORTANT STEPS:
1. Any Organic matter that may be present in
distilled water is decomposed by potassium

Analyte: Ascorbic Acid
Tablets (Miscellaneous
Redox Reaction)
Molecular Formula: C6H8O6
Molecular Weight: 176.12
g/mol
Indicator Used: No indicator
used
Color
Transition/Endpoint: rose
permanganate. Consequently after the solution of
potassium permanganate is affected, the liquid is
allowed to stand for 2 days to ensure completion of
the decomposition reaction.
2. The solution is then filtered through a Buchner
funnel using a sterile membrane, to remove traces
of manganese dioxide, which if present it acts as a
catalyst to promote the formation of more
manganese dioxide at the expense of
permanganate ion.
3. Sodium Oxalate is the best standard to be
used in the standardization of potassium
permanganate, since it can be obtained in very
pure condition.
4. Sufficient sulfuric acid must be added to keep
the hydrogen ion concentration reasonably
constant throughout the titration. thereby preventing
the formation of manganese dioxide and supplying
the hydrogen ions used up in the reduction of the
permanganate ion.
5. The Buret used to measure the permanganate
solution should be washed out immediately after
use to prevent the formation of a deposit of
manganese dioxide on the buret wall.
Type of Half - Reaction: Assay Procedure:
Titration: Direct Sample Stock Solution:
Titration with blank Transfer NLT 20 tablets to a 100-mL volumetric
determination flask containing 250mL of metaphosphoric-acetic
Type of acid TS. Insert the stopper in the flask, and shake
Reaction: Redox by mechanical means for 30 mins or until the
Reaction tablets have disintegrated completely. Dilute with
OA: Dichlorophen water to volume.
ol-indophenol VS Sample Solution:
RA: Ascorbic Acid Transfer a portion of the sample stock solution to a
tablets centrifuge tube, and centrifuge until a clear
pink color that persists for at Titrant/s: Dichloro supernatant is obtained. Quantitatively dilute the
least 5 sec phenol - clear supernatant with water, if necessary, to obtain
Official Requirement: indophenol VS a solution containing 0.5mg/mL of ascorbic acid.
Ascorbic Acid tablets contains Special Blank:
NLT 90.0% and NMT 110.0% Conditions: a mixture of 5.5mL of metaphosphoric-acetic acid
of the labeled amount of TS and 15 mL of water
ascorbic acid Analysis: Transfer a volume of the sample solution
Analysts: equivalent to 2mg of ascorbic acid, into 50-mL
Argana conical flask. Add 5 mL of metaphosphoric acetic
Figueroa acid TS and titrate with titrant. Correct the volume
Manalo of titrant consumed by blank. Calculate the
Oloroso percentage of the labeled claim amount of ascorbic
Robles acid in portion of the tablets taken:
Zamora
Results = { } x 100
Acceptance criteria: 90.0% - 110.0%

Reason/s For Important Steps:

1. No indicator necessary, since the oxidized
form of the dichlorophenol-indophenol is
blue in alkali and red in acid, while reduced
form is colorless, thus the appearance of
pink color as the endpoint is indicated due
to the acidic environment.
2. Blank determination is done to identify some
interference with titrant and analyte.

OA: Dichlorophenol-indophenol VS
RA: Ascorbic Acid
Factor: 2
 Pre- Lab Computations:
Equivalent volume: 0.5mg/mL=2mg/x =4mL (needed volume from sample
stock sol’n to get 2mg of ascorbic acid)
Post - lab computations:

Analyte: Ascorbic Acid Type of Assay Procedure:

