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EXPERIMENT 12:
Preparation and Standardization of
Potassium Permanganate Solution
EXPERIMENT 12:
A. Preparation of Potassium Permanganate
Solution/ Class
EXPERIMENT 12:
LECTURE NOTES:
Asbestos- carcinogenic
for filtration of inorganic matter
should be lined with a glass wool as support
(funnel) when used as a filter.
Should be washed with distilled water until water
coming out of the funnel is clear before KMnO 4 is
filtered.
EXPERIMENT 12:
B. Standardization of Potassium Permanganate
Solution
1. Weigh 0.1-0.2g of Na2C2O4 (weighing bottle)
2. Dissolve it in 250 mL distilled water in a big
beaker.
3. Add 7mL of conc. sulfuric acid
4. Heat the solution to 70C (maintain ---reaction between
sodium oxalate and KMnO4 occurs stoichiometrically in a hot acidic
medium)
EXPERIMENT 12:
LECTURE NOTES
Standardization: primary standardization
Type of Titration: Redox
Method of Titration: Direct Permanganate method
1. Na2C2O4 - primary standard, reducing agent
EXPERIMENT 12:
Lecture Notes
3. H2SO4 -to keep the acid conc. constant
preventing the formation of MnO2
- supply hydrogen ion
4. Hot acidic medium- the reaction between
Na2C2O4 and KMnO4 stoichoimetrically occur
in a hot acidic medium.
EXPERIMENT 12:
LECTURE NOTES
5. Equation:
Molecular
lost=1eX
2= 2e x5= 10e
+3 +4
gained=5e x 2 = 10e
C2O4 -2
MnO41.
2.
3.
CO2
Mn+2
EXPERIMENT 12:
LECTURE NOTES
6. Computation: Normality
meq KMnO4
= meq Na2C2O4
(NxmL) KMnO4 = (g /MEW) Na2C2O4
N KMnO4 = g Na C O
2
MW
h X 1000
mL
KMnO4
NOTE:
EXPERIMENT 12:
LECTURE NOTES
6. Computation: Molarity
mn KMnO4
(MxmL) KMnO
=
4
mn Na2C2O4 x rr
(mg /MW) Na C O
2
X 2KMnO4
5Na2C2O4
M KMnO4 = mg/MW Na C O
2
X 2KMnO4
5Na2C2O4
mL
KMnO4
EXPERIMENT 13:
Preparation and Standardization of
Oxalic acid Solution
EXPERIMENT 13:
A. Preparation of Oxalic Acid Solution/ ClassGroup 5
EXPERIMENT 13:
B. Standardization of Oxalic Acid Solution
1. Run down 30 mL of oxalic acid (Mohr) into a big
beaker (Mohr : IR, FR)
2. Dilute with 200 mL distilled
3. Add 7mL of conc. sulfuric acid
4. Heat the solution to 70C (maintain---reaction between
oxalic acid and KMnO4 occurs stoichiometrically in a hot acidic medium)
EXPERIMENT 13:
LECTURE NOTES
Standardization: Secondary standardization
Type of Titration: Redox
Method of Titration: Direct Permanganate method
1. KMnO4 secondary standard
-strong oxidizing agent
-reacts rapidly with reducing substance (oxalic acid) in
hot acidic medium
- serves as indicator itself due to its intense
color imparting a pink coloration
-disadvantage: unstable
EXPERIMENT 13:
LECTURE NOTES
2. Equation:
Molecular
10e
+2
C2O4 -2
MnO41.
2.
3.
