1
FINAL:
Pharmacology- branch of knowledge concerned with medicinal drugs obtained from
plants or other natural sources; Crude drugs extraction; collecting plant parts for
extraction.
MOISTURE CONTENT ANALYSIS/ DETERMINATION- the loss of mass of a
substance when heated by the process of water evaporation.
*presence of moisture in a crude drug can lead to its deterioration due to either
activation of certain enzymes or growth of microbes.
*you should not dry the drug into direct sunlight. Do not heat above 50-60 temperature
when using the oven. (moisture content can be determined by heating the drug at 150
degree Celsius in an oven to a constant weight and calculating the loss of weight.
*crude drug determination usually done for 40 days up.
*collect plant parts you need to analysis if substances responsible for antiseptic is
present.
*air drying means drying your leaves without sunlight, you just exposed it to the air.
*one factor that affects the presence of your substance is when you direct sun dry it, the
percentage of your extract will decreased.
Do not heat in a direct sunlight so that any volatile present in the crude drug will not be
affected. If you do, it will volatilized and the analysis of your crude drug will be in no
effect.
Black part/spot in your crude drug happens when the bacteria/ yeast takes place. This
is the process of fermentation thus affect the quality of your materials and extraction
since fermentation is acidic.
Weigh anytime your leaves to see the changes of the leaves whilst being air dry, not
until it reach zero grams, you are now ready to extract it.
ASH VALUES- refers to the amount of inorganic matter present in the crude drug or
collected along with the drug; During harvesting of your materials, some materials not
included are mixed with your materials that is why you perform ash values to remove
this unimportant materials.
1. Total Ash Values
2. Acid Insoluble Ash
3. Water soluble Ash
4. Sulphated Ash
Classification of Alcoholic Volatile Oils:
1. Acyclic- e.g. geraniol, linalool, citranellol.
2. Monocyclic- e.g. menthol, alpha-terpineol
3. Dicyclic- e.g. borneol
4. Higher aliphatic alcohols- zingerberol which is sesquiterpene.
Subdivision of Alcoholic Volatile Oils:
1. Saturated aliphatic alcohol- usually found to be esterified with fatty acids during
distillation and these esters with fatty acids during distillation and these esters undergo
hydrolysis to give lower members of the saturated aliphatic alcohols together with lower
members of the fatty acids.Such examples are:
>methanol, ethanol- which are the byproduct of yeast fermentation due to plant starch.
2. Unsaturated aliphatic alcohol- oils found in essential oils or aromatic oils. Such
examples are:
>Geraniol oil(lemon oil) -found abundantly in rose oil, oil of palmarose, oil of lemon
grass.
>Linalool oil- an essential oil which is a major component of linaloe oil from Ceylon
cinnamon.
>Nerol- is the cis-isomer of geraniol found in the oil of Neroli (fresh and tender flower of
orange tree).
PRELIM: METRIC SYSTEM
Scientific Measure:
1. Metric liquid measurement- e.g. volume - liter - graduated cylinder
2. Metric weight measurement- e.g. mass - gram - triple beam balance scale
3. Metric length measurement- e.g. length - meter - meter stick
1 cup = 1/2 pint, 1 cup = 16 tsp, 20 drops = 1 ml
3 tsp. = 1 tbsp, 2 cups = 1 pint, 1 tsp = 5 ml, tbsp = 15 ml
Measuring Weight and Mass:
*when measuring mass/ weight we are dealing with solid.
Weight- measure of the gravitational force acting on a body and is directly proportional
to its mass. Varies slightly with latitude, altitude, temperature, and pressure.
Measure- determination of the volume or extent of a body. They are affected by
temperature and pressure especially gas and liquid.

Weighing- determining a definite weight of material to be used in compounding a
prescription or manufacturing some dosage forms,
Measuring- determining definite volume of liquids to be used in compounding/
manufacturing some dosage forms.
Weight and mass- using beam and balance scale.
When measuring- liquid; When weighing- solid
Weighing Balance- instrument used to determine the relative weight of a substance.
Prescription Balance- weighing medicinal substances required in filling of prescription.
High Precision Analytical Balance- used to weigh very small quantities accurately of
0.1 mg and equipped with digital read out feature with maximum weight 60- 21- gram.
>errors of +- 5% or less is acceptable.
>errors may come from the method and apparatus used resulting to discrepancies of
results.
Conversions Between Metric Units:
> 1 centimeter (cm) = 10 millimeters (mm)
>1 meter (m) = 100 centimeters = 100 millimeters
>1 kilometer (km) = 1000 meters
>1 liter (L) = 1000 milliliter (ml) = 100 centimeters (cl)
>1 kiloliter (kl) = 1000 liters = 1000000 milliliters
>1 grams (g) = 1000 milligrams (mg)
>1 kilogram (kg) = 1000 grams (g)
TYPES OF ERRORS:
1. Intermediate Errors- slightly variations in a series of observations made by the
same observers under identical conditions. The differences are difficult to detect.
Intermediate errors are from the measurement errors
2. Determinate Errors- constant; each of a series of determination arising from
personal error (analyst) like inability to judge color changes sharply resulting to habitual
reading of endpoints, and they are made by faulty procedure, apparatus due to poor
calibration reading; determinate errors are errors committed by disperse person/
analyst.
3. Absolute Errors- differences between mean value and true value
4. Relative Errors- results of dividing the absolute error by the value usually reported
on a percentage basis by multiplying it by 100
5. Percentage Error- maximum potential error multiplied by 100 and divided by the
quantity desired
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Rules in reading measuring liquids:
-eye level, reading/looking at the read out measurement/meniscus.
*meniscus- the upward or downward curve at the surface of a liquid.
Concentration- refers to the amount of solute that is dissolved in a solvent like:
1. Adding salt (solute) to water (solvent)
2. Adding smaller amount of water (solute) to a larger amount of ethanol (solvent)
3. Adding small amount of ethanol (solute) to water (solvent)
Solutions- a liquid mixture in which the minor component is uniformly distributed within
the major component (the solvent)
SOLUBILITY:
1. Diluted solution- has very little solute; can dissolve a lot more solute.
2. Concentrated solution- has a lot solute in it; can dissolve a little more solute
3. Saturated solution- has maximum amount of solute in it; cannot dissolve anymore
solute.
TYPES OF CONCENTRATION EXPRESSION:
1. Percent Composition by Mass (% w/v) - mass of the solute divided by the mass of
the solution multiplied by 100.
e.g. determine the % composition by mass of a 100 mL NaCl solution which contain
20g salt. ANS: 0.2 x 100= 20% w/v
2. Volume percent (%v/v)- volume of solute divided by the volume of the solution
multiplied by 100.
e.g. a wine is about 122% v/v ethanol, it means that for every 100mL of wine is 12mL of
ethanol
3. Mole Fraction (xi)- number of moles of a compound divided by the total number of
moles of all chemical species in the solution. The sum of all mole functions in a solution
is always equal to 1.
Formula:
*mole fraction of solute: moles of solute/ moles of solute + moles of solvent.
*moles fraction of solvents: moles of solvent/ moles of solute + moles of solvent.
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e.g. problem: Given:

