QC 1 Assay Manual

Drug Testing and Assay Manual
TABLE OF CONTENTS
Introduction Remarks & General Laboratory Directions
Experiment Title
1 Weight Variation Test
2 Determination of Content Uniformity
3 Preparation & Standardization of HCl Solution
4 Preparation & Standardization of NaOH
5 Assay of Acetic Acid
6 Assay of milk magnesia
7 Assay of Aspirin
8 Preparations and Standardizations of AgNO3
9 Preparation and Standardization of NH 4SCN
10 Determination of Chloride by the Volhard Method
11 Assay for Iodine Content in Povidine Iodine
12 Preparation and Standardization of EDTA Solution
13 Assay of Calcium Lactate Estornino’s group
14 Preparation & Standardization of KMnO4 Ayon’s group
15 Assay of Hydrogen Peroxide Solution Plaza’s group
16 Preparation and Standardization of H2C2O4 Solution (Oxalic acid) Bedayo’s group
17 Assay of Sodium Nitrite Amon’s group
18 Preparation and Standardization of Iodine Solution Piao’s group
19 Preparation and Standardization of Na2S2O3 Laure’s group
20 Assay of Antimony Potassium Tartrate Joe’s group
21 Assay of Cupric Sulfate Agno’s group
22 The Gravimetric Determination of Soluble Chlorides

College of Health Sciences
1
NOTRE DAME OF DADIANGAS UNIVERSITY
REMARKS AND GENERAL LABORATORY DIRECTIONS
OBJECTIVES OF QUANTITATIVE PHARMACEUTICAL CHEMISTRY LABORATORY
1. The acquisition of a fundamental knowledge of the theory as well as a practical

ability in the application of analytical methods.
2. The development of manipulative skills in the laboratory, with the ability to follow
directions under the supervision of a skilled analyst.
3. A basic knowledge of the reactions taking place during an analysis and the ability to
apply the theory upon which the method is dependent.
4. Aside from the skill of technique, student is expected to develop patience, neatness
and accuracy at all times.
5. Use common sense and think throughout each step af an analytical procedure.
6. perform all qualitative work without even a slight loss of material or gain of
extraneous matter, and to regard every particle of sample, solution or precipitate as
indispensable to the ultimate success of the analysis.
7. Be safety-conscious in every step of the analysis.
8. Above all, absolute integrity is demanded of every quantitative analyst. The operator
is the only person who is familiar with the entire history of an analysis and who
knows whether it is worthy of full confidence.
THE LABORATORY NOTEBOOK
Aside from this laboratory manual, students are required to have a data notebook
(to be designated by the instructor). A few widely used rules are listed below:
1. Use a bound notebook (a small bound notebook for each group).

2. Number all pages consecutively.
3. Enter all data directly into the notebook in ink.
4. Delete unused or incorrect data by drawing a single line through it. Don not erase,
obliterate, or remove data from the notebook. Occasionally, such data become
important at a later date.
5. Write balanced equations for all important reactions that took place.
6. Include one complete example of every calculation made with the data.
7. Date and sign your notebook at the end of each laboratory period (depending on
your assigned task).
ECONOMY OF TIME
Economical utilization of laboratory hours is best achieved through a preliminary

study of the work to be done, followed by a plan for its prompt execution. There is no
2
such thing as “speed” in quantitative work. Economy of time is achieved not by haste,
but by planning the work so that two or more operations may be carried out at one time
and especially by working so accurately that it will be unnecessary to repeat a
determination.
SAFETY IN THE LABORATORY
1. Know the location of all fire extinguishers, showers, and eye wash fountains and
how to use them.
2. Label all chemicals and solutions that are stored outside their original containers.
Include your name and the date of preparation.
3. Tie up long hair (use head cap at all times), especially in the presence of open
flames.
4. Keep work areas clean and uncluttered.
5. Never begin working until your instructor arrives.
6. Never bring food, drinks or smoking materials into the laboratory.
7. Never work without your laboratory gown and never wear open-toed or open-top
shoes.
8. Never heat flammable liquids over an oen flame or outside hood.
PURITY AND STRENGTH REQUIREMENTS
The purity and strength of chemicals and drugs of the U.S.P. and of the N.F are
usually expressed in terms of percent. The official requirements of purity and strength
pertain only when the official methods of assay are employed.
THE ANALYTICAL BALANCE
The introduction of a single-pan substitution type analytical balance has

shortened considerably the time formerly spent on weighingusing the two-pan analytical
balance. The single pan balance maintains a constant weight on the beam at all times,
and the object is weighed by displacing its equivalent weight from the beam. Since the
load on the balance beam is always constant, the substitution weighing eliminates the
need of determining and applying sensitivity corrections to weighing as is the case when
using a two-pan balance.
Rules for the Use and Care of Balance
1. Use the balance assigned by the instructor.

2. Adopt an attitude of personal responsibility for the condition of your balance; the
carelessness of one student may render inaccurate the work of all who use the
same balance.