Molecular Formula: C6H8O6 Titration: Direct Blank:
Molecular Weight: 176.12 with blank 100 mL of water and 25 mL of 2N sulfuric acid. Add
g/mol determination 3 mL of starch TS
Indicator Used: Starch TS Type of Analysis:
Color Reaction: Redox Dissolve the sample in a mixture of 100 mL of
Transition/Endpoint: colorle Reaction water and 25 mL of 2N sulfuric acid. Add 3 mL of
ss to blue OA: Iodine starch TS and titrate immediately with titrant until a
Official Requirement: RA: Ascorbic Acid persistent violet-blue color is obtained.
Ascorbic acid contains NLT Titrant/s: 0.1 N Reason/s For Important Steps:
99% and NMT 100.5% of Iodine VS 1. Ascorbic acid in neutral conditions is
C6H8O6 Special rapidly oxidized by oxygen. And the
Analysts: Conditions: Anal addition of acid helps to have a more
Alarcos yte must be in rapid reaction.
Encabo acidic condition 2. Titration must be done quickly in order
Magaling to prevent atmospheric oxidation of
Nolasco
Ascorbic acid to dehydroascorbic acid.
Reyes
Velasco 3. Blank determination will help in
determining errors. Also, its purpose is
to know the equivalence point of the
titration
OA: Iodine
RA: Ascorbic Acid
Factor: 2, because ascorbic acid gave off 2 electrons in order to form
dehydroascorbic acid.
Pre- Lab Computations:

Wtascorbic acid= 0.1 N iodine VS x 30 mL x

= 0.2642 g

Analyte: Thymol
Molecular
Formula: C10H14O
Molecular Weight: 150.221
g/mol
Indicator Used: Methyl
Orange
Color
Transition/Endpoint: Bleac
hing of methyl orange
Official Requirement:
-Thymol contains not less than
99.0% and not more than
101.0% of C10H14O
Analysts:
Culajara, Jerlin
Laquindanum, Shaira
Post - lab computations:
Type of Chemical Reaction: Assay Procedure
Titration: Iodome Transfer about 100mg of thymol to a iodine-flask and
try dissolve in 25mL of 1N sodium hydroxide. Add 20mL
Type of Assay: of hot diluted hydrochloric acid (1 in 2) and
Indirect Titration immediately titrate with 0.1N bromine VS within 1 to
Type of 2 mL of the calculated endpoint. Warm the solution
Reaction: Redox to 70 and 80¬oC, add 2 drops of methyl orange TS
reaction and continue titration slowly, swirling vigorously after
OA: 0.1 N C10H14O + 2Br2 ------> C10H12Br2O + 2HBr each addition. When the color of the methyl orange
Bromine VS Half - Reaction: is bleached add 2 drops of 0.1N bromine VS, shake
RA: Thymol 2 (C10H14O + 2e- ------> C10H12O + 2H+) for 30 seconds, add 1 drop of methyl orange ts and
4e- + 2Br2 ------> Br2 - + 2Br- shake vigorously. If the solution is red, continue the
Titrant/s: 0.1 N OA: 0.1N Bromine Vs titration, dropwise and with shaking until the color is
Bromine VS RA: Thymol discharged. Repeat the alternate addition of the
Special Factor: 4 titrant and methyl orange ts until red color is
Conditions: Explanation: discharged after the addition of the ts.
 Dilute HCl Since 1 mole of thymol reacts with 2 mol. 4 equivalents of bromine under Each mL of 0.1 N bromine is equivalent to 3.755mg
should be the condition of the assay, the equivalent weight of thymol is 37.55 g, ¼ of C10H14O
hot before gram molecular weight. Therefore, 0.003755 g Reason/s For Important Steps:
it is being Pre- Lab Computations: 1. NaOH: Thymol is only slightly soluble in water at
used in Wt. analyte = N Standard x V Standard neutral pH, but it is extremely soluble in alcohols and
assaying x other organic solvents. It is also soluble in strongly
 Ratio of alkaline aqueous solutions due to deprotonation of
hydrochlori the phenol. Due to the presence of phenolic group,
c acid and It is also soluble in strongly alkaline aqueous
water solutions and gets deprotonated.
should be Wt. analyte = 0.1 N x 30 mL x Due to the presence of activating group (hydroxy
1 is to 2. Wt of Thymol = 112.67 mg, Thymol group) in phenol, it undergoes electrophilic
Mojica, Madel substitution reactions readily and forms
Pereyra, Laica Post - lab computations: polysubstitution products. The hydroxy group in
Uy, Yaneza 1. % Purity phenol is –o and –p directing group, hence
substitution takes place at both position.
2. Hot diluted HCl: hydrochloric acid is heated to
liberate carbon dioxide, HCl: free bromine is only
released upon the addition of an acid
5KBr + KBrO3 + 6HC1 -> 3Br2 + 6KC1 + 3H2
3. Warming of solution: to produce a bromo-
derivative. Bromine reacts vigorously with alkalies to
produce hypobromites and bromides (4). If the
reaction mixture is heated the hypo bromites
undergo auto-oxidation forming bromates and more
bromide (Remmington)
4. Bleaching of methyl orange: The hypobromous
acid is slowly decomposed to yield oxygen which is
responsible for the bleaching property. Bleached
when the equivalence point is exceeded. Bromine is
a very reactive element. Indicators such as Methyl
2. % Pave orange actually change colour due to a mechanism
called tautomerism. This is when the molecule
changes from one arrangement of atoms to another.
One form is coloured A the other form B is a different
colour. It usually involves the movement of hydrogen
ions in the molecule, hence is pH sensitive. With
bromine however the reaction is one of bromine with
the indicator molecule oxidising it to a colourless
3. % OR compound. This is no longer a reversible reaction.