molecular weight of water (H2O)= 18g/mol Mol wt zinc nitrzte = 189g/mol
Molecular weight of glycerol (C3H8O3)= 92g/mol Wt. Of solute= 63g
Volume of solution= 500mL/1000 = 0.5L
Computation:
Water= 90g x 1 mol/18g= 5 mol DETERMINATION OF EQUIVALENT WEIGHT FOR ACIDS:
Glycerol= 92g x 1 mol/92g= 1 mol Molecular wt / no. Of replaceable Hydrogen ion.
Total= 6 mol
COMPOUND MOLECULAR WT EQUIVALENT WT
Mole fraction of water= 5 mol/6mol= 0.833 HCL 36g/mol 36/1= 36
Mole fraction of glycerol= 1mol/6mol=0.167 H2SO4 98g/mol 98/2= 49
Total= 1.000 H3PO4 98g/mol 98/3=33

4. Molarity (M)- number of moles of solute per liter solution. DETERMINATION OF EQUIVALENT WEIGHT FOR ALKALINE:
Formula: number of moles solute/ number of liters of solution Molecular wt/ no. Of replaceable OH

5. Molality (m)- number of moles of solute per 1000g of solvent. COMPOUND MOLECULAR EQUIVALENT WT.
Formula: m= moles of solute/ 1000g solvent KOH 56g/mol 56/1= 56
Ca(OH)2 74g/mol 74/2= 37
6. Normality (N)- number of grams equivalent of solute per liter solution. Al(OH)3 78g/mol 78/3=26
Formula: N= number grams equivalent of solute/ liter of solution
DETERMINATION OF EQUIVALENT WT FOR SALT:
*number of gram equivalent of solute= weight in grams/ equivalent weight. Molecular wt / total + or - valence
*equivalent weight= molecular weight/ number of replaceable H+, OH, salt.
COMPOUND MOLECULAR WT EQUIVALENT WT
In Percent Composition by Mass, you are measuring solid dissolved in a solution NaCl 58g/mol 58/1=58
aqueous solution. Examples are those solution of table salt. Na2SO4 142 g/mol 142/2=71
Al2(SO4)3 342 g/mol 342/3=114
Interpret this. “determine the % composition by mass of a 100mL NaCl solution which
contains 20g salt.” = in every 100mL of Sodium Chloride solution, there is 20 grams of rules:
salt NaCl. (a)1 is equivalent of an acid neutralizes exactly 1 equivalent of a base and vice versa.
(b) 1 equivalent of an oxidizing agent react with exactly 1 equivalent of reducing agent
Molarity is the ratio of moles of solute to the volume of solution in liters. Molality is the and vice versa.
ratio of moles of solute to the volume of solvent in kilograms.
(pag 1000mL, it must be Molarity; pag 1000grams, it must be Molality) Solutions- homogeneous mixture of 2 or more substances. The relative proportions of
which may vary continuously within certain limits.

E.g. PROBLEM SOLVING: determine the normality of a solution which contain 63g of COMPONENTS OF SOLUTIONS:
Zinc nitrate in 500mL solution.
1. Solvent- substance in which another substances is dissolved or the substances
What to do? which is present in layer quantity.
1. Normality= grams equivalent wt. of solute/ liter solution
2. Equivalent wt. Of solute= M.W/ # rep (-A valence) of salt 2. Solute- dissolve substances or the constituent which is present in smaller quantity.
3. Gram equivalent wt of solute= 63g/189g/mol 2 e.g. Salt in water; alcohol in water
=63g/94.5g/mol
= 0.67 mol (Solvent= water, Solute= sugar, Solution= water + sugar)
4. N= 0.67 mol/0.5 mL
=1.34 N
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3 TYPES OF SOLUTIONS: *remedy for supersaturated solution= heating.

1. Liquid solutions- vodka in water (liquid in liquid); sugar solution Dilution- adding of solvent resulting to a solution to a solution of lower concentration.
(solid in liquid solution); carbonated water (gas in liquid solution)
Equation: MiVi = MfVf
2. Gaseous solution- air, natural gas (gas solute in gas solvent) M= Molarity; v= Volume; I= initial values; f= final values
3. Solid solution- brass, steel (alloy) solid solute or solid solvent; hydrogen in platinum
( gas in liquid) 5 TYPES OF CHEMICAL REACTIONS:

Synthesis reaction- two or more elements/compounds combine to form a more

2 TYPES OF SOLUTIONS BY REASONS OF HEAT CHANGE: complex product/ to form a new product.
e.g. 2Na + Cl2= 2NaCl
1. endothermic solution- reaction which in the process of dissolving the solute; heat
is absorbed; if more energy is required to break the bonds within the solute and solvent Decomposition reaction- one chemical species breaks down to simpler
than is released when new bond are formed between the solute and solvent. elements/compounds
e.g. melting in cubes; cooking; photosynthesis; ice melting e.g. 2H20 = 2H2 + O2

2. Exothermic solution- reaction which heat is evolved when dissolved in water like Single replacement reaction- uncombined element replaces a less reactive element a
NaOH; if more energy is release when new bonds are formed between the solute and compound, creating a new compound and a single element.
solvent than is required to break the bonds within the solute and solvent. e.g. 2Al + 2HCl =2AlCl + H2
e.g. rusting of iron; when carbon burns in oxygen to form carbon dioxide a lot of heat is
produced; burning of sugar Double replacement reaction- involves two ionic compounds (in solution) that trade
cations creating two new ionic compounds
e.g. 2HCl + 2Na(OH) = 2NaCl + 2H2O
2 TYPES OF SOLUTIONS ACCORDING TO THE AMOUNT OF SOLUTE PRESENT:
Combustion reaction- hydrocarbon (or other organic molecule) burning in oxygen
1. Diluted solution- contains small proportion of solute relative to solvent. producing carbon dioxide and water.
e.g. 2CH4 + 4O2 = 2CO2 + 4H2O
2. Concentrated solution- contains large proportion of solute relative to solvent.

Chemical Equation- describes what happens in a chemical reaction.

3 TYPES OF SOLUTION ACCORDING TO THE CAPACITY OF SOLVENT TO
DISSOLVED AT A CERTAIN TEMPERATURE AND PRESSURE:

1. Saturated solution- a solution which more solute will dissolved

2. Saturated solution- solution which no mote solute will dissolved.
3. Supersaturated solution- solution that holds more solute than it can normally
dissolved.

