quantitative analysis by UV spectroscopy

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Presentation Transcript

QUANTITATIVE ANALYSIS BY UV - SPECTROSCOPY : 

QUANTITATIVE ANALYSIS BY UV - SPECTROSCOPY Aju S. Sam 1st year M.Pharm Nehru College of Pharmacy

Introduction : 

Introduction LAMBERT’S LAW: “When a beam of light is allowed to pass through a transparent medium the rate of decrease in intensity with the thickness of the medium is directly proportional to intensity of the light.” -dI/dt ∞ I It = I0 e-kt (1)

Slide 3: 

BEER’S LAW “The intensity of a beam of monochromatic light decreases exponentially with increase in concentration of absorbing substances arithmetically.” It = I0e–k’c (2) On simplification and combining (1) and (2) we get

Slide 4: 

log (I0/It) = act This is called BEER-LAMBERT’S LAW. Relationship between Absorbance(A), Transmittance(T) , & Molar extinction coefficient(ε). A = εct = log (I0/It)= log (1/T) = log -T

METHODS USED FOR ASSAY : 

METHODS USED FOR ASSAY USE OF CALIBRATION GRAPH: Step 1: select the λmax . Step 2: prepare series of known conc. Solutions. Step 3: set λmax in spectrophotometer. Step 4: measure absorbance. Step 5: plot calibration curve. absorbance conc.

2. USE OF STANDARD ABSORPTIVE VALUE : 

2. USE OF STANDARD ABSORPTIVE VALUE In this method standard ε value ie ε 1%1cm is used. A = ε1%1cmct e.g. ε1%1cm for methyl testosterone in B.P is 540 at 241 nm.

3.SINGLE OR DOUBLE POINT STANDARDISATION : 

3.SINGLE OR DOUBLE POINT STANDARDISATION Involves measurement of sample and reference. Conc. of reference close to that of sample. C test= A test × C std A std Double point involves use of 2 reference. one greater conc. than sample, other lower conc. than sample. C test=(Atest- Astd1)(Cstd1- Cstd2)+Cstd1(Astd1- Astd2) Astd1-Astd2

4.ASSAY USING ABSORBANCE CORRECTED FOR INTERFERENCE : 

4.ASSAY USING ABSORBANCE CORRECTED FOR INTERFERENCE The concentration of absorbing component = total absorbance – absorbance of interfering substance.

5.Assay after solvent extraction of sample : 

5.Assay after solvent extraction of sample Involves separation of absorbing interferents by solvent extraction, choice of pH . e.g. B.P Assay of Caffeine in Aspirin & Caffeine tablet

6.SIMULTANEOUS EQUATION METHOD : 

6.SIMULTANEOUS EQUATION METHOD Total absorbance of a solution is equal to the sum of absorbance of individual components present. absorbance λ1 wave length λ2 mixture x y

Slide 11: 

A1= ax1bcx+ay1bcy (at 1) A2= ax2bcx+ay2bcy (at 2) C x = A2ay1-A1ay2 ax2ay1-ax1ay2 Cy= A1ax2-A2ax1 ax2ay1-ax1ay2 e.g. B.P assay of quinine related alkaloids in Cinchona bark.

7.ABSORBANCE RATIO METHOD : 

7.ABSORBANCE RATIO METHOD For a substance which obeys BEER’S LAW at all wavelengths, the ratio of absorbance at any two wavelengths is a constant value independent of concentration or path length. In USP the ratio is referred as Q value. e.g. cyanocobalamin exhibits three λmax at 278nm, 361nm, 550nm A361/A550 = 3.30 ± 0.15 A361/A278 = 1.79 ± 0.09

DIFFERENCE SPECTROSCOPY : 

DIFFERENCE SPECTROSCOPY Two samples used, one in reference beam and one in sample beam. Conc. of absorbing substance identical. But some solution parameter like pH is different. Difference absorbance ∆A = A alk - A acid

DIFFERENTIAL SPECTROSCOPY : 

DIFFERENTIAL SPECTROSCOPY

Slide 15: 

0 10 20 30 40 50 60 70 80 90 100 (BLANK) RECEIVER DARK 0 10 20 30 40 50 60 70 80 90 100 HIGH ABSORBANCE 0 10 20 30 40 50 60 70 80 90 100 (BLANK) 0 10 20 30 40 50 60 70 80 90 100 TRACE ANALYSIS 0 10 20 30 40 50 60 70 80 90 100 C1 C1>C2 C2 0 10 20 30 40 50 60 70 80 90 100 MAXIMUM PRECISION

DERIVATIVE SPECTROPHOTOMETRY : 

DERIVATIVE SPECTROPHOTOMETRY Conversion of normal spectrum into its first or higher derivative spectrum. First derivative spectrum- (dA/dλ) v/s λ A λ dA/dλ λ + - λmax Cross over point (λmax)

Slide 17: 

Second derivative spectrum A λ d2A/dλ2 λ + - X+Y X Y

REFERENCES : 

REFERENCES A.H.BECKETT, J.B.STENLAKE.PRACTICAL PHARMACEUTICAL CHEMISTRY, 4TH EDITION, PART TWO; 2005: 275-300. WILLARD,MERRITT,DEAN,SETTLE. INSTRUMENTAL METHODS OF ANALYSIS, 7TH EDITION;1986:159-178. GURDEEP.R.CHATWAL,SHAM.K.ANAND. INSTRUMENTAL METHODS OF CHEMICAL ANALYSIS, 5TH EDITION;2007:140-178.

Slide 19: 

THANKS