3
3. Brush the pan and floor of the balance with a camel’s hair brush before starting to
weigh any substance.
4. Test the adjustment of the balance before each weighing. The bubble should be at
the center of the circle (refer to the manual of the balance)
5. Do not attempt to adjust the balance. Call an instructor or a knowledgeable
laboratory assistant if it requires adjustment.
6. NO sample should ever be placed directly upon the balance pan. Solids are best
weighed by using weighing bottle or watch glass, and liquids are weighed by using a
dropper bottle.
7. Hot objects must be allowed to cool to room temperature before they are placed
inside the balance case.
8. Material spilled on the balance pan or floor must be brushed up at once.
9. To avoid damaging the balance, handle every part with care, i.e. open balance case(
doors on either side) slowly and carefully and put the weighing bottles or any
suitable containers slowly on the balance pan.
10. Most importantly, never use any container that may have amost the same weight as
the balance capacity; For example, if the capacity of the balace is onle 120g, do not
use a container that has a weight of 100g or more.

4
Activity
Weight Variation Test
No.1
Brief Description of the Activity
Objectives
Materials Capsules and uncoated tablets of the same lot number 20 each
Forceps to hold the sample
Weighing bottle
Formula
% wt. variation = Actual wt. per capsule x 100
Average weight
% wt.variation =Diff.bet. Actual wt. per tab &ave.wt. x 100

Average Weight
Compounding Procedure
A. Hard capsules
1. Weigh 20 intact capsules individually recording each weight.
2. Add weights of the 20 capsules for each group and find the average weight.
3. From the average weight, determine the percent variation of each of the 20 capsules.
4. The requirements for weight variation are met if each individual weight is within the limit
of 90% and 110% of the average weight.

5
Note: Refer to the USP for the requirements
B. Uncoated tablets
1. Weigh individually 20 whole uncoated tablets.
2. Add all the weights of the 20 tablets and determine the average weight
3. From the average weight, determine the percentage variation of the 20 tablets.
4. The requirements for weight variation are met if the weights of not more than two of the
tablets differ from the average weight by more than double the percentage.
Worksheet
Score
No.1 Weight Variation Test
Student’s Name Course& Year
SME’s Name Date Performed

Class Schedule Group No.
Objective/s:
Data
A. HARD CAPSULES
Weight of the weighing bottle: ________________
Net weight per capsule:

1. __________ 6. ___________ 11. ___________ 16. ___________
2. __________ 7. ___________ 12. ___________ 17. ___________
3. __________ 8. ___________ 13. ___________ 18. ___________
4. __________ 9. ___________ 14. ___________ 19. ___________
5. __________ 10. __________ 15. ___________ 20. ___________
Total weight of the 20 capsules: __________

CALCULATIONS:
Average weight = weight of 20 capsules
20

6
% wt. variation = Actual weight per capsulex 100

Average Weight
Total weight of 20 capsules: _________________
RESULTS:Capsule no.
1. wt.var. = __________ 11. wt.var. = ____________
2. wt.var. = ____________12. wt.var. = ____________
3. wt.var. = ____________ 13. wt.var. = ____________
4. wt.var. = ____________ 14. wt.var. = ____________
5. wt.var. = ____________ 15. wt.var. = ____________
6. wt.var. = ____________ 16. wt.var. = ____________
7. wt.var. = ____________ 17. wt.var. = ____________
8. wt.var. = ____________18. wt.var. = ____________
9. wt.var. = ____________ 19. wt.var. = ____________
10. wt.var. = ____________20. wt.var. = ____________
B. TABLETS
Weight of the weighing bottle: ________________
Net weight per tablet:

1. _____________ 6. _______________11. _______________16. _______________
2. _____________ 7. _______________12. _______________17. _______________
3. _____________ 8. _______________13. _______________18. _______________
4. _____________ 9. _______________14. _______________19. _______________
5. _____________ 10. ______________15. _______________20. _______________
Total weight of the 20 tablets______________
CALCULATIONS:
Average weight = weight of 20 tablets

20
% wt. variations = Diff. bet. Actual wt. per tab &ave. wt. X 100
Average weight
RESULTS:
Tablet No.
1. wt.var. = ____________ 11. wt.var. = ____________
2. wt.var. = ____________12. wt.var. = ____________
3. wt.var. = ____________ 13. wt.var. = ____________
4. wt.var. = ____________ 14. wt.var. = ____________
5. wt.var. = ____________ 15. wt.var. = ____________
6. wt.var. = ____________ 16. wt.var. = ____________
7. wt.var. = ____________ 17. wt.var. = ____________
7
8. wt.var. = ____________ 18. wt.var. = ____________

9. wt.var. = ____________ 19. wt.var. = ____________
10. wt.var. = ___________ 20. wt.var. = ____________
CONCLUSION:
Activity
Determination of Content Uniformity
No.2
Objectives
Materials Sodium bicarbonate tablets 300 mg

Methyl Orange indicator
Mortar and Pestle
Buret
Analytical balance
Formula
NaHCO3/tablet=mLacid xN x meq.wt.
1 tablet
Percent of labeled amount:
Content of NaHCO3/tablet obtainedx 100

Labelled amount
1. Weigh 10 tablets and determine the weight per tablet. Each group will assay a tablet
separately for content uniformity to be done in two trials.
8
2. Powder each tablet finely in a mortar and transferaccurately into an Erlenmeyer flask.
Add 20ml of water to the mortar and dissolve/disperse the remaining particles.
3. Transfer the washing into flask containing the ground tablet. Repeat the washing with
the first portion in the flask and mix well. Add methyl orange TS and titrate with 0.1 N
sulfuric acid until a pinkish red color is produced.
Note: 1. Sodium bicarbonate tablets contain not less than 95% and not more than 105% of the
labeled amount of NaHCO3.
2.Referto the USP for the requirement for the determination of content uniformity.
Worksheet
No.2 Determination of Content Uniformity Score
Student’s Name Course&Yr
SME’s Name Date Performed