*do not add corrosive chemicals to water instead add water to the corrosive chemicals.
When you add more solute to the solution, the concentration becomes highly
concentrated.

A corrosive substance is one that will damage other substances with which it comes
into contact by means of chemical reaction.
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Analyte/ Active Constituent- a substance whose chemical constituents are being

identified and measured.

Titrant- a solution of known concentration that is added (titrated) to another solution to

determine the concentration of a second chemical species. The titrant may also be
called the titrator, reagent, or standard solution.

Indicator- complex organic compounds which change color at or near point in the
titration where equivalent quantities of analyte and titrant have reacted.

Purpose of Volumetric Analysis- it determines the unknown concentration of a known

reactants. Often referred to as titration method. A laboratory technique in which one
substance of known concentration and volume is used to react with another substance
of an unknown concentration.

Rate of Chemical Reaction- expressed as the amount of chemical substance that

undergoes change in the unit period of time.

Stoichiometric point/ Equivalence point/ End point- theoretical point at which

The Chemical equation identifies the:
equivalent amounts of each component have reacted, thus this is the point at which the
1. Reactants (starting materials) and the product (resulting substance)
components have stopped reacting. It signals the analyst to stop adding reagent and
2. Formula of the participating materials
make the final reading on the burette.
3. Phases of the participating materials (solid, liquid, gas)
4. Amount of each substances or materials.
Titration- a process in which a standard reagent is added to a solution of analyte until
the reaction is in equilibrium or complete or the change in color
Balancing a chemical equation- establishing the mathematical relationship between
e.g. HCL + NaOH ….. NaCl + H2O
the quantity of reactants and product. The quantities are expressed in grams or moles.
(titrant , analyte)
GENERAL METHODS USED IN PHARMACEUTICAL ANALYSIS:
If original color is colorless, and if added another color and then changed color, it
1. Volumetric analysis ( titrimetric)
means that you have reached the point that each mixtures are reacted with one another.
2. Acidimetric/ alkalimetric analysis
3. Precipitation and Complexation Analysis
Buffer solution- resist changes in PH when diluted or when small amount of acid or
4. Oxidation- Reduction methods
base are added.
SPECIAL METHODS USED IN PHARMACEUTICAL ANALYSIS:
* acid + base = it is called neutralization
-usually used in raw materials analysis for making drugs.
1. Ash and water determination
Any strong base/ acid can be used as titrant because most reactions are quantitative,
2. Extractive and crude fiber content
meaning they are easily counted.
3. Constants of fats, fatty oils, waxes, balsams, etc.
4. Assay of volatile oils
Weak Acid- one that dissociates completely, donating only some of its hydrogen ions
5. Assay of alkaloids and amine drugs
into solution.
e.g. Acetic acid, carbonic acif, formic acid, hydrocyanic acid, hydrofluoric acid,
Volumetric Analysis- general term for a method in quantitative analysis wherein the
phosphoric acid
amount of a substance is determined by the measurement of the volume it occupies
Weak Base- a proton acceptor that does not ionize fully in an aqueous solution.
Quantitative Analysis- chemical analysis determined the amounts or proportion of the
e.g. Ammonia, diethylamine, methylamine, sodium bicarbonate
components of a substance or moisture. e.g. the volume of the titrant required to just
completely react with the analyte
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STRONG ACID: MIDTERM & SEMI:

Hydrobromic acid, hydrochloric acid, hydroiodic acid, nitric acid, perchloric acid. Sulfuric
acid, hydrogen chloride (HCl) Direct titration- most basic titration which is commonly used. In direct titration you add
a standard titrant to the analyte until you reach the endpoint.
STRONG BASE:
Barium hydroxide. Calsium hydroxied, lithium hydroxide, potassium hydroxide, sodium In BACK TITRATION, you add an excess of standard titrant to the analyte and then
hydroxide, strontium hydroxide you titrate the excess titrant to determine how much is in excess.

*heating will make the solute dissolved fast Tared- a deduction from the gross weight of a substance and its container made in
allowance for the weight of the container; to determine; reduced to equal or standard
Catalyst- they are enzymes; positive catalyst will speed up the rate of chemical weight.
reaction while negative catalyst will slow down the rate of chemical reactions

Concentration- it will dissolved faster in a solvent LAB: STANDARDIZATION OF HCl (DIRECT TITRATION)
Materials: HCl, Anyhydrous Na2CO3, Methyl Orange (indicator)
= titrate with HCl solution to a salmon color end point.
*when you do standardization, you are performing to know the concentration of the Salmon color ~ pinkish-orange to light pink.
unknown. You will use the known for unknown so you will know its standard. *calculate the normality and molarity*

2 BUFFER SOLUTIONS: During standardization, hydrochloric acid is added to sodium carbonate.

Na2CO3 + HCl ---> NaCl + H2O + CO2
>weak acid mixed with salt of weak acid
>weak base mixed with a salt of weak base Calculation:
Given:
1. equivalent wt. Na2CO3~ 105.99 = 52.99g/mol
Neutralization- chemical process which an acid is make to react/ combined with basic 2. WT. SOLUTE Na2CO3= 0.450g
OH ion. 3. Volume of HCL consumed ~ 24.50mL = 0.245 liter to reach endpoint.

Normality= no. Of equivalent wt. Solute/ liter solution.

*acid have hydronium ion, base have hydroxyl ion.
N= wt. In grams solute
Example of Acid HCl: add sodium hydroxide ---> salt (NHCl)& water Equivalent wt. = M.W/ # rep. Salt/ liter solution
*NHCl- Ammonium Chloride, is the salt of ammonia and hydrogen chloride
N= 0.450g/ 52.99g equivalent/ 0.245 liter
What kind of acid can a neutralization be? = 0.0346g. eqv./liter
-reaction between strong acid and strong base
-” “ strong base and weak base Molarity = # of moles solute / volume solution in liter
-” “ strong base and weak acid = g solute / M.W solute/ liter solution
= 0.450g/105.99g/mol/ 0.245 liter
*but a reaction of weak base and weak acid don’t give a good results because they are =0.017 mol/liter
both weak.
Residual titration- used whenever direct titration is impossible. It is applicable to those
Eg. of Salt: sodium nitrate, magnesium sulfate, sodium chloride, potassium bitartrate, compounds which react too slowly with the titrant because of poor solubility.
monosodium glutamate.
Phenolphthalein- chemical compound with formula C20H14O4 often witten as HPh.
Excess acid in the body is not good, your internal body is already acidic so if you eat Indicator in an acid-base titrations. When it is acidic, it is colorless and when it is basic
acidic food, you can balance it back by taking basic medicines ( neutralize). take basic the color is light pink and purple if too high in PH level due to ionization
substance to destroy acid like the Antacid medicine.
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Sodium Hydroxide Pellets- a strong base and acid neutralizer also used in the CALCULATING THE % OF UNKNOWN (ASPIRIN):
staining procedure of cells.