4. % Dev BT
Miscellaneous Assay of
Iodine Topical Solution for
Sodium Iodide Content
Molecular Formula: NaI
Molecular Weight: 149.89
g/mol
Indicator Used: Amaranth
TS
Color
Transition/Endpoint: pale
brown to red to yellow
Official Requirement:
NLT 2.1g and NMT 2.6g in
each 100 mL
Analysts:
Casil
Gonzales
Mardo
Pajares
Sol
Type of Titration: Chemical Equations: Assay Procedure
Direct titration KIO3 + 2NaI + 6HCl → 3ICl + KCl +2NaCl + 3H2O Transfer 10 mL of the sample into a glass-
Type of Half - Reaction: stoppered 500-mL flask, add 30 mL of water and 50
Reaction: Redox Oxidizing agent: mL of hydrochloric acid, cool to room temperature,
reaction 4e- + 6H + IO3 → I+ + 3H2O and titrate with 0.05 M potassium iodate VS until
OA: Iodide NaI+ the dark brown solution that is produced becomes
RA: potassium Reducing agent: pale brown. Add 1 mL of amaranth TS, and
iodate 2I- > I2 + 2e continue the titration slowly until the red color just
OA: I changes to yellow. The difference in volume, in
Titrant: 0.05 M RA: IO3 milliliters, between the titrant used and half the
potassium iodate Factor: 4 volume of 0.1 N sodium thiosulfate VS used in the
VS Explanation: assay for iodine, multiplied by 14.99, represents the
Special Pre- Lab Computations: number of milligrams of sodium iodide in the portion
Conditions: General Formula using Molar Ration of topical solution taken.
 The Reason/s For Important Steps:
analyte 1. A glass-stoppered flask is used to prevent
should be the vapors of iodine from escaping from the
put in a flask.
500-mL = 0.44967 g 2. Iodine undergo photodecomposition when
glass- Post - lab computations: exposed to light from longer period of time.
stoppered Cover the flask to avoid iodine degradation.
flask 3. A high amount of hydrochloric acid is used
 Addition of for IO3 to be reduced to I+ to form ICl.
HCl 4. Amaranth TS is the indicator used in this
assay. Starch TS is not used because it
decomposes at an acidic medium.
5. At the endpoint is being reached,there is
aneed for rigorous shaking due to the

