Phan1 Part2

Front 1

is based on the measurement of intensity of the light emitted when a metal is introduced into a flame.

Back 1

Flame emission:

Front 2

Is an analytical technique involves the study of the absorption of radiation by neutral atoms in gaseous state

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AAS

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Measures excess energy by emission/fluorescence

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Fluorometry

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Measurement of transmitted light (light that crosses 180 degree

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Turbidimetry

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Measurement of reflected light (light that crosses 90 degree)

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Nephelomety

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Absorption measurement is made in visible spectrum

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Colorimetry

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Rotation of spinning nucleus when magnetic field is applied

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NMR

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Bombardment of molecules causing cracking and fragmentation

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Mass spectroscop

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Structure and identification (ID)

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IR (infrared spectroscopy)

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Structure and ID/ analysis of trace volatile substances. Quantitative

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MS (mass spectroscopy

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Trace analysis of metals

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UV/Vis (visible spectroscopy

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Qualitative/ semi-quantitative, trace metal analysis

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AAS

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UV

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220 – 380

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Visible

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380 – 780 nm

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Near IR

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780 – 3000 nm

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Medium

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3.0 – 15 um

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Far IR

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15 – 300 um

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Group frequency region

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3-8 um (group of constituents

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Finger print region

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8-15 um (specific compound or functional group)

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-radiation of single wavelength - 0.5-10 nm is the usual specrtal region that approximates monochromatic radiation

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Monochromatic radiation

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distance between two atoms increases or decrease

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Stretching

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IR radiation causes the excitation of the vibrations of covalent bonds within that molecule. These vibrations include the stretching and bending modes

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MOLECULAR VIBRATION

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position of the atom changes relative to the original bond axis

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Bending (deformation

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info about the analyte is derived from the measurement of current (flow of electricity)

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VOLTAMMETRY

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it is a method of analysis based on the measurement of current resulting from the electrolysis of an electroactive species at a given electrode potential under controlled conditions

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POLAROGRAPHY

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study and measurement of electrode potential

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Potentiometry

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develops a potential that varies according to the activity (concentration) of hydrogen ions of the specific component in the solution

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Indicating electrodes

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is a process in which a solution of mixture containing inert materials, drug principles and impurities is separated into its components while moving through a bed of fixed porous solid having different and reversible affinities for the substance being separated.

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CHROMATOGRAPHIC METHOD

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– a fixed bed core of large surface area

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Stationary phase

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liquid, mixture or gas (solvent)o a fluid w/c moves through or over the surfaceof the stationary phase.

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Mobile phase

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stationary phase is non-polar, mobile phase is polar

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Reversed phase chromatograph

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The simplest type of chromatographic column Consists of a separation flask and a cylindrical glass tube constricted at one end

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Column chroma

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Cellulose of the filter paper is used as adsorbent

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Paper chromatography

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Follow the same principle as PC Most distinct result most precise

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Thin layer chrom

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When the compounds are radioactive, their position on the column may be determined by the use of a

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GEIGER MUELLER COUNTER

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Bromocresol Green

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-Yellow Spot

-Acid

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2,4 dinitrophenylhydrazine

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Yellow/Red Spot-

Aldehydes-Ketones

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Ninhydrin

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Flourescent

Amino Acids,

Amines

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Mercuric nitrate

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-Yellow Brown Spots-

- Alkaloids

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Bromothymol Blue

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-Light Green Spots

- lipids

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Aniline phthalate

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Gray Black Spots

Carbohydrates

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-liquid-liquid chroma - Difference in solubilit

Ex: paper chroma

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Partition chroma

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-liquid-solid chroma - Because mobile phase liquid and sationary phase solid

-Ex: TLC

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Adsorption chroma

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Based on molecular weight

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Molecular exclusion/ gel filtration chroma

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Based on charge; both contains beads

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Ion exchange

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inert gas (carbon, hydrogen, hellium, argon, nitrogen) analysis of volatile compounds

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Gas Chroma

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is defined as the time required by an average molecule of component to pass from the injection point through the column to the detector

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Retention time (tR)

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is defined as the volume of carrier gas necessary to carry an average molecule of the component from the point of injection to the detector

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Retention volume (vR)

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Best chromatogrpahic method because it containes all four principles

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HPLC

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Filter paper

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PC

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thin layer made up of silica gel

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TLC

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solid embedded in the colum

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CC

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liquid surfaces

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GC

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solid

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HPLc

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Adsorption

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CC TLC GC

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Partition

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PC

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Adsorption, partition, ion exchange and molecular exclusion