Ionization- any process by which electrically neutral atoms or molecules are converted
to electrically charged atoms or molecules (ions). formed by gaining or losing electrons.
If gained electrons = negative charge (anion)
If loss electron = positive charged (cation)

LAB: PREPARATION IN STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION:

*titrate with sodium hydroxide, a light pink color as your endpoint*

Reaction Equation- final step to determine the computed molarity and normality of
sodium hydroxide solution.

LAB: ASSAY OF ASPIRIN ( RESIDUAL TITRATION)

* titrate the excess NaOH solution with std. HCl solution to the disappearance of the
pink color*
*perform blank determination*

*if the substance lighten, that means it achieved equilibrium.

*aspirin fail to react with sodium hydroxide ion because it is too slow that is why we add USUAL INDICATORS USED IN PRECIPITATION:
HCl do it would react to the excess sodium hydroxide ions thus there would be 1. Ferric ammonium sulfate test solution ( volhard method)
conversion of pink colored disappear that is the residual titration. 2. Potassium chromate test solution (mohr’s method)
*Aspirin is a weak acid. 3. Adsoprtion indicators such as (i) dichlorofluorescein t.s (ii) fosil t.s, (iii)
*The excess sodium hydroxide is now titrated with standard hydrochloric acid until all tetrabromophenolphthalein t.s (fajan’s method)
sodium hydroxide reacted with hydrochloric acid ions.
STANDARD SOLUTION USED IN PRECIPITATION: IF POTASSIUM
*The pink color will go back to colorless solution, that is what we called residual titration.
1. ) 0.1N Silver Nitrate Solution CHROMATE=
BLANK DETERMINATION- repeating the whole operation w/o the substance being 2. ) 0.1N Ammonium Thiocyanate Solution MOHR’S METHOD
analyzed. The difference between the titration represents the amount of NaOH required.
3 METHODS OF PRECIPITATION: IF SILVER NITRATE=
A blank titration is carried out by titrating a fixed and known concentration of titrant into
1. Volhard method VOLHARD METHOD
a solvent with zero analyte. The only difference from the regular titration is the absence
of analyte 2. Mohr’s method
3. Fajan’s method
DETERMINATION OF ENDPOINTS: (precipitation is about to form)
1. Cessation of precipitate or the appearance of turbidity. *AgNO3- silver nitrate, AgCl- silver chloride, NaCl- sodium chloride,
2. Use of internal indicators NaCl + AgCl = AgNO3
3. Instrument methods like use of potentiometer apparatus.
Precipitation reactions- when one mixed ions that form compounds that are insoluble,
PRECIPITATION- a reaction wherein soluble ions in separate solution when mixed a precipitate is formed.
together form an insoluble compound that settles out of the solution.

LAB: PREPARATION OF STANDARD SILVER NITRATE SOLUTION:
*volhard method used*
LAB: STANDARDIZATION OF POTASSIUM THIOCYANATE SOLUTION:
*volhard method used*
*titrate with potassium thiocyanate to a flesh brown color end point.
Potassium thiocyanate can be used in titration involving silver nitrate solutions,
chloride, bromide, and iodide indirectly by adding excess silver nitrate solution to the
sample containing halide, thus, halide are precipitated, and the excess silver nitrate are
titrated with potassium thiocyanate using ferric alum indicator (back titration)
A back titration is a titration method where the concentration of an analyte is
determined by reacting it with a known amount of excess reagent whereas a direct
titration directly measures the concentration of the unknown compound. The addition of
excess reagents is not done as in back titrations.
USING SILVER NITRATE SOLUTION, TWO REACTIONS WILL TAKE PLACE:
1st titration: AgNO3 + KSCN ---> AgACN precipitate + KNO3 + excess SCN
2nd titration: FeNH4 (SO4)2 + excess SCN ---> Fe (SCN)3 ppt. + K2SO4 + (NH4)2SO4
LAB: ASSAY OF MERCURIC OXIDE
*volhard method
*titrate with potassium thiocyanate to a flesh color endpoint
*titrant= silver nitrate (sodium chloride). sodium chloride is white in color.
Mercuric oxide- a yellow to orange precipitate, odorless, stable in air, discoloured
when expose to light, soluble in water.
Halides are compounds of Halogens, they consist of a halogen anion, also called a
halide ion and a cation. Hence, the name is given as halides.
e.g of HALIDES: sodium chloridem hydrogen, iodide, methyl chloride ,etc.
(HALIDES such as fluorine, chlorine, bromine, iodine)
After using Ferric Ammonium Sulfate T.S, the reaction will turn into brown precipitate
( ferric precipitation ion)
8
* add the AgNO3 (silver nitrate) with KSCN ( potassium thiocyanate) to precipitate silver
nitrate, resulting to AgSCN (white precipitated) many will precipitate. FeNH4 (SO4)2 +
Excess SCN ---> Fe(SCN)3ppt. + K2SO4+(NH4)2SO4
FENH4 also react with the excess SCN
*para maubos lahat ang unreacted silver nitrate na nag precipitate, we do residual
titration using the potassium thiocyanate pero after that nagkaroon na naman ng
bagong excess ito ay silver thiocyanate so the experiment is not yet complete, kaya
mag back titration again but using Ferric Ammonium Sulfate test solution.
FERRIC AMMONIUM SULFATE TEST SOLUTION HAS TWO PURPOSE:
> as an indicator
> as a reactant to react at the excess thiocyanate ions.
Potassium thiocyanate or (KSCN) ; abbreviation for precipitate= ppt
When you add silver nitrate to sodium chloride, it will produce to silver chlorite
precipitate (white in color) + sodium nitrate, you can see it in the erlenmeyer flask.
LAB: ASSAY OF AMMONIUM CHLORIDE:
*volhard method
*titrate the excess ferric ions with standard KSCN solution to the reddish brown
precipitate.
Rules in using indicator:
- 3 drops for titration unless otherwise directed
- when strong acid is titrated with strong alkali, use methyl red, methyl orange, or
phenolphthalein as the indicator.
- when weak acid is titrated with strong alkali, use only phenolphthalein.
- when weak alkali is titrated with strong acid, use only methyl red.
- a weak alkali should not be titrated with a weak acid or vice-versa since no indicator
will give sharp endpoint.
- the appearance of a color is more easily observable that the disappearance thus
always titrate when possible to the appearance of the color.
 9

Complexation- a reaction wherein metal ion combines with a molecule which van
donate electron resulting to a compound called complex.
Ligand- any atoms or molecules that binds with a central atom, usually a metallic
element to form a complex. Such reaction is called a complexation.
Sample problem: Calculate the present NaCl in the sample of 0.2182g NaCl assayed
by volhard using 50mL of 0.985 AgNO3 and 11.75mL of 0.1340N potassium
thiocyanate. Each mL of 0.1340N potassium thiocyanate. Each mL of 0.1N AgNO3 (0.1
mcg) which is consumed by NaCl is equivalent to 0.1 x 58,44 NaCl ~ 5.844/1000
=0.005844

If the combining molecules contain 2 or more group that can form several bonds to a
single metal ion, the term is called chelates.