Objective/s:
Result:
A. Data
Weight of 10 tablets
Weight per tablet
Volume of H2SO4 USED {ml}
Normality of H2SO4:
B. Calculations:

9
NaCHCO3/ tablet= mL x N x meq. Wt.

1 tab
% labeled amount= content of NAHCO3/ tab obtainedX 100

Labeled amount
C.Conclusion
Preparation and Standardization of NaOH

Solution
Activity
No.3
Objectives
Materials
NaOH pellets (AR grade)

10
Potassium acid phthalate, KHP (AR grade)
Phenolphthalein
Formula
ml NaOH x N = g KHP____
meq. Wt. KHP
N NaOH= g KHP____
meq.Wt. KHP x mlNaOH
Preparation of NaOH Solution
1. Weigh roughly 20 g of NaOH in a previously tared small beaker.

2. Add distilled water to dissolve the NaOH.
3. Pour the NaOH solution into a 1 L volumetric flask.
4. Rinse the beaker with distilled water and pour the rinsing into 1 L volumetric flask.
5. Add enough distilled water to complete the volume to 1 L.
6. Store the solution in a 1 L stock bottle with plastic cap.
7. Label properly.
Standardization of NaOH solution:

11
1. Weigh accurately 1.5 – 2.0 g of KHP (previously dried @ 110°C for 1 hour) into an
Erlenmeyer flask.
2. Dissolve with 50 mL of distilled water by shaking the flask.
3. Add 2 drops of Phenolphthalein indicator.
4. Titrate to a faint pink color using a base buret
5. Perform 2 determinations
6. Determine the normality of NaOH solution.
Worksheet
No.3
Preparation and Standardization of NaOH Solution
Score
Student’s Name
Course&Yr
SME’s Name
Date Performed
Class Schedule
Group No.
Data and Results:
Trial 1 Trial 2
Wt. of KHP, g
Final Reading- NaOH, ml
Initial Reading-NaOH , ml
Volume NaOH used

12
Normality of NaOH
Average Normality
. CALCULATIONS:
A. ANALYSIS/ CONCLUSION:
Preparation and Standardization of HCl Activity
Solution No.4
Objectives
Materials Hydrochloric Acid

Standard NaOH solution
Phenolphthalein
Formula
HCl + NaOHNaCl + H2O
meq. HCl = meq. NaOH

ml HCl = mL NaOH x N

13
N of HCl = mL NaOH x N
ml of HCl
Preparation of HCl solution:

1. Pour around 50 ml of distilled water into a 1 L volumetric flask
2. ADD 43.0 ml of HCl cautiously and gradually shaking after addition
3. Mix well, pour HCl solution into a stock bottle (glass is preferred)
4. Label and preserve for future use. [note: solution should be restandardized prior to use]
Standardization of HCl solution:

1. From a Geisslerburet, run down 20 ml of the prepared HCl solution into a 250-ml
Erlenmeyer flask.
2. Add enough distilled water to make the volume to around 50 ml
3. Add 3 drops of phenolphthalein indicator.
4. Titrate with NaOH using a Mohr buret to a light pink color end point
5. Perform 2 determinations
6. Determine the normality of HCL solution.
Worksheet
No.4 Preparation and Standardization of HCl Score

solution
Date
SME’s Name
Performed
Objective/s:
A. Data:
Trial 1 Trial 2
Volume HCl used, ml
Initial Reading-NaOH
Volume NaOH used
14
Normality of HCl
Average Normality
B. Computation
Trial 1
Trial 2
Average
C. Analysis/Conclusion:
Activity
Assay of Acetic acid
No.5
Objectives
Materials Commercial vinegar (Del Monte & another

brand)
Phenolphthalein
Formula
% Acetic acid (v/v) =
mLNaOH x N x meq.wt. CH3COOHx 100

15
Volume of sample
1. Pipet 10-15 mL of commercial vinegar into an Erlenmeyer flask

2. Add 40 ml of distilled water
3. Add 2-3 drops of phenolphthalein indicator
4. Titrate to a pale pink color with standard NaOH solution.
Reaction:
CH3COOH + NaOH CH3COONa + H2O
Worksheet
No.5 Assay of Acetic Acid

Score
Course&
Student’s Name
Year/ Sec
Date
SME’s Name
Performed
A. Data:
Trial 1 Trial 2
Volume of sample, ml
Volume NaOH used
% CH3COOH (by volume)
Average % CH3COOH
B.Computation

16
Trial 1
Trial 2
Average
A. Analysis/Conclusion:
Activity
Assay of Milk Magnesia
No.6
Objectives
Materials milk of magnesia 5g

1 N sulfuric acid
Methyl Red TS

17
Formula
% Mg(OH)2 = [(mL H2SO4 x N) – (mL NaOH x N)] x meq. Wt.x 100

Weight of sample
1. Place about 5 g of milk of magnesia,previously well shaken in its original

container,in a taredflask,and weigh accurately.
2. Add 25 ml of 1 n H2SO4 and after solution is complete, add methyl red TS
3. Titrate the excess acid with standard NaOH solution.
Reaction:
Mg (OH)2 +H2SO4  MgSO4 + 2H2O
H2SO4 + 2NaOH  Na2SO4 + 2H2O
Note: USP requires that milk of magnesia contains not less than 7 and not more than 8.5%
Mg(OH)2.
Worksheet
No.6 Assay of Milk of Magnesia Score