Diazotization Titration (or
Nitrite Titration) of
Sulfamethazine
Molecular Formula:
C12H14N4O2S
Molecular Weight: 278.33
g/mol
Indicator Used: Starch-
iodide paper
Color
Transition/Endpoint: format
ion of immediate blue
different heterogeneous phases of iodine
and iodate
Type of Titration: Chemical Equations: Assay Procedure
Direct titration Accurately weigh about 500 mg in the case of
Type of sulfonamide, or otherwise the quantity specified in
Reaction: Redox the individual monograph, and transfer to a suitable
reaction open vessel. Add 20 mL of hydrochloric acid and
OA: 50 mL of water, stir until dissolved, cool to about
Sulfamethazine 15°C, and slowly titrate with 0.1 M sodium nitrite VS
RA: sodium that previously has been standardized against USP
nitrite sulfanilamide RS. Place the buret tip below the
surface of the solution to eliminate air oxidation of
Titrant: 0.1 M the sodium nitrite and stir the solution gently,
sodium nitrite VS maintaining the temperature at about 15°C.
Special Titrate until the glass rod dipped into the titrated
Conditions: Soluti solution produces an immediate blue ring when
on must be kept at touched to a starch-iodide paper.
15°C to form Each mL of 0.1 M sodium nitrite is equivalent to
stable diazo 27.83 mg of C12H14N4O2S (sulfamethazine).
compounds. Reason/s For Important Steps:
1. Hydrochloric acid is added to form nitrous
acid with sodium nitrite. An acidic
environment is needed to form nitrous acid.
2. The tip of buret is immersed in the solution to
prevent volatilization of nitrous acid.
3. Optimum temperature is 10-15°C for most
amines to form relatively stable diazo
compounds.
Half - Reaction:
OA: Sulfamethazine
RA: sodium nitrite
Factor: 1
Explanation:
ring/color on starch-iodide
paper
Official Requirement:
Not less than 99.0% and not
more than 100.5% of
Sulfamethazine calculated on
dried basis.
Analysts:
Ham, Jadden
Mardo, Jemimah
Ortiz, April
Robles, Elijah
Velasco, Alleli
Analyte: Cupric Sulfate
Molecular Formula: CuSO4
Molecular
Weight: 169.6016 g/mol
Indicator Used: Starch TS
Color
Transition/Endpoint: Disch
arge of the dark blue/black
color from the solution.
Official Requirement:
Cupric sulfate is anhydrous or
contains five molecules of
water of hydration. It contains
not less than 98.5% and not
more than 100.5% of cupric
sulfate (CuSO4), calculated on
the dried basis.
Analysts:
Tan, Hugh Jasper
Mojica, Maria Madel
Pre- Lab Computations:
0.1N x 30mL x 278.33 g/mol
1000 x 1F
Wt substance = 0.83499 wt of sulfamethazine
Post - lab computations:
N/A (due to committed errors)
Type of Chemical Equations: Assay Procedure
Titration: Iodome Reaction Between Cupric Sulfate and Potassium Iodide Sample Solution: Place 650 mg of Cupric Sulfate in
try 2CuSO4 + 4KI → 2CuI + I2 + K2SO4 a weighed container fitted with a ground-glass
Direct titration with Half - Reactions stopper. Dry, allow to cool in a desiccator, and
blank e+ + Cu2+ → Cu+ weigh again to obtain the weight of the sample.