*single- ligands
*double- chelates (read as kilets)

The earliest titrimetric applications involving metal ligand complexation, the use of APPLICATION OF PRECIPITATION:
monodentate ligand such as Cl- and CN-. however, limited the utility of complexation > Qualitative and quantitative
titration to those metals that formed only a single stable complex. The most widely used > more useful for antigen detection to as least as 1mcg.
of these new ligands was the Ethylenediaminetetraacetic Acid (EDTA) which forms > blood, seminal stains, food adulteration.
strong 1:1 complexes with many metal ions.

Ethylenediaminetetraacetic Acid (EDTA) is an amonocarboxylic acid. EDTA which is

a lewis acid has 6 binding sites ( the four carboxylate complex, in which EDTA forms a
cage-like structure around the metal ion is very stable) the actual number of
coordination sites depends on the size of the metal ion however all metal EDTA
complexes have a 1:1 stoichiometry.

LAB: ASSAY OF SODIUM CHLORIDE IN A DRIED FISH

*mohr’s method
*titrate with standard silver nitrate solution to the appearance of a brownish red color. LAB: STANDARDIZATION OF EDTA:
*fajan’s method
HOW TO SOLVE ITS ALIQUOT ( FROM DRIED FISH EXP) *add 5 drops of eriochrome black test indicator
Grams of solute use/ 250 mL * titrate with EDTA to the first appearance of a clear blue color.
E.g . if you use 2 g then, 2/250mL and x/50mL = 0.4mL
Non-hydroscopic means that it cannot moist in the atmosphere while hydroscopic tend
HOW TO CALCULATE % OF SODIUM CHLORIDE: to moist in the air. e.g. Salt is hydroscopic because when you left it uncover, it will moist.

Gram NaCl / gram of sample used in aliquot portion x 100 EDTA is not hydroscopic; it react to metal; it should br stored in a container that is
metal-free so we can avoid imperfect experimentation.
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PROPERTIES OF EDTA: 2 KINDS OF BUFFER SOLUTIONS:

1. Versatile chelating agents forming 4-6 bonds with single metal ion
2. Forms chelates with bond transition metal ion & main group ions.
3. React with metal ions forming a water-soluble, stable complex nor chelate compound,
4. Always combined with metal ions in 1:1 ratio
5. Rapid reaction and quantitative with polyvalent metal such as: Al+++, BI+++, Ca++,
Cu++, Hg++, Mg++, and Zn++
6. Monovalent metal ions yield relatively weak an unstable complexed
7. Organic solvents increases stability of the complex while neutral salt such as NaCl
decreases the stability.
1. Acidic buffer solution- has PH less than 7; commonly made from weak acid and
one of its salt often sodium salt. E.g.a mixture of ethanoic acid and sodium ethanoate. If
the solution contained the equal molar concentrations of both acid and the salt, it would
have a PH of 4.76
2. Alkaline buffer solution- has a PH level greater than 7, they are commonly made
from weak base and one of it is salt. E.g. a mixture of ammonia solution and ammonium
chloride. If they are mixed in equal molar proportions, the solution would have a PH of
9.25

USE OF EDTA: 2 TYPES OF WATER HARDNESS:

1. Soap & detergent since it forms calcium and magnesium ions. The hard water ions Temporal hardness- due to bicarbnate ion, HCO3-, being present in the water. It can
are bound to EDTA and cannot interfere with the cleaning action of soap or detergent. be removed by boiling the water to expel CO2 as indicated by the ff eq. :
2. They removed metal ions present in enzymes of food responsible for spoilage. HCO3……… H2O + CO2 (g)
3. Promote color retention in dried banana/beans, chick peas, etc.
4. Improves flavor retention in canned carbonated beverages Permanent hardness- due to the presence of the Ca++, Mg++. Fe++, and SO4-, it
5. It inhibits rancidity in salad spreads, sauces, etc. cannot be eliminated by boiling, and only through using chemical then it can be
*rancidity- having an unpleasant smell or taste usually from chemical change or eliminated.
decomposition.
THE DEGREE OF HARDNESS OF WATER IS CLASSIFIED IN TERMS OF ITS
GUIDELINES IN THE STANDARDIZATION OF EDTA: CALCIUM CARBONATE CONCENTRATIONS AS:
1. The disodium salt is preferred in preparing the standard solution of EDTA since it is HARDNESS RATING CONCENTRATION OF CONCENTRATION OF
more water soluble, non-hydroscopic and very stable. CALCIUM CARBONATE CALCIUM CARBONATE
2. The water to be used should be metal-free. Thus, a glass distilled water is preferred. (mg/L) (ppm)
3. Solutions are best in polyethylene containers or in an alkaline 2% solution of EDTA SOFT 0-60 0-60
to remove any metal MEDIUM HARD 61-120 61-120
HARD 121-180 121-180
*ammonium water is a buffer solution. Ammonium buffer resist change because it is
buffer solution. *parts per million (ppm)
This is an abbreviation for "parts per million" and it also can be expressed as milligrams
BUFFER SOLUTION- one which resist changes in PH when small quantities of an acid per liter (mg/L). This measurement is the mass of a chemical or contaminate per unit
or an alkali are added to it. volume of water.

WHY CONCERNED ABOUT HARDWATER? - hardwater is not a health hazard. People LAB: ASSAY OF AMMONIUM CHLORIDE:
regularly take calcium supplements. Drinking hardwater contribute a small amount of calcium *volhard method
and magnesium toward the total human dietary needs of calcium and magnesium.
*titrate the excess ferric ions with st. KSCN solution to the reddish brown precipitate.
 11

LAB: STANDARDIZATION OF EDTA:

*titrate with EDTA to the first appearance of a clear blue color.

The purpose of HCl will help neutralize calcium bicarbonate.

Why boil?- because it will yield a product of carbon dioxide, this product help affect the
reaction.