Course&
Student’s Name
Year/ Sec
Date
SME’s Name
Performed
Objective/s:
Data and Results:
A. Data:
Trial 1 Trial 2
Volume of sample, g
18
Volume NaOH used

% Mg(OH)2
Average % Mg(OH)2
B. Computation
Trial 2
Trial 2
Average
C. Analysis/ Conclusion:
Activity
Assay of Aspirin
No.7
Objectives
Materials Aspirin (USP grade)

Standard HCl solution
Phenolphthalein

19
Formula
C6H4OCOCH3COOH + 2 NaOH C6H4OHCOONac + CH3COONa + H2O
NaOH + HClNaCl + H2O
Formula:
% C9H8O4 = (mL HCl B.T. – mL HCl x C9H8O4 A.T.) x NHCl2000 x 100

Wt. sample
B.T. = Blank Test

A.T.= Actual Test
Procedure:
1. Weigh 1 g of Aspirin accurately in a tared Erlenmeyer flask.
2. Run down 50 ml of standard NaOH solution to a weighed sample of aspirin.
3. Cover with an inverted beaker and boil for 10 minutes.
4. Allow to cool.
5. Add 2 drops of phenolphthalein.
6. Tiltrate the excess NaOH with standard HCl solution to the disappearance of the pink
color.
7. Perform a blank determination following the same procedure following the same
procedure without the sample.
Worksheet
No.7 Assay of Aspirin Score

Student’s Name Course&Year
Date
SME’s Name
Performed
Objectives/s:
A. Data and Results

20
Blank Actual
Weight of sample,
Final reading-NaOH, mL
Initial reading-NaOH
Volume NaOH used
Normality of NaOH
Final Reading-HCl
Initial reading-HCl
Volume of HCL used
Normality of HCl
% C9H8O4
B. COMPUTATION
C. ANALYSIS/ CONCLUSION
Preparation and Standardization of Activity
AgNO3 Solution No.8

Objectives
Materials Silver nitrate crystals (analytical grade)

NaCl primary standard (AR)
0.1 M Potassium cromate solution
21
Formula
Preparation of AgNO3 Solution
1. Weigh accurately 4.3 g of pure AgNO3 crystals in a previously tared small

beaker. CAUTION: Silver nitrate will stain skin and fingernails a dark
brown. Avoid direct contact with the solid or its solutions.
2. Dissolve the silver nitrate in enough distilled/deionized water and pour
into a 250 mL volumetric flask.
3. Rinse the beaker with distilled water and transfer the rinsing to the
volumetric flask.
4. Add enough distilled water to complete the volume to 250 mL.
5. Store the solution in an amber colored bottle.
Standardization of Silver nitrate
1. Weigh accurately 0.20 to 0.25g of Standard NaCl (previously dried in an

oven at 1100C for 1 hour and stored in a dessicator) into a 250-ml conical
flask.
2. Dissolve the crystals in 50 mL of distilled/ deionized water.
3. Add 2 ml of 0.1 M potassium chromate solution
4. Titrate with standard silver nitrate solution, swiring the solution constantly,
until the reddish color of silver chromate begins to spread constantly, until
the reddish color of silver chromate begins to spread more widely through
the solution, showing that the end point is almost reached. The formation
of clumps of silver chloride is also an indicator that the end point is near.
Continue the addition of silver nitrate dropwise until there is a permanent
color change from the yellow of the chromate ion to the reddish color of
silver chromate precipitate.
5. Perform another trial.

22
Worksheet
No.8 Preparation and Standardization of Score

AgNO3 Solution
Date
SME’s Name
Performed
Objective/s:
A. Data and Results:

Trial 1 Trial 2
Weight of naCl,g

23
Final Reading- AgNO3, ml

Initial Reading- AgNO3,
Volume AgNO3, used
Normality of AgNO3,
Average Normality
B. CALCULATIONS
Trial 1
Trial 2
Average
C. ANALYSIS/ CONCLUSION: Include all reactions involved
Ammonium Thiocyanate No.9

Objectives
Materials Ammonium thiocyanate, reagent grade

Standard silver nitrate solution
Ferric ammonium sulfate T.S (ferric alum)
Nitric acid, C.P

24
Formula
V AgNO3 x N = VNH4SCNx N
NNH4SCN=V AgNO3 x N
VNH4SCN
A. Preparation of NH4SCN Solution

1. Dissolve about 2.2 g of reagent grade ammonium thiocyanate in 250 mLof
distilled water in a volumetric flask
2. Transfer in a stock bottle and label.
Standardization of NH4SCN
1. Place 15 mL of 0.1 N silver nitrate accurately measured from a pipet or buret in
an Erlenmeyer flask.
2. Dilute with 20 mL of distilled water, then add 1 ml of nitric acid and 1 ml of ferric
alum T.S.
3. titrate the solution with the ammonium thiocyanate solution until a red-brown color
appears.
4. Calculate the normality of the solution.
Reaction
AgNO3 + NH4SCN AgSCN + NH4NO3
Fe NH4 (SO4)2 + 3 NH4SCN  Fe (SCN)3 + 2 (NH4)2SO4
Volhard Method: Assay of Sodium Activity
Chloride No.10
Objectives
Materials Sodium chloride 250 m