CO2
Mn+2
EXPERIMENT 13:
LECTURE NOTES
3. Computation: Normality
meq H2C2O4
= meq KMnO4
(NxmL) H2C2O4
(NxmL) KMnO4
N H C O = N x mL KMnO4
mL H C O
2
EXPERIMENT 13:
LECTURE NOTES
3. Computation: Molarity
mn H2C2O4
(MxmL)H C O
2
mn KMnO4 x rr
(MxmL) KMnO
2KMnO4
M H C O = MxmL KMnO
2
2KMnO4
mL H C O
2
X 5H2C2O4
X 5H2C2O4
EXPERIMENT 14:
Assay of Sodium Nitrite
EXPERIMENT 14:
Assay of Sodium Nitrite
1. Weigh 0.4 to 0.5g NaNO2 accurately
2. Dissolve it in enough distilled water to make
100mL in a volumetric flask
3. Pipet 10 mL NaNO2 solution (wash pipet first)
4. Introduce it into a beaker containing a mixture of:
25 mL KMnO4 (Geissler buret: IR, FR)
100 mL distilled water
5 mL conc. H2SO4
EXPERIMENT 14:
Assay of Sodium Nitrite
5. Warm the liquid to 40C and allow it to stand for
5 minutes. (to accelerate the oxidation of HNO to HNO )
6. Add 25 mL of standard oxalic acid solution (Mohr: IR,
2
FR)- (KMnO4 is decolorized because the oxalic acid was added in excess)
7. Heat to 80C
8. Titrate with standard KMnO4 to a light pink end
point ( Geissler: IR,FR)
9. One determination /pair
10. Look for USP specifications for NaNO2
11. Compute Mean % purity as a class
12.Disposition
EXPERIMENT 14:
LECTURE NOTES
Assay of Sodium Nitrite
Type of Titration: Redox
Method of Titration: Residual Permanganate method
1. NaNO2- reducing agent
2. KMnO4 oxidizing agent
Note : Ferrous, Calcium, Lead (II) and titanium compounds are also
assayed by permanganate method
EXPERIMENT 14:
LECTURE NOTES
2. Equation:
Molecular
2NaNO2 + H2SO4
2HNO2 + Na2SO4
+3
5HNO2 +2KMnO4+ 3H2SO4
+7
+5
5HNO3+ 2MnSO4+ K2SO4+ 3H2O
+2
gained= 5e X2=10e
+3
+4
2KMnO4 + 5H2C2O4 + 3H2SO4
2MnSO4 + 10CO2 + K2SO4 + 8H2O
+7
gained = 5ex2=
10e
+2
EXPERIMENT 14:
LECTURE NOTES
2. Equation:
Half ionic equation
NO2MnO4-
C2O4 -2
MnO4-
NO3Mn+2
CO2
Mn+2
EXPERIMENT 14:
LECTURE NOTES
3. Computation: Normality
meq NaNO2 = meq KMnO4 that reacts with NaNO2
gpure NaNO2= [(NxmL) Total KMnO - (N x 25mL) H C O ]
4
MW
hx1000
x MW
h x 1000
X 100
_______
EXPERIMENT 14:
LECTURE NOTES
3. Computation: Molarity
mn NaNO2 = mn KMnO4 that reacts with NaNO2 x rr
gNaNO2= [(MxmL) Total KMnO4 - (M x 25mL) H2C2O4 X KMnO4 ]
X HNO2
H2 C2 O 4
X 100
X 2 KMnO4
]x5
KMnO4
HNO2
NaNO2 X
MW
HNO2
1000
2NaNO2 x
MW
EXPERIMENT 15:
Preparation and Standardization of
Sodium thiosulfate Solution
EXPERIMENT 15:
LECTURE NOTES
Experiment 15-18:
Type of Titration: Redox
Method: Iodimetry/ Iodometry
1.
EXPERIMENT 15:
LECTURE NOTES
2. Iodometry- is a process where in the sample of an oxidizing agent is
made to liberate an equivalent amount of iodine from KI which is
titrated with Na2S2O3 solution.
Pharmaceutical solutions assayed Iodometrically:
1. Iron
6. arsenous
2. Copper
7. chlorine
3. Manganese 8. Bromine
4. Chromium
9. Iodine
5. Cobalt
EXPERIMENT 15:
A. Preparation of Starch Solution
1. Triturate 1g of arrowroot starch with 10 mL of
distilled water. (starch paste)
2. Boil 200 mL of distilled water
3. Add the starch paste to it with constant stirring
4. Boil the mixture gently until it forms a thin,
translucent liquid.