PROPERTIES OF HARDWATER:
1. It measures the capacity of the water when calcium ion binds with the soap causes
the formation of insoluble compound Ca+++ ions from water.
2. Has a high mineral content of cations with a charge of +2 like Ca++ and Mg++
3. Formed when water percolates (diffuses or penetrates) through the deposits of
limestones ( CaCO3 ) and chalk ( MgCO3).
4. Mineral deposits are formed by ionic reaction resulting to the formation of insoluble
precipitates. E.g. when hardwater is heated. Calcium ions react with bicarbonates
(HCO3 - ions) to form insoluble calcium carbonates.
Equation: Ca++ (aq) + 2HCO3- (aq) ……….. CaCO3 + 2H2O+ CO2
5. The solid deposits called scale coats the container where water is heated as the
deposits build-up, they reduced the efficiency of heat transfer so food may not be
cooked evenly and create a dramatic effect on the power bills.
LAB: DETERMINATION OF TOTAL HARDNESS IN WATER:
* titrate with the standard EDTA to the first appearance of a clear blue color.
*calculate the total hardness as ppm CaCO3
2 PROCESS ON HOW TO SOFTEN HARDWATER:
1. Ion-exchange process ( lime-soda process) - it removes calcium and magnesium
ions from the water supply resulting to the formation of insoluble precipitates. The water
is treated with a combination of slaked lime ( CaCOH)2) and soda ash (Na2CO3) to
form CaCO3 and MgCO3 precipitates. The solid can be collected, removing the scale
forming cations from the water supply.
2. Ion- exchange apparatus- hardwater is passed through an ion exchange apparatus
and the Ca++ ions from the tap water replace the Na+ ions placed in the other ion
exchange apparatus, thus water is softened, containing sodium ions in place of calcium
ions. Soft water is produced and collected for household use.
REDOX REACTION:
Oxidation- compound A; losses electrons
Reduction- compound B; gains electrons
 12

A combination of oxidizing and reducing agents results in a reaction which maybe used to ferric sulfate. Fe6+2 --> FE^+3 + e is 151.91g or 1 gram-molecular wt, BECAUSE:
as basis for the quantitative measurement of one of the reactants. Fe= 55.845; S= 32.065; O= 65; ~Total = 151.91

THE EQUIVALENT WEIGHT OF OXIDIZING AGENTS WHICH DETERMINE THE

CONCENTRATIONS OF STANDARD SOLUTIONS CAN BE CALCULATED AS:

The number of electrons gained by a given oxidizing agents sometimes depends on the
1. Permanganate ion to manganous ions- no indicator used since standard solution
conditions like: the pH of under the reaction is carried out.
used is colored) MnO4- +5e --> Mn^+2

OXIDATION-REDUCTION REACTION
*each molecula of KMNO4 gains 5 electrons when permanganate is reduced in acid
-this method if analysis involves in a change in valence based of Faraday’s Law. It says
media, 1/5 mol or 158.03/5= 31.61g. so a liter of 0.1N solution of KMNO4 should
that “in every oxidation-reduction reaction, the charge loss or gained by one substance
therefore contain 31.61g KMNO4 (KMNO4 MOLECULAR WEIGHT IS 158.03)
must necessarily be gained or loss by another substance.” There is always a transfer of
electrons in oxidation- reduction reaction.
2. Dichromate ion to chromous ion. Cr2O7^-2 - 6e --> 2Cr^+3

OXIDATION-REDUCTION METHOD IS DONE BY:

1/6 mole or 294.18/6 = 49.03g. 1 equivalent of potassium dichromate (k2Cr2O7)
1. Direct titration method
2. Indirect titration method (permanganate)
3. Bromate ion to bromide. BrO6-3 + 6e --> Br (in the presence of sulfurcis acid). 1/6
3. Residual titration method ( oxalic acid & permanganate)
mole, or 267.01/6= 27.83g is 1 equivalent pf potassium bromate (kBrO3)
4. Ceric Sulfate method ( ceric sulfate solution & dilute sulfuric acid) is a strong
4. Ceric ion to cerious ion. Ce^4 + e --> Ce^+3.
oxidizing agent and more stable than st. Permanganate solution provided sufficient
sulfuric acid is present to prevent hydrolysis and precipitation of the basic salts.
One more or 332.24g/1 is 1 equivalent of ceric sulfate Ce(So)2
5. iodimetric and iodometric method

5. Iodine ion to iodide ion. I2 + 2e --> 2l-

THEORIES:
Direct Combustion of the Elements- it is the simplest type of oxidation-reduction
One half mole or 1 gram- atomic weight, 123.90g is 1 equivalent of iodine. The
reaction. E.g. such as:
reduction of the iodine in potassium iodate to lower oxidation state varies, depending on
- the oxygen gas ignites with hydrogen gas to form water. O2 + H2-->2H2O (OXYGEN
the conditions specified for the variation assays in which solutions of potassium iodate
IS REDUCED AND HYDROGEN IS OXIDIZED)
are usually expressed in terms of molarity rather than molality. ‘
-when carbon burns in the presence of oxygen it forms carbon dioxide. C + O2 --> CO2
( CARBON IS OXIDIZED & OXYGEN IS REDUCED)
PROPERTIES OF STANDARDIZED POTASSIUM PERMANGANATE SOLUTION:
- when carbon unites with sulfur, it forms carbon sulfide. C+S--> CS2 ( CARBON IS
1. Easily standardized because reaction in solution is rapid
OXIDIZED & SULFUR IS REDUCED)
2. Can retain its concentration over a long period of time when proper precautions are
observed in its preparation and preservation.
The equivalent weight of a reducing agent is that which loses electron equivalent to
3. Use as indicator in titration where very slight excess of permanganate imparts to
96,500K and can be calculated by diving the gram-molecular weight by the number of
solution a distinct pink color.
electrons lost by each molecules. E.g. the equivalent weight of Ferrous sulfate oxidized

