Assiut university Faculty of science Chemistry department

Prepared by:*Group 1 :- Leader/ Sondos Nady Said -Members/ -Khadega Gamal Mohamed -Hanan Mohamed Osman

*Group 2 :-Leader/ Doaa Mohamed Mostafa -Members/ -Doaa Mohamed Taha -Eman Ahmed Abd El-Kareem -Hala Abd El-Mabod Mohamed
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Estimation of Nitrogen content by kieldhl's method

** Idea
(Sample Containing Nitrogen) digestion H2SO4 (conc.) Kieldhal catalyst NaOH (NH4)2SO4

NH3 bsorbed in water

distillation

NH4OH

Followed by titration aganist HCl

** Calculations:
Wt. of Nitrogen = (N x V) HCl . = (N x V) HCl .
eq.wt . 1000 14 1000

Consumed volume of HCl in the Nitrogen content =

wt .of Nitrogen in sample x 1000 wt. of sample

Facts about kieldhal method: - The using of kieldhol catalyst such as selenium and mercuric sulphate improve the sulphuric acid digestion. - Kieldhal method is not suitable for azo compounds and any substance where oxygen is attached to nitrogen as in the nitro and nitroso compounds, because there is a tendency to lose some of the nitrogen as gaseous nitrogen or as an oxide. But such compounds can be estimated by kieldhal method after their reduction by hydrogen iodide and red phosphorus before undergoing the digestion process. Also, the lose of Nitrogen of these substances

can be avoided through digestion process if we add an excess of glucose to the digestion mixture. ** Example: 0.02035 gm of glycine yielded an amount of NH3 that required 10.96 ml of 0.025 N HCl. Estimate the Nitrogen content? wt. of N in the sample= (N x V)HCl .
=

14 1000

(0.025) (10.96) .14 1000 =3.836 10 3 gm

Nitrogen content

(3.936) (10 3 ) 100 0.02035

= 18.25 %

Estimation of Nitrogen content by Dumas method

Idea
Comound ignition O2 CO2 + H2O + SO2 + X2 + N2

N2 Pass through KCH without absorbtion and its volume is measured

CO2 + H2C + SC2 + X2 are absorbed by Pot. hydrate

- any oxides of nitrogen that might have been produced during the combustion re converted into nitrogen by passing through a heated cupper spiral. Example:
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0.02357 gm of acetanilde gave 2.21 ml of N2 at 18 0C and 754 mm.

Estimate the nitrogen content

P1 = 754 mm At STP P2 = 760 mm
PV PV 1 1 = 2 2 T1 T2 V2 = P 1V1 T2 . = 2.0569 ml T1 P2

T1= 18 + 273 = 291 0k T2=273 0k V2 = ?

V1= 2.21 ml

at STP 22400 ml of N2 contains 28 gm N2

2.0569 ml N2 contains ?? gm N2 wt. of N2 in the sample
(2.0569) (28) =2.6 x 10 3 gm 22400 2.6 x 10 3 nitrogen content in sample = x 100 = 11% 0.02357 =

Estimation of Sulfur content by Carius method

Idea
Compound Containng Sulfur HNO3 Fuming H2SO4

BaCl2 BaSO4

Calculation
BaSO4 contains S

m.wt. of BaSO4 .wt. of BaSO4

CO2

contains

C S

CO2

contains

C wt. of S in sample?

Wt. of S in the sample =

( wt. of BaSO4 )(at. wt .of S ) ( m.wt . of BaSO4 )

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Sulfur content = Example

wt . of S in the sample x 100 wt . of sample

0.2563 gm of sulfur containing compound gave 0.2655 gm of barium sulphate . calculate the sulfur content in the sample . Wt. of sulfur in the sample = =
(0.2655)(32) = 0.0365 gm ( 233)
0.0365 x 100 =14.234 0.25636

( wt . of BaSO4 )( at. wt.of S ) ( m.wt . of BaSO4 )

Sulfur content =

%
O

If molecular formula of this compound is C13H12N2S -Theortical sulfur conteant = 14.05 %

Ph-NH-C-NH-Ph

Estimation of Halogen content by Carius method

Idea

- This method is not suitable for sulfur containing compounds because Ag2S will be formed and cause an error in the calculation .

Calculation:
AgX contains X

m.wt. of AgX m.wt. of AgX

CO2 CO2

contains contains

C (at. Wt. of X) C wt. of halogen in sample?