Nitrobenzene 5 ml
0.1 N ammonium thiocyanate
25
0.1N silver nitrate 50 ml

Ferric alum solution 2 ml
Nitric acid 3 ml
Formula
NaCl + AgNO3AgCl + NaNO3
% NaCl= (mL AgNO3X N) – (mL NH4SCN x N) x meq. Wt. NaCl x 100

gram sample
1. Weigh accurately about 250mg of sodium hloride, dissolve it in 50 mL of water
in a glass-stoppered flask.
2. Add 50 ml of 0.1-N silver nitrate, 3 ml of nitric acid, 5 ml of nitrobenzene, and 2
ml of ferric ammonium sulfate TS.
3. Shake well, and titrate the excess silver nitrate with 0.1-N ammonium
thiocyanate..
Worksheet
Score
No.10
Volhard Method: Assay of
Sodium Chloride
Date
SME’s Name
Performed
Objective/s:

Trial 1 Trial 2
Weight of NaCl,g

26
Final Reading- NH4SCN, ml

Initial Reading-NH4SCN
Volume NH4SCNused
Volume of AgNO3
% NaCl
Average % NaCl
B. CALCULATIONS
Trial 1
Trial 2
Average
Assay for Iodide content in Povidone- Activity
iodine No.11
Objectives
Materials Sodium bisulfide TS

0.1 N silver nitrate 25 ml
nitric acid 10 ml
Povidone-iodine 500 mg

27
Formula
% Iodine= (mL AgNO3 x N- mL NH4SCN x 126.9N) 1000x 100

gram sample
1. Dissolve about 500 mg of povidone- iodine, accurately weighed, in 100 ml of water in an
Erlenmeyer flask
2. Add sodium bisulfide TS until the color of iodine has disappeared completely. Add 25.0 ml of
0.1 N silver nitrate and 10 ml of nitric acid, mix.
3. Titrate the excess silver nitrate with 0.1 N ammonium thiocyanate, using ferric ammonium
sulfate TS as an indicator
4. Perform a blank determination
5. Calculate the amount of iodine ion.
Note: To calculate the amount of iodine ion, the amount of available odine determined using
sodium thiosulfate is subtracted from the total iodine as determined above to obtain the amount
of iodine ion.
Blank test is conducted to correct for matrix interferences.
Worksheet
Score
No.11 Assay for Iodide Content in

Povidone-Iodine
Course&Yr
Student’s Name
Date
SME’s Name
Performed
Objective/s:

Trial 1 Trial 2
Weight of sample,g

28
Final Reading- NH4SCN, ml

Initial Reading- NH4SCN
Volume NH4SCNused
Volume of AgNO3
% Iodide
Average % iodide
B. CALCULATIONS
Trial 1
Trial 2
Average
C. ANALYSIS/ CONCLUSION: Write all the equations for the chemical reactions
involved
EDTA Solution No.12

Objectives
Materials Disodium ethylenediaminetetraacetate

Calcium carbonate as primary standard
Dilute HCl solution
Sodium Hydroxide T.S
Hydroxynaphthol blue powder
29
Formula
mmol EDTA= mmol CaCo3 mL EDTA x M = wt. of caCO3
mmol wt. of CaCO3
Molarity of EDTA = wt. of caCO3

mmol wt. of CaCO3 x VEDTA
A. Preparation of EDTA solution

1. Dissolve about 4.8 g of EDTA powder in sufficient distilled water in a
small tared beaker.
2. Transfer the solution to a 250-mL volumetric flask
3. Rinse the beaker with distilled water, adding the rinsing into the flask
4. Dilute to volume with distilled water
5. Standardize the solution using the following procedure
B. Standardization of EDTA solution

1. Weigh accurately 100 mg of primary standard CaCO 3 and transferit
to a flask
2. Add 20 mL of distilled water and sufficient diluted HCl to dissolve the
carbonate
3. Dilute with distilled water to 100 mL
4. Add 15 mL of NaOH solution (pH should be around 13), then add a
pinch of hydroxynaphthol blue indicator
5. Titrate the solution with EDTA until it turns into a deep blue color
6. Run a second trial and calculate its molarity.
Worksheet
No.12 Preparation & Standardization of Score

EDTA Solution
Date
SME’s Name
Performed
Objective/s:
A. Data & Results

Trial 1 Trial 2

30
Weight of CaCO3,g
Final Reading- EDTA, ml
Initial Reading- EDTA
Volume EDTA used, mL
Molarity of EDTA
Average molarity
B. CALCULATIONS
Trial 1
Trial 2
Average
Activity
Assay of Calcium Lactate
No.13
Objectives
Materials Calcium lactae powder

Diluted HCL solution (23.7 in 100) or 3N
EDTA solution, 0.05
Sodium hydroxide TS

31
Formula
% Calcium lactate= VEDTA x M x millimole of C6H10CaO6 x 100

Weight of sample
% Calcium lactate= VEDTA x M.F x titer x 100

Weight of sample
1. Weigh accurately about 400 mg of calcium lactate powder in a suitable container and
dissolve in 150 mL of water containing diluted HCl solution
2. Add 15 mL of sodium hydroxide T.S. and a pinch of hydroxynaphthol blue podwer
3. Titrate with 0.05 M EDTA solution until a deep blue color is obtained.
Worksheet
No.13 Assay of Calcium Lactate Score

Date
SME’s Name
Performed
Objective/s:
A. Data & Results

Trial 1 Trial 2
Weight of sample,g
Final Reading- EDTA, mL
Initial Reading- EDTA
32
Volume EDTA used, mL