EXPERIMENT 15:
LECTURE NOTES
Starch test solution- serves a indicator
Starch grains contain:
1. - amylose (water insoluble)- with Iodine forms a
violet color
2. -amylose (water soluble)- with Iodine forms
blue color
EXPERIMENT 15:
LECTURE NOTES
1. Larger grains- arrow root and potatoes( will give
more - amylose)
2. Smaller grains- rice and corn ( will give lesser amylose)
EXPERIMENT 15:
B. Preparation of Sodium Thiosulfate Solution/
Class
EXPERIMENT 15:
C. Standardization of Sodium Thiosulfate Solution
EXPERIMENT 15:
C. Standardization of Sodium Thiosulfate Solution
EXPERIMENT 15:
C. Standardization of Sodium Thiosulfate Solution
EXPERIMENT 15:
LECTURE NOTES
Standardization: primary standardization
Type of Titration: Redox
Method of Titration: Iodometry
1. KIO3- primary standard (oxidizing agent)
2. Na2S2O3 titrant; reducing agent
EXPERIMENT 15:
LECTURE NOTES
3. Equations:
Molecular:
+5
gained=5eX2= 10e
2KIO3+ 10 KI + 12HCl
-1
lost= 1 x2=2eX 5= 5e
0
lost= 1 x 2=2e X5= 10e
EXPERIMENT 15:
LECTURE NOTES
3. Equations:
Molecular:
+5
gained=5eX2= 10e
KIO3+ 5 KI + 6HCl
-1
lost= 1 x2=2eX 5= 5e
gained = 1x2=2e X 1= 2e
-1
+2.5
EXPERIMENT 15:
LECTURE NOTES
3. Equations:
Half- ionic equation:
IO3- I2
I I2
S2O3-2
I2
S4O6-2
I-
EXPERIMENT 15:
LECTURE NOTES
3. Equations:
Half- ionic equation:
S4O6-2 + 2I-
EXPERIMENT 15:
LECTURE NOTES
4. Computation: Normality
meq Na2S2O3
= meq KIO3
(NxmL) Na2S2O3 = (g /MEW) KIO3
N Na S O = g KIO
2
MW
h X 1000
mL Na S O
2
Note: g= 1.1g
= x
500 mL
50mL
h=6
EXPERIMENT 15:
LECTURE NOTES
4. Computation: Molarity
mn Na S O
2
(MxmL) Na S O
2
M Na S O
2
mn KIO3 x rr
=
mg KIO3
MW
mg KIO3 X
MW___ 1 KIO3
mL Na2S2O3
3 I2
1 KIO3
2Na2S2O3
1 I2
3 I2______ x 2Na2S2O3
1 I2
EXPERIMENT 16:
Preparation and Standardization of
Iodine Solution
EXPERIMENT 15:
A. Preparation of Iodine Solution/Class
1. Weigh roughly 14.0g of Iodine crystals
2. Dissolve it in a solution of 36 g KI in 400 mL of
distilled water. (KI is a solubilizing agent to increase the solubility of
Iodine crystals)
EXPERIMENT 16:
B. Standardization of Iodine Solution
1.
2.
3.
4.
EXPERIMENT 16:
LECTURE NOTES
Standardization: secondary standardization
Type of Titration: Redox
Method of Titration: Iodimetry
1. Na2S2O3 solution - secondary standard; reducing
agent
2. Iodine titrant; oxidizing agent
EXPERIMENT 16:
LECTURE NOTES
3. Equations:
Molecular:
+2
lost=0.5 x2= 1e x 2= 2e
2Na2S2O3+ I2
0
+ 2.5
2NaI+ Na2S4O6
-1
EXPERIMENT 16:
LECTURE NOTES
3. Equations:
Half ionic :
S2O3-2
I2
2S2O3-2 + I2
S4O6-2
I-1
S4O6-2 + 2I-
EXPERIMENT 16:
LECTURE NOTES
4. Computation: Normality
meq I2 = meq Na2S2O3
(NxmL) I2 = (NxmL) Na2S2O3
N I = N x mL Na S O
mL I
2
EXPERIMENT 16:
LECTURE NOTES
4. Computation: Molarity
mn I2 =
mn Na2S2O3 x rr
(MxmL)
I2 =
(MxmL) Na S O
2
Na2S2O3
M I2 = MxmL Na S O
2
mL I
X 1 I2 ___
2 Na2S2O3
X 1 I2 ___
EXPERIMENT 17:
Assay of Tartar Emetic
EXPERIMENT 17:
Assay of Tartar Emetic
1. Weigh 0.4 to 0.5g tartar emetic accurately (tared flask)
2. Dissolve it in 30 mL distilled water
3. Add 25 mL of saturated solution of sodium bicarbonate
(neutralize the HI formed thus preventing a reversible reaction and allowing the reaction
to proceed to completion)
EXPERIMENT 17:
LECTURE NOTES
1. Tartar Emetic (KOSbC4H4O6. H2O)
double salt
Reducing agent
2. Method of Titration: Direct Iodimetric method
3. Equation:
Molecular
+3
lost= 2e-
KOSbC4H4O6 + I2 + 2NaHCO3
0 gained= 1x2= 2e
+5
EXPERIMENT 17:
LECTURE NOTES
3. Equation:
Half ionic
Sb +3
Sb +5
I2
I-1
EXPERIMENT 17:
LECTURE NOTES
4. Computation: Normality
meq KOSbC4H4O6. H2O =
(g /MEW) KOSbC H O
4
6.
H 2O =
meq I2
(NxmL) I
h X 1000
x 100
EXPERIMENT 17:
LECTURE NOTES
4. Computation: Molarity
mn KOSbC4H4O6. H2O =
g pure
MW
KOSbC4H4O6. H2O =
mn I2 x rr
(MxmL) I
x 1 KOSbC4H4O6. H2O
1 I2
1000
gpure KOSbC H O
4
6.
