Finals

Gravimetric Method
Assay of Sodium Lauryl Sulfate for Sodium Content
Special Method
Acid Value Determination of Cooking Oil
Saponification Value of Cooking Oil
Assay of Phenol Content of Clove Oil
Assay of Caffeine Content of Instant Coffee
Powder

Gravimetric Analysis
Assay of Sodium Lauryl Sulfate Content
Ex 23
Compiled by Danielle Co
Gravimetric analysis
The principle behind gravimetric analysis is
that the mass of an ion in a pure compound
can be determined and then used to find the
mass percent of the same ion in a known
quantity of an impure compound
quantitative methods that are based on
determining the mass of a pure compound to
which the analyte is chemically related
Classifications of Gravimetric methods
, the analyte is
separated from a solution of the sample as a
precipitate and is converted to a compound
of known composition that can be weighed
, the analyte is
separated from other constituents of a
sample by conversion to a gas of known
chemical composition. The weight of this gas
then serves as a measure of the analyte
concentration.
, the analyte is
separated by deposition on an electrode by
an electrical current. The mass of this
product then provides a measure of the
analyte concentration.



Classifications of Gravimetric methods
Traditional Method.
Cheap, easily available apparatus, simple to
carry out.
Slow, especially when accurate results are
required.
Wide range of sample concentrations (ng - kg).
No calibration required (except for the
balance).
Accurate
the analyte is converted to a sparingly soluble
precipitate. This precipitate is then filtered,
washed free of impurities, converted to a
product of known composition by suitable
heat treatment, and weighed
1. Preparation of the solution
2. Digestion
3. Precipitation
4. Digestion
5. Filtration
6. Washing
7. Drying or igniting
8. Weighing
9. Calculation
Properties of Precipitating Agent:
Should react specifically or selectively with
the analyte
Specific precipitating agent
rare, react only with a single chemical species
Selective precipitating agent
more common, react with a limited number of
species
Properties of Good Precipitate:
Easily filtered and washed free of
contaminants.
Of sufficiently low solubility that no significant
loss of the analyte occurs during filtration and
washing.
Unreactive with constituents of the
atmosphere
Of known chemical composition after it is
dried or, if necessary, ignited.
Use in making shampoos, toothpastes,
mouthwashes, bodywash, soaps, detergents
and body wash
Side effects: Hair loss, skin & eye irritation,
cancer
Na
2
SO
4
+ BaCl
2
2H
2
O BaSO
4
+ 2 NaCl
+ 2 H
2
O
Wt of ppt obtained the one that we obtained after
drying inside the oven
MW of anlayte MW of the chemical that is sought
MW of ppt MW of the chemical being dried &
weighed
Ex 24
Determining the degradation of oil products
Acid Value/Acid Number/Acidity Index
the weight of KOH in mg needed to neutralize
the organic acids present in 1g of fat and it is a
measure of the free fatty acids (FFA) present
in the fat or oil
0.5 N , 0.1 N , 0.02 N
alkali
Oil sample and
phenolphthalein
1. Determines the age of the oil (Rancidity)
Presence of free fatty acids
An increment in the amount of FFA in a sample of
oil or fat indicates hydrolysis of triglycerides
Chemical treatment
Catalytic action of light & heat (High temperature and
relative humidity during storage)






Usually the causes are enzymes (lipases)
and microorganisms (lipases-producing,
like Candida albicans). Lipases are enzymes,
which break down fats into monoglycerides
(digest fats).
For Saturated Fatty Acids (butter, coconut)
Rancidity gives off flavorful smell (tasty
smell)
Microorganisms
Tissue from which the oil or fat was
extracted
FREE RADICALS
(MUTAGENIC & CARCINOGENIC)
Rancidity
- oxygen damages foods
Oxygen molecules interact with the structure of
the oil and damage its natural structure in a way
that can change its odor, its taste, and its safety
for consumption
For Mono & Polyunsaturated Fatty acids
off-flavors and odors due to the formation of
peroxides, carbonyls, aldehydes, trienes


2. Determination of Adulterants
3. Used to monitor the quality of the oil and
prevent problems caused by degradation.

If stored in light, clear bottles, in tins with a
large air bubble at the top, at higher storage
temperature or at direct sunlight
During cooking, especially if it is highly
unsaturated. The higher the temperature (like
in frying), the faster it oxidizes
During storage, if attacked by lipase-producing
bacteria and microorganisms
If passed trough machines or vessels, made of
or containing iron

Is rancid oil bad for your health?
I experience a Bleeding
Liver , Necrotic liver
My kidney is damaged
and I over eat!

store cooking oils in dark or covered/wrapped
bottles away from direct sunlight, or in metal tins
with the oil nearing the top of the tin
store cooking oils in cool and dark places best
refrigerated (keep in mind that highly
monounsaturated oils, like olive oil will become
semi-solid at low temperatures)
use lower cooking temperatures (with the right
cooking oils below) and DO NOT reuse oils for
cooking or frying!
in commercial applications, with the use of natural
(polyphenols, ascorbic acid, mixed tocopherols) or
synthetic antioxidants, added to oils

What oils should you use for cooking?
The best oils for cooking are those that are highly
saturated or primarily monounsaturated in this
order:
coconut oil (warning: low smoke point use lower
cooking temperatures)
butter, organic (or ghee clarified butter)
palm oil
lard
extra-light olive oil
pomace oil
extra-virgin olive oil (lower smoke point)

Formula for Acid value
mgKOH/meqKOH is 56.11


Saponification Value of Cooking
Oil
Ex 26
Saponification
a process that produces soap, usually from
fats and lye
involves base (usually sodium
hydroxide commonly called caustic
soda NaOH) hydrolysis of triglycerides, which
are esters of fatty acids, to form the
sodium salt of a carboxylate
the number of milligrams
of potassium hydroxide required
to saponify 1g of fat under the
conditions specified
Saponification Value
Saponification Number
Koettsdorfer Number
Sap Value
Saponification Value interpretation

Less
soapiness
More
soapiness
Good soap
Substance present in
oils or fat that are not
saponified by alkali
hydroxides but are
soluble in ordinary fat
solvents
Fail to form soap

Saponifable
Matters
Unsaponifiable
Matters
Saponification equation