Experiment 6 ELEMENTAL ANALYSIS

By: Catherina Barcel and Rogelio Rivera

INTRODUCTION

Elemental Analysis
It is the process where a substance is analyzed for its elemental composition C,H,O,N,S,P,X

In the case of our experiment, what we did was a qualitative elemental analysis, that is, we only want to know what elements make up the substance

SODIUM FUSION (Lassaignes test)

When an organic material is strongly heated with sodium, it turns into an inorganic sodium salt

WHY SODIUM? Because sodium is highly reactive, has a low melting point, and most of its salts are soluble in water.

CAUTION!!!
Sodium is highly reactive in water, it violently reacts with water The reaction is highly exothermic

OUR TEST SAMPLES

P-chloroaniline

thioacetamide

PROCEDURES

Sodium fusion
A piece of Na was heated in a test tube until no vapor was observed P-chloroaniline was added The test tube was heated to initiate the reaction. Then, the tube was removed and heated again to redness The tube was placed in water (it shattered, its okay.) Allow excess sodium to react. Then the solution was boiled and filtered

QUALITAIVE TESTS

Sulfur test
Fusion solution + water in test tube Add nitroprusside Blue violet solution should be seen

Nitrogen Test
Add FeSO4 to fusion solution in test tube. Add KF and boil Add FeCl3 and add sufficient H2SO4 to dissolve excess iron hydroxides and to acidify the solution ( to dissolve any free alkali) Blue solution should be seen

Halogen Test
If the sample is positive for nitrogen or sulfur, acidify the fusion solution with HNO3 and boil Add AgNO3 and look for precipitates. Heavy curdy-type precipitate indicates the presence of halogens. If sample is only slightly turbid, test is negative. AgCl(white precipitate) AgBr (pale yellow precipitate) AgI (yellow precipitate)

RESULTS
Test sample Sulfur Nitrogen Cl P-chloroaniline + + Halogen Br I -

Thioacetatamide

DISCUSSION

Sodium fusion
It was developed by J.L. Lassaigne It is used for detection of halogens, sulfur, and nitrogen In theory, when sodium is reacted with any halogens, sulfur, or nitrogen, they will be converted to inorganic salts and can therefore be detected by inorganic analysis

Sulfur Test
Sodium nitroprusside reacts with sodium sulfide to form Na4[Fe(CN)5NOS] which forms the deep blue-violet color

It can also be noted that sulfur has a distinctly smelly odor.

Nitrogen Test
Addition of Fe2+ from the FeSO4 and Fe3+ from the FeCl3 converts the CN- ions into ferric ferrocyanide which gives the prussian blue color

Halogen Test
Beilstein test By Fredrich Konrad Beilstein A preheated (to remove any NaCl present from the handling of the wire) copper wire is dipped into the fusion solution and then burned. A blue green flame indicates the presence of a halogen. The color comes from the light emitted from the excited states of the copper halide.

 The AgCl test: The reactions of the halogen ion with the silver ion are as follows:

White precipitate

Pale yellow precipitate

Yellow precipitate

BUT WAIT, THERES MORE!

Oxygen
There is no direct method for the detection of oxygen (Vogel). If the known chemical formula is still insufficient to account for the mass of the sample Ignition If it relights a glowing splint Organic molecules produce blue flames when heated when they contain oxygen

For Phosphorus
Ammonium molybdate reagent Add a large excess of that to the test solution and it will produce a yellow precipitate.

Phosphorous also smells like phosphine (garlicky or rotting flesh smell) during sodium fusion Note that arsenic also behaves like phosphorus in this test so oxidize it first to be sure!

OTHER METHODS

For Sulfur
Acidify the fusion solution Add a few drops of lead acetate A black precipitate will be apparent if the solution contains sulfur

Black precipitate

For Nitrogen
Mix p-nitrobenzaldehyde with in methoxyethanol and o-nitrobenzaldehyde in methoxyethanol and an aqueous solution of sodium peroxide. Add a small amount of the fusion solution and a deep purple color tests positive for cyanide ions.

How do we differentiate between AgCl, AgBr and AgI?

Try the solubilities in ammonia.

If you really, really want to make sure that the precipitate is AgCl
If the silver chloride is filtered off, washed with distilled water, and then shaken with sodium arsenite solution it is converted into yellow silver arsenite (Vogel).

Silver iodide and silver bromide are unaffected.

If you really have doubts, there may be multiple halogens

Reaction if iodine is present

Reaction if bromine is present

For chlorine, add excess glacial acetic acid and slight excess of lead dioxide. Boil and repeat silver nitrate test for halogens.

END OF DISCUSSION.

REFERENCES
Vogels Textbook of Macro and Semimicro Qualitative Inorganic Analysis 5th ed, 1979 Vogels Textbook of Practical Organic Chemistry 5th ed, 1989 www.wikipedia.org Higher batches