H2O =
1 I2
(MxmL) I x
2
1 KOSbC4H4O6. H2O
X MW
1000
X 100
EXPERIMENT 18:
Assay of Cupric Sulfate
EXPERIMENT 18:
Assay of Cupric Sulfate
1. Weigh 0.4 to 0.5g cupric sulfate accurately (tared
iodine flask)
2. Dissolve it in 50 mL distilled water
3. Add 4 mL of 6 N acetic acid
4. Add 3 g of KI (Note the color change after adding: reddish brown color
indicates plenty of I2 is liberated)
EXPERIMENT 18:
Assay of Cupric Sulfate
7. Continue the titration with std. sodium thiosulfate
solution until the disappearance of blue color. (FR)
8. One determination per pair
9. Compute for the % purity of cupric sulfate as a
class.
10. Look for USP/NF specs
11. Disposition
EXPERIMENT 18:
LECTURE NOTES
Assay of Cupric sulfate
1. CuSO4.5H2O (oxidizing agent)
blue vitriol
2. KI (reducing agent)
3. Type of Titration: Redox
4. Method of Titration: Iodometry
EXPERIMENT 18:
LECTURE NOTES
5. Equations:
Molecular
+2
gained= 1e X2 =2e
2CuSO4.5H2O +4KI
+1
I2 + 2Na2S2O3
2NaI + Na2S4O6
EXPERIMENT 18:
LECTURE NOTES
5. Equation:
Half ionic
Cu +2
Cu +1
I2
I-1
EXPERIMENT 18:
LECTURE NOTES
4. Computation: Normality
meq CuSO4O6. 5 H2O =
(g /MEW) CuSO
g
4.
5H2O =
meq Na2S2O3
(NxmL) Na S O
2
h X1000
x 100
EXPERIMENT 18:
LECTURE NOTES
4. Computation: Molarity
mn CuSO4. 5H2O =
g pure
CuSO4. 5H2O =
mn Na2S2O3 x rr
(MxmL) Na S O
2
2 Na2S2O3
MW
x 1 I2 __________
2 CuSO4. 5H2O
1 I2
1000
gpure CuSO
4.
2 Na2S2O3
1 I2
1000
X 100
EXPERIMENT 19:
ASSAY OF ASCORBIC ACID
EXPERIMENT 19:
A. Preparation of Standard Potassium
Bromate/Class- Group 8
EXPERIMENT 19:
Assay of Ascorbic Acid
1. Weigh accurately 3 to 5 vitamins
2. Pulverize them thoroughly in a mortar, and
transfer the powder to a dry weighing bottle.
3. Weigh accurately 0.4 to 0.5 g sample into a dry
250 mL conical flask (with cover)
4. Dissolve the sample in 50mL of 1.5 M H2SO4 (freshly
prepared; converts BrO to Br ); then add about 5g of KBr.
( will produce excess Br2)
5. Titrate immediately with standard KBrO3 to the
first faint yellow due to excess Br2 (Geissler: IR, FR)
3
EXPERIMENT 19:
Assay of Ascorbic Acid
6. Record the volume of KBrO3 used.
7. Add 3g of KI and 5mL of starch indicator; back titrate
with standard Na2S2O3 to the disappearance of blue
color. (titration should be done without delay to prevent the air oxidation of
ascorbic acid)
EXPERIMENT 19:
LECTURE NOTES:
Assay of Ascorbic Acid
1.Type of Titration: Redox
2. Method: Bromination
Applicable for chewable vitamin C (not coated tablets)
The binder in most Vitamin C tablets remains in the suspension
through out the analysis. If the binder is starch, the characteristic
color of the complex with I2 appears upon the addition of KI
The volume of Na2S2O3 needed for the back titration seldom
exceeds a few millimeters.
EXPERIMENT 19:
LECTURE NOTES
3. Equation:
BrO3 + 5Br- + 6H+ 3Br2 + 3H2O
4.
+ Br2
Ascorbic acid (C6H8O6)
+ 2 Br- + 2H+
Br2 + 2 I- Br- + I2
I2 + 2 S2O3-2 2 I- + S4O6-2
EXPERIMENT 19:
LECTURE NOTES
4. Computation: Normality
meq AA
gpure AA
MW
hx1000
g pure
AA=
EXPERIMENT 19:
LECTURE NOTES
Computation: Normality KBrO3
NKBrO = 2.6g KBrO
3
MW
h X 1000
1000 mL
Note: h=6
Equation:
BrO3 Br2
EXPERIMENT 19:
LECTURE NOTES
4. Computation: Molarity
mn AA
gpure AA
MW
2Na2S2O3
1I2
1000
g pure
AA=
1 I2
1000
EXPERIMENT 19:
LECTURE NOTES
Computation: Molarity KBrO3
MKBrO = 2.6g KBrO
3
MW
1000
1L