-a procedure by which solutes are separated by differential migration process in asystem consisting of 2 or more phases components: *stationary *moobile *solute

the aximum height of a wave

AKA stochiometric point -theoritical point at which equivalent amounts of the analyte and titrant have reached -N1V1=N2V2 or M1V1=M2V2 (molarity is used when the stochiometric point between titrant and titrand is 1:1)

single chemical species (specific components) *eg: total caffaine content in coffee beans

-closeness of TWO OR MORE actual measurements obtained in exactly the same way -describes the REPRODUCIBILITY of measurement *overage deviation *standard deviation *coefficiennt of variation or range

endpoint in volhard

fajans titration

total of class of plant principles (group of compounds) *e.g: total alkaloidal compound in coffee beans

-selected or trace compounds

measurement of reflected light in a suspension

*SP:solid adsorbent spread thinly on a glass or plstice plate -ex: silica gel, alumina caco3 *MP: organic solvent which is less polar that the SP -ex: hexane, ethyl acetate

overage or arithmetic ____ -obtainedby dividing the sum of replicate measurements by the number of measurements in the set

endpoint in mohr

AKA: reaction capacity values * number of reacting entities per reagent

the disance between two identical adjacent point in a wave

indicator used in mohr

transmittance decreases exponentially as the thickess of the solution increases arithmethically

*VS: EDTA *1st std: caco3 indicators: *eriochrome back T (EBT)-mg, zn *hydroxynahthol blue (hnb)- ca *dithiozone (dt)- al, bi example assay: -direct: zno, bi content of glycobiarsol (in all EDTA complexation reaction, ratio of EDTA to metal is 1:1 [EDTA]= molarity

*energy is directly prportinal to frequency *energy is inversely proportionl to wavelength e=hv

if RF is high= non polar if RF is low= polar

-isolates the restricted region of spectrum *filters- dedicated to a single band of wavelength *monochromators- designed for special scaning (ex: prisms, gratings)

bisulfite method (cassia flask) or hydroxyllamine method (titration)

measurement of an acid by a standard base

-AKA volumetric analysis +method in wwhich the volume of a solution of KNOWN concentration during anlysis is taken as the AMOUNT of ACTIVE constituent in the sample

primary std used in fajans

*VS: KMNO4 *1st std: na2c2o4 *indicator: non (sef indicating) *endpoint: slight pink example assay -direct:h4o2 -indirect: malic acid contect of cherry juice -residual (oxalic acid-back titrant): kno4, nano2, kmno4

-substance of HIGH DEGREE -serves as a REFERENCE MATERIAL (standard) in titrations -used in direct standardization purposes

the time required for one cycle to pass a fixed point in waves

-fixed bed of large surface area --may be aporous orfinely divided solid or a liquid that has been coated in a thin layer of an inert suppoertingmateria -particles should be as small and homogenous as possible

the number of cycles which pass a fixed point in space per secnd

*for crude drugs -proximate -ultimate *for chemical drugs -proximate -complete

vs used in fajans

for analysis of gaeous ions

2 titrants -AKA bak titration *1st VS added in EXCESS; 2nd VS used to titrate the excess (unreacted) 1st VS (bak titrant) indications: insoluble sample, volatile sample resection too slow, it does not give a sharp endpoint

-for correction -to enhance the reliability of the endpoint

-based on partition between 2 immiscible solvents -both SP and Mp are in liquid form

*CLOSENESS of an ACTUAL value to the THEORITICAL (true) value and is expressed by error - measures agreement between result and accepted value *absolute error *relative error

determination of a metal in the presence of anothe metal masking agents: *triethanolamines: fe, mn, al *thioglycols: hg, cu, pb, bi **cyanide: cu, co, ni, zn *flourine: ca, mg, al

*VS:ce(so4)2 *1st std: as2o3, fe filling(old) *indicator: o-phennatrolin endpoint: red to blue example assay: -direct: feso4, feso4 tab, hydroquinone, menadione

used to separate compund from mixture -SP: solid adsorbent packed in a vertical glass column *ex: silica gel, aluminacaco3 -MP: organic slvent aded to the top and flows down through the column -ex: hexane, ethyl silicate

-geenrates beam of radiation *continuum sources (ex: deuterium lamp, tungsten lamp,nernst glower) *line sources (ex; hollow cathode)

- fluid that moves through or over the surface of the stationary phase -maybe liquid or gas

point with the maximum downward displacement

based on the determination of retention factors

indicator in volhard

-coponents must be in solution or vapor state -the relative affinity of the solutes for each of the phases must be reversible

-since the speed of light in a vacuum is constant, there is an inverse relationship between wavelength and frequency *the higer the frequency, the shorter the wavelength *the longer the wavelength,, the lower the frequency

what special methods are used for natural products?

reagents of known concentration -AKA volumetric/standard solution

holds the sample to be analyzed *quartz cuvette- UV or visible region *silicate glass or plastic cell- visible region *nacla or k

the numer of cycles per unit distance

-widely usd and preffered currect assay of biological and pharmaceutical product -SP: clumn packed with glass or plastic beads coated with silicone derivatized with non polar functional group

what is used in instrumental method for natural products?