determination. 2I- → I2 + 2e- Dissolve in 50mL of water. Add 4 mL of 6N acetic
Type of OA: Cupric Sulfate acid and 3 g of potassium iodide.
Reaction: Redox RA: Potassium Iodide
reaction Factor: 1
Reaction Titrimetric System
Explanation: The factor is 1 since copper (II) gains 1 electron and is
Between Analyte Mode: Direct Titration
reduced to copper (I).
and Potassium Reaction Between Liberated Iodine and Sodium Thiosulfate Titrant: 0.1 N sodium thiosulfate VS
Endpoint detection: Visual
Iodide
OA: Cupric
Sulfate Analysis: Titrate the liberated iodine in theSample
RA: Potassium solution with the Titrant, adding about 2g of
Iodide potassium thiocyanate and 3 mL of starch TS as the
Reaction Half Reactions
endpoint is approached. Perform a blank
Between 2S2O32- → S4O62- +2e-
determination, and make any necessary correction.
Liberated Iodine 2e- + I2 → 2I-
and Titrant OA: Iodine
Each mL of 0.1N sodium thiosulfate is equivalent to
OA: Iodine RA: Sodium Thiosulfate 15.96 mg of cupric sulfate (CuSO4).
Pausal, Nicole RA: Sodium Factor: 2
Cas, Angelica Thiosulfate Explanation: The factor is 1 since 1 electron was lost by 1 mole of Acceptance criteria: 98.5%-100.5% on the dried
Encabo, Jewel thiosulfate ion. basis.
Macabanti, Heena Titrant/s: 0.1 N Pre- Lab Computations: Reason/s For Important Steps:
Sodium 1. Dry the sample
Thiosulfate VS Cupric sulfate may contain waters of hydration.
Special
According to United States Pharmacopoeial
Conditions: The
Convention, Inc. (2017), acceptance criteria for the
special conditions Wt CuSO4 = 0.4788 g sample will be based on the dried basis. This aids to
involved in the Post - lab computations:
correct for the waters of hydration it contains.
assay is the drying 1. % Purity
2. Add 6N acetic acid.
of the cupric
According to Knevel, & DiGangi (1977), in alkaline
sulfate before use,
solutions, reactions of iodine with OH- produces
performing the
first hypoiodite and finally iodate ions. These ions
titration in acidic
oxidize thiosulfate, at least partially, to a higher
environment, and
oxidation state, which is undesired since the
adding potassium
stoichiometry of the reaction no longer holds true
thiocyanate and
when this happens. Also according to Christian,
starch indicator TS
Dasgupta, & Schug (2014), the reason for using
near the end of
acid solution is that the reactions between many
titration, and
oxidizing agents and iodide are promoted by high
performing a
acidity.
blank
determination.
3. Add 2g of potassium thiocyanate
According to Foote, & Vance (1935, 1936), a
modification involving the addition of soluble
thiocyanates added just before the endpoint is
reached, aids in the liberation of more iodine in the
reaction. This is because iodine tends to adsorb
strongly on the solid cuprous iodide precipitate. The
2. % PAverage potassium thiocyanate is added to displace the
adsorbed iodine, leading to the precipitation of the
more insoluble cuprous thiocyanate instead of