Molarity of EDTA
% Calcium lactate
Average % C6H10CaO6
B. CALCULATIONS
Trial 1
Trial 2
Average
KMnO4 No.14
Objectives
Materials Potassium permanganate

Glass wool
Sodium oxalate
Conc. H2SO4
Formula
N KMnO4 = gNa2C2O4 mL KMnO4 x Na2C2O4

2000

33
Preparation of KMnO4 solution:
1. Weigh roughly 1 g of KMnO4

2. Dissolve it in 300 ml of water in a beaker
3. Cover with a watch glass and boi; the solution for 15 minutes
4. Allow to stand for at least 2 days
5. Filter through glass wool into an amber colored bottle.
Standardization of KMnO4 solution:
1. Weigh 0.2 g of Na2C2O4

2. Dissolve it in 250 ml distilled water in a big beaker
3. Add 7 ml of conc. H2SO4
4. Heat the solution to 700C
5. Titrate with potassium permanganate solution until a light pink color which
persists for 15 seconds s obtained.
Equation:
2 KMnO4 + Na2C2O4 + 8 H2SO42 MnSO4 + K2SO4 + 10 CO2 + 5 Na2SO4 + 8 H2O
Worksheet
No.14 Preparation and Standardization Score

of KMnO4
Date
SME’s Name
Performed
Objective/s:
A. Data:
Trial 1 Trial 2
Weight of Na2C2O4, g
Final Reading- KMnO4, ml
Initial Reading- KMnO4,
Volume KMnO4 used, mL
Normality of KMnO4,
Average Normality
34
B. Computation
Trial 1
Trial 2
Average
Activity
Assay of Hydrogen Peroxide Solution
No.15
Objectives
Materials Hydrogen peroxide solution 2 ml

Diluted sulfuric acid 20 ml
0.1-N potassium permanganate
Formula
35
1. Pipet 2 ml of hydrogen peroxide solution into a suitable flask containing 20 ml of water

2. Add 20 ml diluted sulfuric acid, and titrate with 0.1 N potassium permangate
3. calculate for the % of H2O2
Equation:
5H2O2 + KMnO4 + 3H2SO4 502 + 2MnSO4 + K2SO4 + 8H2O

34.01
Note: A solution of H2O2 should contain not less than 2.5 g and not more than 3.5 g of
H2O2.
Worksheet
No.15 Assay of Hydrogen Peroxide Score

solution
Date
SME’s Name
Performed
Objective/s:
A. Data:
Trial 1 Trial 2
Volume of sample, mL
Initial Reading- KMnO4,
Normality of KMnO4,
% H2O2
Average % H2O2
B. Calculations

36
Trial 1
Trial 2
Average
Preparation & Standardization of Activity
H2C2O4 No.16
Objectives
Materials Oxalic acid

Conc. Sulfuric acid
Standard KMnO4 solution
Formula
meq. H2C2O4 = meq. KMnO4
mL H2C2O4 x N = mL KMnO4 x N
N H2C2O2 = mL KMnO4 x N
mL H2C2O4

37
Preparation of oxalic acid solution:
1. weigh roughly 1.6 g of H2C2O4
2. Dissolve it in enough distilled water to make 250 mL
3. Store the solution in an amber colored bottle
Standardization of oxalic acid solution:

1. Run down 30 ml of H2C2O4into a big beaker
2. Dilute with 200 ml of distilled water
3. Add 7 ml of conc. H2C2O4
4. Titrate with KMnO4 to a light pink end point which persists for 15 seconds
Equation:
2 KMnO4 + 5 H2C2O4+ 3 H2SO4 2 MnSO4 + K2SO4 + CO2 + 8 H2O
Worksheet
No.16 Preparation & Standardization of

H2C2O4 Solution
Score

Date
SME’s Name
Performed
Objective/s:
A. Data:
Trial 1 Trial 2
Initial Reading- KMnO4,ml
Normality of KMnO4,
% H2C2O4
Average % H2C2O4
B. Calculations

38
Trial 1
Trial 2
Average
Activity
Assay of Sodium Nitrite
No.17
Objectives
Materials Sodium nitrite

Standard KMnO4
Standard H2C2O4
Conc. H2SO4
Formula
% NaNO2 = H2C2O4 NaNO2{total ml of KMnO4} – {ml x N} 2000

wt. of sample in the aliquot portion taken
1. Weigh 0.5 g of sodium nitrite accurately
2. dissolve it in enough distilled water to make 100 ml in a volumetric flask
3. pipet 10 ml of sodium nitrite solution
39
4. Introduce it into a beaker containing a micture of

20 ml KMnO4
100 ml of distilled water
5 ml of conc. H2SO4
5. Warm the liquid to 400C and allow it to stand for 5 minutes
6. Add 25 ml of standard oxalic acid solution
7. heat to 80C
8. titrate with standard KMnO4 to a light pink
Equation:
2 NaNO2 + H2SO4 2 HNO2 + Na2SO4

5 HNO2 + 2 KMnO4 + 3 H2SO4  5 HNO3 + K2SO4 + 2 MnSO4 + 3 H2O
2 KMnO4 + 5 H2C2O4 + 3 H2SO4 2 MnSO4+ K2SO4 + 1OCO2 + 8 H2O
Worksheet
No.17 Assay of Sodium Nitrite Score