-middle result when replicate data are arranged in increasing or decreaing order -less affected by extreme values (outliers)

volhard titration

*AKA intermediate error -due to UNCONTROLLED variables -variations in a series of observations (by the same observer under identical condition) -AFFECT MEASURE PROPORTION

compounds capabl of changing colors near the end

-molecules are separated according to their site by their ability to penetrate a seive-like structure -ex: size exlusion chromatography

mohr titration

-chemical compound reagents -physical boiling point, melting point, optical purity, refractive index *biological potency or effectivness of drugs: animal models; microbial assay- antibiotics

en dpoint in fajans

utilized, highly specific interactions between one kind of solute moleculeand a second molecule covalently attached to the SP ex: protein affinity chromatography

-SP: water molecules bound to the cellulose of the filter paper -MP: non polar or hydrophobic solvents

1 titrant

functional group that absorbs maximum radiation in the uv or visible regions

-AKA analyte/active constituents *sample being analyzed

standard solutions whose purity has been determined by chemical analysis -used in INDIRECT standardization process

-converts radiant energy to a usable elecrical signal *phototubes *photoomultipliers *photoiodides (more sensitive)

transmittance decrase exponentially as the concentration of the solution increases arithmethically

--chemical or general methods: titration, gravimetry --instrumental methods: UV-Vis, IR, MS, chromatography --special methods: ash content, water content, constants for fats and fixed oils

actual point aquivalent amounts of the analyte and titrand have reacted *point where a physical change occurthat is associated with the condition of chemmical equivalence

-used to analyze volatile substances *SP: either a solid adsorbent or liquid ion in inert support *MP: chemically inert carrier gas (helium or nitrogen)

*occurs occasionally; are often large, and may cause result to be either high or low *OFTEN A PRODUCT OF HUMAN ERROR

acetalization method (peppermint- total menthol content))

- a form of energy that has both wave and particle properties -described by means of a classical sinusoidal wave model

assay for RA: I2+RA --2I-VS:I2 *first std: arsenic o3 *indicator: starch (appearance of blue) sample assay:: -direct: vit.C -residual: nahso3, methionine

for determination of functional groups

vs used in mohr

-used for the separation of charged molecule their bindings to fixed charges on a support uses: *most effective method for water purification *separation of amino acid *SP: employs either cationic or anionic exchanger which is capable of exchanging counter ions in the surrounding medim in reversible process

primary std used in mohr

-indicates the amount of each substance in the sample -exact amount or proportion of components expressed in 1% purity and compared to official compendia -e.g: gravimetric, volumetric, physichochemical and special methods of analysis.

assay for OA: rxn: 2I-+OA(sx)--I2 I2 +2S2O32- -- 2I-+s4o62- *VS: nas2o3 *1st std: k2cr2o2 *indicator: starch (disappearance of blue) example assay: -direct: cuso4, naocl -residual: phenol, resorcinol,thyroid hormones, ses2

point with the maximum upward displacement

fnctional group which does not give rise to a bsorption band by itself, but upon being attracted to a chromophore

*measurement of base by a standard acid indicators (aquaeous)- uses water as solvent SA+SB= phenolphthalein, methyl orange/red (non aquaeous)-non polar very week acid/base

for quantitative and qualitative analysis

displays the transduced electrical signal into number *ex: charge transfer devices

each constituent

-stationary phase -normal phase- sp is polar; mp non polar -reverse phase- sp is non polar; mp is polar

-reveals the identity of the sample elements and compounds in the sample -presence or absence of components -e.g: USP sample test

what is used in in chemical methods for natural products

primary std used in volhard

volhard VS

measurement of a transmitted light in a suspension *antibiotics *vitamins

*adsorption *partition *on exchange *pore penetration/ permeation *affinity

a branch of science that studies the interaction between electromagnetic radiation and matter *principle: the intensity of radiant energy transmitted, reflcted, or emitted is related to the concentration of the cheical species that absorbs energy

-measurement of excess energy lost by emission (flourescence) *thiamine *riboflavin

for structure elucidation

-the sp is a solid on which th sample is absorbed while the mp may be a liquid or a gas *thin layer chromatography *column chromatography *HPLC *gas chromatography

-AKA determinate error >with definite value and identifiable cause >same magnitude or replicate measurements made the same way >CCAN LEAD TO BIAS ND AFFECT ACCURACY OF RESULTS *instrumental errors *method errors *personal errors