oc 1. elemental b.pharm organic chemistry by amit z chaudhari
TRANSCRIPT
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ELEMENTS
Amit Z Chaudhari
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FLOW
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Quantitative analysis of elements
3Organic Chemistry_ AZC_2016_ Elemental
Estimation of C and H[sum12]
Principle:- Organic substance is burnt in excess of oxygen gas. C and H are
oxidized to CO2 and water.
CxHy + O2 xCO2 + y/2 H2O
Figure:
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Apparatus :- Oxygen supply: it oxidizes and flows the generated water and CO2
toward adsorbent assembly.- Furnace: heating purpose- Combustion Tube:
- is a hard round glass tube.- Substance, CuO gauze and copper oxide (CuO) are placed
in it as in figure.- CuO gauze (placed at front) prevents the backward diffusion of
the products.- Substance is place in porcelain boat.- CuO layer and CuO gauze(placed in toward the end) prevents any
vapours of substance leaving the tube unoxidized.
Quantitative analysis of elements
Organic Chemistry_ AZC_2016_ Elemental
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Absorption apparatus :- A U-tube packed with Conc. H2SO4 to absorb water.- A set of bulbs containing conc. KOH, to absorb CO2.- A Guard-tube filled with anhydrous CaCl2, to prevent entry of atm
moisture. Procedure:- Combustion tube heated in furnace to remove moisture and CO2
already present.- Note down the weigh U-tube and bulbs filled by absorbents- Then assamble all parts.- Heat- Pass O2 - After combustion of all sub. Pass strong flow of O2 to remove all
CO2 and water and finally detaches all assembly.
Quantitative analysis of elements
Organic Chemistry_ AZC_2016_ Elemental
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Calculation:
- % of C = 12y/44 * 100/w where,
y = increase wt of potash bulb (wt of CO2)w = wt of substance
- % of H = 2x/18 * 100/w where,
x = increase wt of U-tube (wt of H2O)w = wt of substance
Quantitative analysis of elements
Organic Chemistry_ AZC_2016_ Elemental
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Quantitative analysis of elements
7Organic Chemistry_ AZC_2016_ Elemental
Estimation of N[win14, win12, sum14, sum15]
- Two methods and
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Quantitative analysis of elements
8Organic Chemistry_ AZC_2016_ Elemental
Dumas method[win 14, win13]
Principle:- Nitrogenous compound when heated with copper oxide in atm of
CO2 yield free nitrogen.
- CxHyNz + CuO xCO2 + y/2H2O + z/2 N2
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Quantitative analysis of elements
9Organic Chemistry_ AZC_2016_ Elemental
Dumas methodFigure:
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Quantitative analysis of elements
10Organic Chemistry_ AZC_2016_ Elemental
Dumas method
Apparatus:- CO2 generator: generated by chemical methods (magnesite
(MgCO3) or a Kipp’s apparatus containing marble and dil. HCl.)- Gas is passed to combustion tube.- Combustion Tube: Substance, CuO gauze and coarse copper
oxide (CuO) and copper spirals are placed in it as in figure.- CuO gauze (placed at front) prevents the backward diffusion of
the products of combustion.- Substance is mixed with excess fine CuO.- Coarse CuO layer generates N2 gas by oxidizing the sample.- Reduced copper spiral (placed in toward the end) reduces any
oxides of N formed during combustion, to N2.
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Quantitative analysis of elements
11Organic Chemistry_ AZC_2016_ Elemental
Dumas method
Apparatus:- Schiff’s Nitrometer: N2 is estimated by passing into this apparatus
where CO2 and other gas byproducts are absorbed by caustic potash soln and the N2 collects in the upper part of the graduated tube.
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Quantitative analysis of elements
12Organic Chemistry_ AZC_2016_ Elemental
Dumas method
Procedure:- The assembly is fitted up as shown in fig. - Keep the tap of nitrometer is left open.- CO2 is passed to replace air. When the air babble rising through
the potash soln disappear, it shows that only CO2 is coming and all air is removed from assembly.
- After leveling the potash layer in graduated tube, the tap of nitrometer is closed.
- Heat the combustion tube. - Formed N2 is collected automatically in nitrometer.- When the combustion is complete, a strong current of CO2 is
passed to sweep the last traces of N2 from it.- The volume of N2 collected is noted.
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Quantitative analysis of elements
13Organic Chemistry_ AZC_2016_ Elemental
Dumas method
Calculation:
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Quantitative analysis of elements
14Organic Chemistry_ AZC_2016_ Elemental
Kjeldahl’s Method[win15, win11] [sum13]
Principle:- Nitrogenous compound when heated with H2SO4, ammonium
sulphate is formed.- Ammonium sulphate is than treated with excess alkali and the
librated ammonia gas absorbed in excess of standard acid.- Back titration of acid gives the amount of ammonia (and hence of
N).
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Quantitative analysis of elements
15Organic Chemistry_ AZC_2016_ Elemental
Kjeldahl’s MethodFigure:
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Quantitative analysis of elements
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Kjeldahl’s MethodApparatus:- Kjeldahl flask- Kjeldahl trap: serves to retain any alkali comes up on vigorous
boiling.- Water condenserProcedure:- Take substance , conc. H2SO4 in Kjeldahl flask- Add little amt of K2SO4 (raises the b.p.) and CuSO4 (as catalyst).- Flask is loosely Stoppard and heated.- After completion of heating, cool it and transferred in to round
bottomed flask.- Add NaOH solution.
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Quantitative analysis of elements
17Organic Chemistry_ AZC_2016_ Elemental
Kjeldahl’s Method- Assemble the apparatus as in fig.- Upon heating of RBF, the liberated ammonia distilled into conical
flask containing acid soln.- When no more NH3 comes from reaction. conical flask is
displaced and excess of acid is back titrated.
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Quantitative analysis of elements
18Organic Chemistry_ AZC_2016_ Elemental
Kjeldahl’s MethodCalculation:
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Quantitative analysis of elements
19Organic Chemistry_ AZC_2016_ Elemental
Estimation of X
Carious method[win12]
Principle:- When substance containing X is heated with fuming nitric acid in
presence of silver nitrate, reaction will form silver halide from which amount of X is calculated.
Figure:
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Quantitative analysis of elements
20Organic Chemistry_ AZC_2016_ Elemental
Carious methodApparatus:- Carious tube: a hard glass bomb tube- Narrow weighing tube: for organic compound- Iron jacket present in furnaceProcedure:- An accurately weighed amount of org. compound is taken in a
narrow weighing tube.- Carious tube is loaded with fuming nitric acid, small amt of
AgNO3 crystals and tube containing org. compound as shown in figure.
- Upper end of carious tube is sealed.- It is enclosed in iron tube and strongly heated in a furnace. - Org. compound ionized and the halide combines with silver
nitrate to give a ppt of silver halide.
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Quantitative analysis of elements
21Organic Chemistry_ AZC_2016_ Elemental
Carious method- After 6 hr, the tube is cooled and then broken.- Ppt of silver halide are washed, dried and weighed.
Calculation:
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End of topic
Reference:Organic Chemistry – Bahl &
BahlOrganic Chemistry – P.L.
Sony
IMP Q. For 1st MID Sem Exam
(1)quantitative estimation of nitrogen (5)(2)Dumas method (5)(3) kjeldahl’s method (5)