Date
SME’s Name
Performed
Objective/s:
A. Data:
Trial 1 Trial 2
Initial Reading- KMnO4
Total Volume KMnO4 used,
mL
Normality of KMnO4,
Volume H2C2O4
N of H2C2O4
% NaNO2
Average % NaNO2
B. Calculations
Trial 1

40
Trial 2
Average
Iodine Solution No.18

Objectives
Materials Iodine crystals (analytical grade)

Potassium iodide
6 N HCl
Arsenic trioxide (analytical grade)
1 N NaOH
Methyl orange
Sodium bicarbonate
Starch T.S (freshly prepared)
Formula
N I2 = g As2O3
mL I2 x meq.wt.As2O3
N I2 = g As2O3
mL I2 x As2O3 /4000
Preparation of Iodine solution:
1. Weigh roughly 3.5g of iodine crystals
2. Dissolve it in a solution of 9g potassium iodine in 100 ml of distilled water
3. Add 3 drops of 6N HCl

41
4. Add enough distilled water to complete the volume of 250 ml

5. Store in an amber colored bottle.
Standardization of Iodine solution:

1. Weigh accurately 0.2 g of arsenic trioxide
2. Dissolve it in 20 ml of 1 N NaOH
4. Add 2 drps of methyl orange
5. Add 6 N HCl until yellow color is changed to pink
6. Then add 2 g of sodium bicarbonate
8. Add 3 ml of starch T.S.
9. Titrate with iodine to a blue end point
Worksheet

of Iodine Solution
Date
SME’s Name
Performed
Objective/s:

Trial 1 Trial 2
Weight ofAs2O3,g
Final Reading- I2, ml
Initial Reading-I2, ml
Volume I2, used,ml
Normality of I2
Average N I2
B. CALCULATIONS
Trial 1

42
Trial 2
Average
C. ANALYSIS/ CONCLUSION: write all the equations for the chemical reactions
involved.
Na2S2O3 Solution No.19

Objectives
Materials Sodium thiosulfate

Sodium carbonate
Formula
N Na2S2O3 = ml I x N
ml Na2S2O3
Preparation of sodium thiosulfate solution:
1. Weigh roughly 6.5 g of sodium thiosulfate and 0.1 g of sodium carbonate
2. Dissolve this in 250 ml of recently boiled and cooled water
Standardization of sodium thiosulfate solution

1. Run down 30 ml of sodium thiosulfate solution
3. Add 5 ml of starch solution
4. Titrate with iodine to a blue color end point
43
Equation:
2 Na2S2O3 + I2 2 NaI + Na2S2O6
Worksheet

of Na2S2O3 Solution
Date
SME’s Name
Performed
Objective/s:

Trial 1 Trial 2
Volume of Na2S2O3 used,
ml
Initial Reading- I2, ml
Volume I2, used,ml
Normality of I2
Normality of Na2S2O3
Average N Na2S2O3
B. CALCULATIONS
Trial 1
Trial 2

44
Average
C. ANALYSIS/ CONCLUSION: write all the equations for the chemical reactions
involved.
Assay of Antimony Potassium Activity
Tartrate No.20
Objectives
Materials Antimony potassium tartrate (tartar emetic)

Standard iodine solution
Staurated solution of sodium bicarbonate
Starch T.S
Formula
% KOSbC4H4O6 . ½ H2O = % KOSbC4H4O6 . ½ H2O ml I2 x N x 2000 x 100

wt. sample
1. Weigh 0.5 g tartar emetic accurately in a tared flask

2. Dissolve it in 30 ml of distilled water
3. Add 25 ml of saturated solution of sodium bicarbonate
4. Add 5 ml of starch T.S.
5. titrate with standard iodine solution to a blue color end point
Equation:
KOSbC4H4O6 + I2 + 2 NaHCO3 KO2SbC4H4O6 + 2 NaI + CO2 + H2O

45
2 HI + 2NaHCO3 2 NaI + 2H2O + CO2
Worksheet
No.20 Assay of Antimony Potassium Score

Tartrate
Date
SME’s Name
Performed
Objective/s:

Trial 1 Trial 2
Wt. of sample, gram
Initial Reading- I2, ml
Volume I2, used,ml
Normality of I2
% KOSbC4H4O6
Average % KOSbC4H4O6
B. CALCULATIONS
Trial 1
Trial 2

46
Average
Activity
Assay of Cupric Sulfate
No.21
Objectives
Materials Cupric sulfate

Acetic acid
Potassium iodide
Standard sodium thiosulfate solution
Formula
% CUSO4 . 5H2O =CUSO4 . 5 H2Oml x N Na2S2O3 x 1000 x 100

wt. sample
Procedure
1. Weigh accurately 0.5g of cupric sulfate in a tared Erlenmeyer flask
2. Dissolve it in 50 ml of distilled water
3. Add 3 ml of 6 N acetic acid
4. Add 3 g of potassium iodide
5. Titrate the liberated iodeine with standard sodium thiosulfate until a golden yellow
color is obtained
6. Add 3 ml of Starch T.S.
7. Continue the titration with standard sodium thiosulfate solution to the
disappearance of the blue color
Equation:
47
2 CUSO4 . 5_H2O + 4 Ki  2 CUI + I2 + 2 K2SO4 + 10 H2O
I2 + 2 Na2S2O3  2 NaI + Na2S4O6

Sodium Sodium
Thiosulfate tetrathionate
Worksheet
No.21 Assay of Cupric Sulfate Score

