550-7000C Diluted HCl

(TOTAL INORGANIC SALTS)

(SILICA)

Weigh accurately 10g of drug

Dry in an oven at 1050C for 5 hours

Cool to room temperature Weigh until constant weight

wt. before wt. after % Moisture = ---------------------------- x 100 wt. of sample

loss on drying % Moisture = ------------------ x 100 wt. of sample

(wt. before wt. after) wt. of ether-soluble extractives % Moisture = -------------------------------------------------------- x 100 wt. of sample

volume of water in mL % Moisture = ----------------------------- x 100 wt. of sample


Place methanol in flask

Titrate with KF reagent until endpoint (canary yellow) Add weighed

Titrate with KF reagent to final endpoint

F=

F=

F=

weight of water % Moisture = ----------------------------- x 100 wt. of sample

F=

F x mL of KF reagent % Moisture = ------------------------------ x 100 wt. of sample in mg

spontaneous evaporation oven-drying


Macerate 2g of drug in 70mL diluted alcohol Shake mixture during 8hrs at 30-minute interval
Stand for 16hrs without shaking

Dry to constant weight at 1000C in oven

Evaporate 50-mL aliquot portion filtrate to dryness in water bath

Filter and wash residue to make 100-mL filtrate

Treat accurately weighed sample in ether Treatment with boiling acid Treatment with boiling alkali

Dry residue and weigh

Weigh residue and incinerate using dull red heat

Filter through ashless filter paper

Weigh accurately 5g of oil or fat

Add alc.KOH and heat under reflux condenser

Evaporate alcohol and dissolve residue in water, then extract with ether

Dry the residue and weigh until constant weight

weight of residue % Unsaponifiable = --------------------------- x 100 Matter wt. of sample

Weigh accurately 200 mg of oil sample

Add 20mL of CCl4, then 25.0mL of ICl

Stopper, shake occasionally and stand for 30mins protected from light

Perform blank test

Titrate liberated I2 with std. Na2S2O3 to disappearance of blue color

Add 20mL KI and 100mL recently boiled & cooled water

Weigh accurately 2g of fatty alcohol sample

Add 2.0mL of pyridine and 10mL of toluene

Add 10.0mL of CH3COCl, then stopper flask and heat in water bath for 20mins.

Perform blank test

Titrate CH3COOH formed with std. NaOH to light pink color using Pp as indicator

Add 25mL distilled water, stopper and shake vigorously, then allow to stand


Oil Sample (free alcohol + alcohol as ester) acetylation Oil Sample (alcohols in ester form) saponification Determine SV of acetylized product

Pipet oil sample into an EF

Run down 50.0mL of Hydroxylamine HCl

Stand for 10mins., then add indicator

Titrate with std. NaOH to endpoint

Perform blank test

Pipet spirit into an EF

Add 1mL kerosene

Add acidified saturated CaCl2 solution and rotate bottle vigorously

Add sufficient CaCl2 soln to bring oil to neck

Take the reading


weight of residue % Alkaloid = --------------------------- x 100 wt. of sample

* Indicator used is methyl red.

TYPES OF ANALYSIS
1. Proximate analysis - determination of the amount of a class of compound present in given sample Example: alkaloids 2. Ultimate analysis - determination of the amount of a specific component of the given sample Example: morphine