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The Kjeldahl analysis in Section 11-8 is used to measure the nitrogen content of organic compounds, which are digested in boiling sulfuric acid to decompose to ammonia, which, in turn, is distilled into standard acid. The remaining acid is then back-titrated with base. Kjeldahl himself had difficulty in 1880 discerning by lamplight the methyl red indicator end point in the back titration. He could have refrained from working at night, but instead he chose to complete the analysis differently. After distilling the ammonia into standard sulfuric acid, he added a mixture of KIO3and KI to the acid. The liberated iodine was then titrated with thiosulfate, using starch for easy end-point detection even by lamplight. Explain how the thiosulfate titration is related to the nitrogen content of the unknown. Derive a relationship between moles ofNH3 liberated in the digestion and moles of thiosulfate required for titration of iodine.

Short Answer

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The relationship between moles of NH3liberated in the digestion and moles of thiosulfate required for titration of iodine is derived.And how thiosulfate titration is related to the nitrogen content of the unknown is explained.

Step by step solution

01

Using the concept of mole.

  • The mole concept is a simple way to express the amount of a substance. Any measurement is divided into two parts: the numerical magnitude and the units in which the magnitude is expressed. For example, if the mass of a ball is 2 kilogrammes, the magnitude is '2' and the unit is 'kilogramme.'
  • When dealing with particles at the atomic (or molecular) level, even one gramme of a pure element is known to contain a large number of atoms. This is a common application of the mole concept. It primarily focuses on the unit known as a'mole,' which is a count of a very large number of particles.
02

Determining the ratio of moles.

In Kjeldahl analysis, 1molNH3of is equal to1molofH:

n(NH3)=n(H+)

Since there are 2 moles of H+inH2SO4they moles are doubled:

n(NH3)=n(H+)

After the initial role="math" localid="1654863625697" H2SO4reacts with NH3 the excess H2SO4reacts with KI and KI03 and it is titrated with thiosulfate.To determine the ratio of moles of H2SO4and thiosulfate we have to use reactions 16-18 and 16-19:

IO3-+6H++8I-⇌3I3-+3H2O(1)I3-+2S2O32-⇌S4O62-+3I-(2)

By using reaction (1) we can determine the ratio of moles of sulfuric acid and triiodide:

6n(H+)=3n(excessH2SO4)=3n(l3-)l:36n(H+)=n(excessH2SO4)=n(l3-)

By using reaction (2) we can determine the ratio of moles of triiodide and thiosulfate:

n(l3-)=12n(S2O32-)

Therefore, the ratio of moles of sulfuric acid and thiosulfate are:

role="math" localid="1654864150133" n(excessH2SO4)-12n(S2O32-)

Moles ofNH3are:

n(NH3)=2n(H2SO4)n(NH3)=2(n(excessH2SO4)-n(excessH2SO4))

By replacing excess moles of sulfuric acid with moles of thiosulfate we get:

n(NH3)=2n(initialH2SO4)-12n(S2O32-)

Hence the relationship between moles of NH3liberated in the digestion and moles of thiosulfate required for titration of iodine is derived. And how thiosulfate titration is related to the nitrogen content of the unknown is explained.

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