3. % Deviation from OR
4. % Deviation between Trials
cuprous iodide. This makes the iodine more
accessible to the starch collodial particles, hence
yielding a sharper endpoint. This reason was also
mentioned by Christian, Dasgupta, & Schug (2014).
4. Prepare fresh starch TS.
According to Knevel, & DiGangi (1977), starch
solutions deteriorate rapidly, which is why they
should be prepared freshly every day when needed.
5. Add the starch TS as the endpoint is
approached.
According to Knevel, & DiGangi (1977), the
reversibility of color formation is decreased when
the iodine concentration is high, which will make it
difficult to determine the true endpoint. This is why
the starch is added after most of the iodine has been
reduced.

6. Perform a blank determination.

According to Knevel, & DiGangi (1977), a blank
determination is run if there is reason to believe that
the reagents if the official procedure or the
conditions under which the analysis is performed
may interfere or compete with the titrant or
complement the titrant. The blank determination is
performed in this procedure to determine if the
other materials present in the sample solution
(potassium iodide), affect the determination of the
endpoint.

Analyte: Liquefied Phenol Type of Titration: Chemical Equations: ASSAY PROCEDURE

Residual [1] HCl is added, bromine is set free. Sample solution: Place 2g of Liquefied Phenol in a
Molecular Formula: Iodometry with 5KBr + KBrO3 + 6HCl -> 6KCl + 3Br2 + 3H2O 1000 ml volumetric flask and dilute with water to
Half rxn: volume.

Molecular Weight: 94.11
g/mol
Indicator Used: Starch TS
Color Transition/Endpoint:
Red wine colored solution to
faint blue
Official Requirement:
Liquefied Phenol is phenol
maintained in a liquid
condition by the presence of
about 10% of water. It
contains NLT 89.0% by weight
of C6H6O.
Blank (2Br- -> Br2 + 2e-) 5 (Oxidation) Analysis: Pipet 20-ml of the sample solution into an
determination (10e- + 12H+ + 2BrO3- -> Br2 + 6H2O) (Reduction) iodine flask, [1] add 30.0ml of 0.1N Bromine VS,
Type of -------------------------------------------------------- then add 5ml of hydrochloric acid, and [2]
Reaction: Redox 10Br- -> 5Br2 + 10e- immediately insert the stopper. Shake the flask
reaction 10e- + 12H+ + 2BrO3- -> Br2 + 6H2O repeatedly during 30 minutes, [3] allow it to stand
Reaction -------------------------------------------------------- for 15 minutes, [4] add quickly 5ml of potassium
Between 10Br- + 12H+ + 2BrO3- -> 6Br2 + 6H2O iodide solution (1 in 5), taking precautions against
Liberated Iodine Simplified: the escape of bromine vapor, and at once insert the
and Titrant 5Br- + 6H+ + BrO3- -> 3Br2 + 3H2O stopper in the flask. Shake thoroughly, remove the
OA: Iodine 2] bromine reacts with phenol stopper, and rinse it and the neck of the flask with a
RA: Sodium small quantity of water so that the washings flows
Thiosulfate into the flask. [5] Add 1 mL of chloroform, and
shake the mixture.
Titrant/s: 0.1 N Titrate the liberated Iodine with [6] 0.1N sodium
Sodium thiosulfate VS, adding 3ml of Starch TS as the
Thiosulfate VS endpoint is approached. Perform a blank
Excess: 0.1N determination. Each mL of 0.1N Bromine is
Bromine VS equivalent to 1.569mg of C6H6O.
[3] Excess bromine liberates I2 [1] The bromine reacts with phenol to form a white
crystalline precipitate of tribromophenol and
hydrobromic acid.
[2] The flask should be tightly stoppered to prevent
[4[ Liberated iodine reacts with sodium thiosulfate the escape of the volatile bromine and it is shaken
gently for 30 minutes to allow the oxidation of
phenol to tribromophenol to go to completion.
[3] allowing the flask to stand for 15 minutes to
fasten the reaction.
[4]
Potassium iodide will react with excess bromine
that will liberate iodine, the free iodine then reacts
FACTOR IS 6 with 0.1N Sodium thiosulfate VS.[5] This is to
dissolve the precipitated tribromophenol which
would interfere with the clear observation of
endpoint.
PRE LAB COMPUTATION: [6] not used as a primary standard, its solution is
unstable, decomposed by CO2 and certain type of
 Wt. analyte = N Standard x (Vexcess - α) bacteria.
x

Wt. analyte = 0.1N Standard x (30 mL - 10 mL)

x

The quantity of 12 formed is determined by titration with thiosulfate.