Wt. of halogen in the sample

( wt .of AgX )( at.wt. of x ) ( M .wt . of AgX )

Halogen content =

wt . of ha log en in the sample x100 wt . of the sample

- this method can not be used for compound contains more than one type of halogen. Example 0.1872 gm of chloral hydrate gave 0.4856 gm in carious method

Calculate chlorine content

wt. of chlorine in the sample = = Chlorine content=
( wt . of AgCl )(at .wt .ofcl ) m.wt. of AgCl

(0.4856) (35.5) =0.12 gm (143.5)

0.12 x100 = 64% 0.1872

Theortical chlorine content= 64.33 %

Determining the empirical and molecular formula of organic compounds

empirical formula: is the formula that shows the type of the elements consisting the compound and the simplest ratio between their numbers. Molecular formula: is the formula that shows the type of the elements consisting the compound and the number of each element atoms. for example Molecular formula Empirical formula glucose C6H12C6 CH2O

Estimation of Carbon and hydrogen in organic compounds

1 gm tka Organic Compund O2

CO2

H2O

absorbed by scda. lime

absorbed by nhydrouse magnesium perchorte

for estimating carbon

CO2 contains C

m.wt. of CO2 .wt. of CO2

CO2

contains

C at. Wt. of C

CO2

contains

C Wt. of carbon in sample?

Wt. of carbon in sample = Carbon conent (percent) =

( wt. of CO2 )(at.wt . of C ) ( M .Wt.of CO2 )

wt . of Carbon in the sample x100 wt. of smple

for estimating Hydrogen content

H2O contains 2H

m.wt. of H2O .wt. of H2O

CO2

contains

C 2 (at. Wt. of H)

CO2

contains

C wt. of Hydrogen in sample?

Wt. of hydrogen in sample = hydrogen content (percent) = for any element

( wt. of H 2 O )(2 at. wt.of H ) ( M .Wt.of H 2 O )

wt. of hydrogen in sample x 100 wt . of sample

No. of moles = wt of element/ at.wt of element

Calculated the molecular formulation of an organic dibasic acid which gave the next results on analysis: a) 0.249 gm of dicarboxylic acid gave on combustion 0.528 gm CO2 and 0.081 gm H2C. b) 1.9 gm of silver salt of that acid, on ignition gave 1.08 gm of silver.

Solution
M.w.t. of carboxulic acid = acid is dibasic n = 2 m.wt. of carboxylic acid =
1.9 2 108. 107 1.08
wt . of silver salt n 108. 107 w.t of silver metal

= 166 g/mole

for carbon
CO2 contains C

m.wt. of CO2 .wt. of CO2

CO2

contains

C at. Wt. of C

CO2

contains

C Wt. of carbon in sample?

Wt. of carbon in sample =

( wt . of CO2 )(at.wt . of C ) ( M .Wt.of CO2 )

= (0.528)(12) 44

= .144 gm

No. of moles of carbon in the sample =

0.144 12

= 0.012 mole.

for Hydrogen
H2O contains 2H

m.wt. of H2O .wt. of H2O

CO2

contains

C 2 (at. Wt. of H)

CO2

contains

C wt. of Hydrogen in sample?

Wt. of hydrogen in sample =

( wt. of H 2 O )(2 at. wt.of H ) ( M .Wt.of H 2 O )

= (0.081)(2 1) 18

= 9 x 10-3 gm No. of moles of hydrogen in sample= For Oxygen wt. of oxygen in sample = wt. of sample [wt. of c + wt. of H] = 0.249 [0.1444 + 9 x 10-3]= 0.096 gm. No. of moles of oxygen in sample =
0.096 16
9 10 3 = 9 10 3 moles 1

= 6 x 10-3 moles

by division on the lowest no. of moles 6 x 10-3 The empirical formula is

C 0.012 H 9103 O6103
6 10 3 6 10 3 6 10 3

C 2 H 1.5 O

M.wt. of empirical formulae = (2 x 12) + (1.5 x 1) + (16) = 41.5 M.wt. of molecular formula = 166
M .wt . of molecular Formula 166 = =4 M .wt . of empricial formula 41.5

Molecular formula = 4 (empirical formula) = 4 (C2H1.5O) = C8H6O4

COOH COOH

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