Date
SME’s Name
Performed
Objective/s:

Trial 1 Trial 2
Wt. of sample, gram
Final Reading- Na2S2O3,ml
Initial Reading- Na2S2O3, ml
Volume I Na2S2O3, used,ml
Normality of I Na2S2O3
% CUSO4
Average % CUSO4
B. CALCULATIONS
Trial 1
Trial 2
Average
48
Gravimetric Methods:Determination Activity
of Soluble Chloride No.22

Objectives
Materials Soluble chloride salts (to be given as unknown)

5% silver nitrate solution
Diluted nitric acid
Glass wool
Suction filtration set-up
Formula
3. Test the solution by touching a strip of blue litmus paper with moist stirring rod. If it
is not acid in reaction, add sufficient acid to to make it so.
4. Measure out 5 ml in excess of the amount of silver nitrate solution theoretically
required to precipitate all the chlorine as silver chloride. Add the silver nitrate
solution in a small successive portions, stirring, gradually heat the mixture to the
boiling point
5. Cover the beaker with a watch glass, and with occasional stirring, gradually heat
the mixture to the boiling point
6. Turn down the flame and digest the mixture, without boiling for 10 min.
7. if a precipitate forms, add 5 ml more silver nitrate solution, str, allow to settle, and
test as before. Set the beakers aside away from direct sunlight to allow the
precipitate to settle.
Note: The solution is acidified with nitric acid to prevent the precipitation of other
substances insoluble in water but soluble in nitric acid, such as carbonates, oxides
and phosphates. The acid helps to coagulate any colloidal silver chloride. Too geart
an excess of nitric acid must not be added, since it exerts some solvent action on
silver halides. The acidified solution should not be heated until the silver nitrate is
49
added, since chlorine may be liberated and lost.
8. During intervals in the above procedure, carefully clean and prepare two Gooch
crucibles for filtration (Note: matted Gooch crucibles are prepared ahead of time.
These should have been dried to constant weight at this point).
9. After the crucibles have been properly prepared, heated to constant heat, and
weighed, fit them into the suction flask.
10. Decant most of the supernatant liquid into the Gooch crucible, using gentle suction
to hasten filtration, guiding the liquid into the crucible by means of glass rod held
against the lip of the beaker. Wash the precipitate three times with 15 ml portions
of 0.01-N nitric acid
11. When the third wash solution has been added to the precipitate, transfer the
precipitate into the Gooch crucible using a steam of wash solution from the wash
bottle and a “policeman” to dislodge all particles that adhere to the sides of the
beaker and guide rod
12. Wash the precipitate on the glass filter with several small protions

50

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Drug Testing and Assay Manual

Introduction Remarks & General Laboratory Directions

1 Weight Variation Test

2 Determination of Content Uniformity

3 Preparation & Standardization of HCl Solution

4 Preparation & Standardization of NaOH

5 Assay of Acetic Acid

6 Assay of milk magnesia

8 Preparations and Standardizations of AgNO3

9 Preparation and Standardization of NH 4SCN

10 Determination of Chloride by the Volhard Method

11 Assay for Iodine Content in Povidine Iodine

12 Preparation and Standardization of EDTA Solution

13 Assay of Calcium Lactate Estornino’s group

14 Preparation & Standardization of KMnO4 Ayon’s group

15 Assay of Hydrogen Peroxide Solution Plaza’s group

16 Preparation and Standardization of H2C2O4 Solution (Oxalic acid) Bedayo’s group

17 Assay of Sodium Nitrite Amon’s group

18 Preparation and Standardization of Iodine Solution Piao’s group

19 Preparation and Standardization of Na2S2O3 Laure’s group

20 Assay of Antimony Potassium Tartrate Joe’s group

21 Assay of Cupric Sulfate Agno’s group

22 The Gravimetric Determination of Soluble Chlorides

REMARKS AND GENERAL LABORATORY DIRECTIONS

OBJECTIVES OF QUANTITATIVE PHARMACEUTICAL CHEMISTRY LABORATORY

1. The acquisition of a fundamental knowledge of the theory as well as a practical

THE LABORATORY NOTEBOOK

1. Use a bound notebook (a small bound notebook for each group).

Economical utilization of laboratory hours is best achieved through a preliminary

SAFETY IN THE LABORATORY

PURITY AND STRENGTH REQUIREMENTS

THE ANALYTICAL BALANCE

The introduction of a single-pan substitution type analytical balance has

Rules for the Use and Care of Balance

1. Use the balance assigned by the instructor.

College of Health Sciences

College of Health Sciences

% wt.variation =Diff.bet. Actual wt. per tab &ave.wt. x 100

College of Health Sciences

Note: Refer to the USP for the requirements

No.1 Weight Variation Test

Student’s Name Course& Year

SME’s Name Date Performed

Net weight per capsule:

Total weight of the 20 capsules: __________

College of Health Sciences

% wt. variation = Actual weight per capsulex 100

Weight of the weighing bottle: ________________

Net weight per tablet:

Total weight of the 20 tablets______________

Average weight = weight of 20 tablets

8. wt.var. = ____________ 18. wt.var. = ____________

Materials Sodium bicarbonate tablets 300 mg

Percent of labeled amount:

Content of NaHCO3/tablet obtainedx 100

No.2 Determination of Content Uniformity Score

Student’s Name Course&Yr

SME’s Name Date Performed

Weight per tablet

8. wt.var. = 18. wt.var. =