= 0.03137 g, phenol

=
X = 1.5685 g of Liquified Phenol

LEAD MONOXIDE Type of Chemical Equations: Assay Procedure

Titration: Indirect Reaction of potassium dichromate to potassium iodide: Accurately weigh about 300 mg, freshly ignited in
Molecular Formula: PbO Titration K2Cr2O7 + 7H2SO4 + 6KI → 3I2 + Cr2(SO4)3 + 4K2SO4 + 7H2O muffle furnace at 300 ± 50°: and dissolve it by
Molecular Weight: 223.2 Type of Reaction of potassium iodide to sodium thiosulfate: warming with 10 mL of water and 1 mL of glacial
g/mol Reaction: Oxidation- 2Na2S2O3 + I2 → 2NaI + Na2S4O6 acetic acid. Dilute with 75 mL water, heat to boiling,
Titrant: 0.1 N Sodium Reduction Reaction Half - Reaction: add 50.0 mL of 0.1 Potassium Dichromate VS, and
Thiosulfate OA: Cr2O72- Reaction of potassium dichromate to potassium iodide: boil for 2-3 minutes. Cool, transfer to a 200 mL
Indicator Used: Starch TS RA: I- Cr2O72- + 14H + 6e- → 2Cr3+ + 7H2O volumetric flask with the aid of water, dilute with
Color (2I- → I2 + 2e-) 3 water to volume, mix, and allow to settle. Withdraw
Transition/Endpoint: Blue Special Conditions: 100 L of the clear liquid and transfer to a glass
to colorless Igniting Lead stoppered flask. Add 10 mL of sulfuric acid and 1g of
Official Requirement: Monoxide in a muffle OA: Cr2O72- potassium iodide, insert the stopper, miz gently and
NLT 98% Lead Monoxide is furnace. RA: I- allow to stand for 10 minutes. Then titrate the
found. Factor: 3 liberated iodine, representing the excess of
Analysts: Explanation: F=3 because kailangan ng 3 moles ng Iodine para dichromate, with 0.1 N sodium thiosulfate VS, adding
Casil, Debbie equivalent sila ng dichromate; para mag proceed ang reactiona 3 mL of starch TS as the endpoint is approached.
Figueroa, Jasmin Maciel Pre- Lab Computations: Reason/s For Important Steps:
Magaling, Monica Mae M. -Boiling/heating expels carbon dioxide whis is present
Nacar, Krysca Cae N. in carbonic acid, may act like any other causing
Pereyra, Laica Marie R.
Urgena, Nhia hydrolysis and decomposition of sodium thiosulfate.
(Knevel & Digangi,1997)
wt = 0.2232 g -Standing the solution for 10 minutes prevents
Post - lab computations: turbidity.
-Lead Monoxide is converted to lead acetate which
reacts with potassium dichromate in the presence of
acetic acid.
-Potassium dichromate oxidises the iodide ion in the
presence of acid to an equivalent volume of iodine.
-Potassium iodide is used to react with lead chromate
because it is an alkali metal that makes lead chromate
soluble. It also enhances the sensitivity of the
indicator.
-Interaction of the iodide and iodine ion with the
colloidal B-amylose results in the production of an
intensely blue colored solution, and this color change
is reversible, the color being discharged when the
iodine is reduced with sodium thiosulfate or another
reducing agent.
-The reversibility of color transformed is decreased
when the iodine concentration is high.
- For the use of indirect methods, the indicator
therefore is added at a point when virtually all the
iodine has been reduced to iodide ion, causing the
disappearance of color to be more rapid and sudden.
A diffuse end-point would result from slow
dissociation of the starch-iodo complex if a large
amount of iodine were absorbed by the starch.
Proper Disposal and Precautions
Lead Monoxide
 Do not breathe dust, fume, gas. Wash face,
hands and any exposure thoroughly after
handling. Dispose of contents/container to an
approved waste disposal.
Potassium Dichromate
  Keep away from heat. Avoid contact with skin
and eyes. Keep away from incompatibles such
as reducing agents, combustible materials,
organic materials. Dispose in hazardous waste
container.
Sodium Thiosulfate
 Do not breathe dust. Keep away from
incompatibles such as oxidizing agents, acids,
alkalis. Dispose of contents to an approved
waste disposal.