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HPLC

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-Measure of gas liberated or removed under the conditions described by the assay

-Uses nitrometer (commonly used the nitrogen content )

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Gasometric assaY

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4 types of volatile oils

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-specific gravity

-Specific assay

-Polarization

-Refractive index

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- Measures optical activity (levo and dextro)

-Using polarimeter

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Polarization

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bending of light passing from one medium to another

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Refraction

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ratio of velocity of light in air to velocity of light in medium

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Index of refraction

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-Ester value

-Amount of alcohol (acetylization flask ) -Determination of aldehydes and keton

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Specific assay

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- using cassia flask

-most common method in determining the aldehyde content of the sample

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BISULFITE METHOD

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-only use if there is a small/little amount of aldehyde and ketone in the sample. - assay of phenol content with NaOH

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HYDROXYLAMINE METHOD

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Acid -base

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Glass

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Potentiometric

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Ag ( silver)

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Chelometric

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Hg2 -Hg2

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Reduction - Oxidation

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Platinum

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value or number of physical and chemical properties.

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Constant

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compounds consisting of fatty acids combined with glycerol via ester linkages.

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Fats

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contain relatively high quantities of liquid glycerides

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Fixed oils

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making the fixed oils liquids-found in plants

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Glyceryl oleate

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solid consistency of fats- found in animals

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glyceryl stearate

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esters (RCOOR) of high molecular weight monohydric alcohols and high molecular weight fatty acids.

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Waxes

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substances containing benzoic or cinnamic acids

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Balsams

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are natural or induced solid or semi-solid exudates from plants characterized by being insoluble in water, soluble in alcohol and ether, crystallizable and softening or melting at a moderate heat

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Resins

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- # of mg of KOH (solvent of fats and fixed oils) required to neutralize the free acids in 1g of substance

- it may be expressed as the number of milliliters of 0.1N sodium hydroxide required to neutralize the free acids in 10 grams of sample

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Acid value

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# of mg of KOH required to saponify the esters on 1g of the substance

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Ester value

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-# of mg KOH required to neutralize the free acids and saponify the ester in 1g of substance - also known as, “Koettsdorfer number”

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Saponification Value (AV + EV)

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# of mg of KOH equivalent to the OH content of 1g of the substance

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Hydroxyl Value

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-# of g of iodine absorbed by 100g of a substance

- used to determine whether the substance or fixed oils would be drying, semi- drying or non-drying

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Iodine value

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Drying

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>120- linseed, cod (components of paint.

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Semi-drying

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100-120

-Cocopese

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Non-drying (OlAlangutan)

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<100

olive, almond (good cooking oil

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Present in oils/fats that are not saponified by alkali OH but soluble in ordinary fat solvents

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Unsaponifiable matter

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vegetable origin

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Phytosterol

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animal origin

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Cholesterol

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present in fungi

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Ergosterol

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Very Dull Red Heat

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500C-550C

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Dull Red Heat

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550C-700C

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Bright Red Heat

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800C- 1000C

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Yellow, Red Heat

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1000C-1200C

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White Heat

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1200C- 1600C

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part of total ash not soluble in 3N HCl (content: silica)

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Acid insoluble ash

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represents sol. chlorides, alkali, and nh4 salts

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Water soluble ash

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treated with H2SO4 (sulfuric acid

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Sulfurated ash

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-determination of ash content: igniting the sx in to dull redness (550-700C)

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Residue on ignition

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% of test material that is volatilized and driven off at 800+/- 25degC

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Loss on ignition

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amount of volatile matter that is driven off at 110-120 deg.c

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Loss on Drying

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-800±25c

-if so, additional 15 min. ignition period

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Ignite to constant weight

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-110-120c

-if so, additional hour ignition period

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Drying to constant weight

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with very low water concentration

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Dew point method

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with extremely low water conc

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Electrolytic method

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complete burning, no access to air

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Incineration

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start burning, access to air

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Ignition

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no access to air, decomposition process

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Carbonization

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❖ Xylene and toluene ❖ Yields 2-4 ml of moisture ❖ Uses toluene moisture apparatus

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Method II: Azeotropic/ Distillation

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❖ Methods of choice for 1-2g of sample ❖ Vegetable drugs (10g) dried for 5 hrs ❖ Biologics

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Method III: Gravimetric/Drying/Thermal

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prevent the pyridine and sulfur complex

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Anhydrous methanol

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prevent the reverse of the reaction with water; binds with sulfur that interferes the endpoint in titration

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Pyridine

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for nitrogen determination

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KJELDAHL METHOD