5 REDUCING AGENTS USED FOR THE PREPARATION OF STANDARD
SOLUTION ARE OXIDIZED:
1. Oxalate ion to carbon dioxide
2. Thiosulfate ion to tetrathionate
*The net oxidation number (valence number) of the four sulfur atoms in two thiosulfate
ions is 8+ while that of the 4 sulfur atoms in the tetrathionate ions must thiosulfate ion
losses one electron. So that one mole or 248.17g is 1 equivalent of sodium thiosulfate,
Na2S2O3•5H2O
3. Arsenite ion to arsenate ion
*arsenic trioxide is soluble with sodium pr potassium hydroxide and is represented by
the arsenite ion (ASO2-) which shows arsenic in the trivalent form. In a neutral or
alkaline medium, the arsenite ion is a reducing agent that gives up 2 electrons per atom
of arsenic. In acid medium, the reaction is reversed with the pentavalent arsenic in the
arsenate ion serves as an oxidizing agent.
4. Titanous ion titanic ion
*1 equivalent of thtanium thrichlordie, (TiCl3is 154.26g)
5. Ferrous ion to ferric ion
*1 equivalent of ferrous ammonium sulfate, Fe(NH4)2(SO4) • 6H2O is 1 gram
molecular weight or 392.14g
Asbestos is a naturally occurring fibrous silicate mineral. Fibrils released into the
atmosphere by abrasion & other processes. Asbestos is a group of minerals that occur
naturally as bundles of fibers. They are found in soil and rocks.
13
PREPARATION OR POTASSIUM PERMANGANATE SOLUTION:
1. Weigh around 1g of potassium permanganate
2. Dissolve in 300mL distilled water in a beaker
3. Cover with watch glass and boil the solution for 15 mins.
4. Allow to stand for 2 days
5. Filter through asbestos
6. Keep in amber colored bottle
7. Write the chemical equation of the reaction
Since the permanganate- oxalate reaction is run at elevated temperature, it is not
advisable to titrate permanganate directly with the standard oxalate solution. The
temperature at the conclusion of the filtration should not be less than 60 degree celcius.
The permanganate solution is slowly added fro a burette with constant stirring until a
pale pink color which persist for 15s. is produced.
PREPARATION OF OXALIC ACID SOLUTION:
1. Weigh roughly 1.6g oxalic acid
2. Dissolve in enough distilled water to make 259 mL
3. Store in an amber bottle
2 TYPES OF RESIDUAL TITRATION IN AN OFFICIAL ASSAYS OF POTASSIUM
PERMANGANATE SOLUTION:
1. Titration in which an excess of standard potassium permanganate solution
- is employed to oxidized a substance and the amount in excess is determined by
reduction with: (a) excess standard oxalic acid (b) excess ferrous ammonium sulfate
and back titration with mote standard potassium permanganate solution.
2. Titration in which an excess of standard oxalic acid solution
- is added to the substance and the excess oxalic acid is titrated with std. Potassium
permanganate solution,
LAB: STANDARDIZATION OF OXALIC ACID SOLUTION:
*titrate with potassium permanganate to slight pink end point which persists for 15s.

LAB: ASSAY OF SODIUM NITRITE:
*by residual titration where an excess potassium permanganate solution is employed to
oxidized a substance, and the amount in excess is determined by reduction with excess
standard oxalic acid and back titration with more of the standard potassium
permanganate.
*titrate with std. Potassium permanganate solution to a pink endpoint.
Chemical reaction:
1st reaction (rxn): 2NaNO2 + H2SO4 --> 2HnO2 + Na2SO4
2nd reaction: 6H ion + 5HNO2 + 2MnO4 ion --> 5HNO3+2Mn ion + 3H2O
3rd reaction: 16H ion + 2MnO4 ion + 5C2O4 ion --> 2Mn ion + 5CO2 + 8H2O
IODIMETRIC - IODOMETRIC METHODS OF OXIDATION-REDUCTION REACTION:
Iodimetry- a direct procedure of reversible reaction which can be applied in analysis of
reducing agents (analytes) like thiosulfate and arsenite using the standard solution of
iodine.
Properties of iodimetry: iodine is not soluble in water but dissolve readily in the
presence of Kl. There will be a formation of the free iodine (triiodine ion) in the solution.
For this reason, std. Iodine solution used in iodimetry are solutions of iodine in Kl
solution. Then the excess kl will be used as reducing agent in iodometry so that the
iodine formed will remain in the solution through its interaction with the potassium
iodide. l2 + kl --> kl3
Iodometry- an indirect procedure of reversible reaction (2l --> l2 + 2e) which can be
applied in analysis of oxidizing agents like: cupric salts, ferric salts, and available
chlorine. The presence of 1 part pf iodine in several million parts of solution is readily
detected using starch t.s. indicator solution.
Iodine imparts a distinct blue color at the end point. The starch solution deteriorate
quickly and must be prepared fresh each day.
Decantation is the process of separation of liquid from solid and other immiscible (non-
mixing) liquids, by removing the liquid layer at the top from the layer of solid or liquid
below.
14
In hot water, starch granules burst and form a colloidal B- amylose, known as the
soluble starch and should be separated by decantation from A- amylose (amylopectin)
which are insoluble. The interaction of iodine and iodine ion with colloidal B- amylose
will result in the production of an intensely blue colored solution, and this color change
is reversible, this is the color being discharged when iodine is reduced with sodium
thiosulfate or another reducing agent.
LAB: STANDARDIZATION OF IODINE:
*add 6N HCl until yellow color is change to pink
*titrate with iodine to a blue endpoint.
LAB: STANDARDIZATION OF SODIUM THIOSULFATE
*titrate with std. Iodine to blue color endpoint
*write the balance equation. Na2SO3 +l2 --> Na2S4O6 +2Nal
FATTY ACIDS- a carboxylic acid with a long aliphatic chain of carbon atoms which is
either saturated or unsaturated. They have unbranched chain of an even number of
carbon atoms from 4- 28.
Fats are in form of triglycerides. Fatty acids are derived from triglycerides which are
very important dietary sources of fuel not only in animals but as well as in plants, when
metabolized, they yield large quantities of ATP (Adenosine triphosphate) fatty acids are
released between meals from fat depots in adipose tissues, stored as glycerides.
Fats are triglycerides that are solid at room temperature; usually derived from animals;
mostly saturated fatty acids.
Oils are triglycerides that are liquid at room temperature; usually derived from plants or
fish; mostly unsaturated fatty acids.
What are the 3 types of triglycerides?
The three types of fatty acids that compose triglycerides are saturated,
monounsaturated and polyunsaturated fatty acids. From these three types of fatty
acids come the three types of triglycerides, or fats; saturated, monounsaturated and
polyunsaturated triglycerides.

WHY IS ALCOHOL ADDED TO KOH? - because alcohol is a suitable solvent to
dissolved the KOH.
TRIGLYCERIDES in human is called CHOLESTEROL & GLYCEROL in plants.
3 STRUCTURES OF TRIGLYCERIDES :
> FATTY ACIDS
 Volatile oild
 Waxy solid
 Fixed oil
e.g. sources of fatty acid: face, nuts, beans, edible oil, etc.
FATTY ACIDS:
1. Saturated - It is one of the unhealthy fats, along with trans fat. These fats are most
often solid at room temperature. Foods like butter, palm and coconut oils, cheese, and
red meat have high amounts of saturated fat; fatty acids without any double bonds
between the carbon atoms. General formula of R-COOH. The R-group is a straight
chain hydrocarbon of the form CH3(cH2)n with varying lengths from short chained
(volatile oil), 30 94 more (waxy solid) and from 12-22 for most common and important
fatty acids from plants and animals.
 Laluric acid, myristic acid, palmitic acid, stearic acid.
2. Unsaturated fats- which are liquid at room temperature, are considered beneficial
fats because they can improve blood cholesterol levels, ease inflammation, stabilize
heart rhythms, and play a number of other beneficial roles; found in the cell membrane
as components of the phospholipids to help maintain the membrane fluidity and cannot
be synthesized in the body. They are those that has atleast one double bond in the
carbon chain usually found in plants and nut oils.
 Monounsaturated fats- oleic acid (omega-9)
 Polyunsaturated- omega-6 ( linoleic acid, CLA, GLS, Arachidonic acid) ; omega-3
(linolenic acid, EPA, DHA)
Omega- good fats needed by our body.
15
Carboxylic acid is an organic compound containing a carboxyl functional group, they
occur widely in nature and are also synthetically manufactured by humans. Upon
deprotonation, carboxylic acid yield a carboxylate anion with the general formula
R-COOH-, which can form a variety of a useful salt such as soaps.
NOMENCLATURE:
e.g. omega 3- the double bond is located on the 3rd carbon atom
Omega 6- the double bond is located on the 6th carbon atom.
GRAVITATIONAL ANALYSIS:
- a set of methods used in analytical chemistry for quantitative determination of an
analyte based on its mass.
Acid Value (neutralization number or acid number or acidity):
- mass of potassium hydroxide in mg required to neutralized one gram of chemical
substances being analyzed (sample)
- measure of the amount of carboxylic acid groups in a chemical compound such as
fatty acids or mixture of a compound. A known sample is dissolved in organic solvent
(usually isopropanol) and use phenolphthalein as the indicator, titrated with a solution of
potassium hydroxide with known concentration.
- used to quantify the amount of acid present in a sample
- it is the quantity of base expressed in mg of KOH required to neutralize the acidic
constituents in 1g sample.
Rosin- oxi substance
Meg- milliequivalent if expressed in mL, if expressed in Liter they equivalent.
Substances like balsam and resin are mixed with alcohol and ether to dissolve the
coloring matters that might interfere with the observation of the endpoint when an alkali
is added.
Solid fats (waxes)- usually melted on a water bath and titrated while hot.
 16

e.g. probem: find the acid value of rosin weighing 1.1g which required 28mL of 0.110N
NaOH to bring about the endpoint (light pink color).

Step 1: DETERMINE THE mcg OF NaOH CONSUMED BY THE SAMPLE.

28mLL X 0.11ON = 3.080 meg
Step 2: MULTIPLY 3.080 meg BY 56.11g/mol KOH = 0.0173 mg of KOH REQUIRED
TO NEUTRALIZED THE FATTY ACIDS IN 1.1g ROSIN SAMPLE.
Step 3: DIVIDE THE SAMPLE WEIGHT INTO mg OF KOH IN ORDER TO FIND THE
mg OF KOH REQUIRED TO NEUTRALIZE THE FATTY ACIDS IN EXACTLY A GRAM
OF SAMPLE. 0.01728mg/1.1g = 0.1571 mg/1 g SAMPLE
Step 4: COMBINING ALL THE MATHEMATICAL OPERATIONS (steps 1,2,3)
Acid Value of Rosin = 28mL x 0.11N X 0,0561mg/meg 1.571
1.1g sample = 1.1g sample = 1.43mg/1g
Rosin sample
Step 5: COMPARE THIS VALUE WITH THE TRUE VALUE RANGE FOR ROSIN AND
DETERMINE WHETHER IT CONFORMS OR NOT, THE DECIDE OR NOT. THEN
DECIDE OR GIVE YOUR DISPOSITION. WHETHER IS IT PURE OR INFERIOR OR
ADULTERATED? ~ according to the range table, this rosin oil is not pure because it
Substances like balsam and resins are mixed with alcohol and ether to dissolve the
has wide range gap , therefore, what we are determining (rosin) is a fake rosin oil
coloring of the endpoint when an alkali is added
(refers to the table)

Solid fats (waxes) are usually melted on a water bath and titrated while hot,
SUBSTANCE OFFICIAL REQUIREMENT; ACID
VALUE
The presence of free acids in oils, fats, and waxes is due to the hydrolysis of the
USP ff:
CARNAUBA WAX 2-7 1. The esters decomposing them
OLEIC OIL 196-201 2. Chemical treatment
SODIUM STEARATE 196-211 3. Bacterial action
STORAX, AMERICAN 36-85 4. Catalytic action of light and heat
STORAX, LEVANT 50-85
TOLU BALSAM 112-168 *as a rule, fresh & recently prepared fatty substances contain little or no free acids.
ROSIN 160-180 Upon aging, the acid value increases slowly at first and rapidly later if the substances is
WHITE WAX 17-24 not well protected fro, the simultaneous action of light and heat.
NF
SYNTHETICSPERMACETI </ -5
YELLOW WAX 18-24

This acid value use to identify whether they are inferior or adulterated.
 17

The value of substances like fats, oil, and waxes are based upon their content of free
acids. e.g. Tolu balsam value is required to be not less than 112 and not more than 168.
an acid value less than 112 indicates that the acid content of Tolu balsam is low and
that it is inferior quality and must be therefore adulterated. On the other hand, acid
value greater than 168 indicates adulteration with substances having high acid value.
Adulteration- the act of making something impure or altering its original form by adding
materials or elements that aren't usually part of it; any material which is or could be
employed for making the food unsafe or sub-standard or containing extraneous matter.

SAPONIFICATION:
- is the addition of an acid to a base resulting to be a salt.
Acid (oil) + Base (lye) = Salt (soap)

Saponification value- the amount of base required to neutralize the free acids and
saponify the ester that is contained in 1g fat sample.

LAB: SAPONIFICATION VALUE DETERMINATION:

*add 1ml phenolphthalein and titrate the exces KOH with std. HCl solution
*perform blank determination

GENERAL EQUATION:
1. RCOOH + KOH --> RCOOK + HOH (acid value)
2. RCOOR + KOH --> RCOOK + ROH (saponification value)
Excess KOH + HCl --> KCl + HOH

SAMPLE PROBLEM: calculate the saponification value of cotton seed oil sample used
in the experiment, if a 1.532g sample is refluxed with 20mL of about 0.5100N alcoholic
KOH, required 15.70 mL of 0.5100N HCl for the residual titration, the blank was run
using the same volume of 0.5100N alcoholic KOH and required 26mL of 0.5100N HCl
to bring about the endpoint.