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CHEMISTRY P3

Dr PROPH J

Proph J
TABLE OF
CONTENTS
EMPHASIS HEADING 1 PRACTICAL ............................ 1

Heading 2 QUALITATIVE ANALYSIS .............................................. 1


Heading 2 QUANTITATIVE ANALYSIS ............................................ 2
QUALITATIVE ANALYSIS

Take good note of the following points.

✅ For tests involving more than one reagent, the order of addition of
the reagents may be changed. In most situations, the test remains the
same, and you should use the order in the qualitative analysis book in
interpreting the change order in the examination protocol.

✅The color you observed in carrying out the experiments would in


most cases differ slightly from those written in the qualitative analysis
book and given in the color charts. Most often, this arises due to
differences in concentration or complicated mixtures and or impurities
or low qualities of the reagent. You should approximate the colors you
observed to the standard ones given in the inference book. Such
approximations are indispensable in writing the correct inferences.
Making a Reference

1) Carry out the experiment steadily with much self-confidence and


take fast decisions about your observations.

2) From here, move straight to the “MAJOR OBSERVATION(S)” column


(for major reagents). There, look for section, 1,2,3, etc. and
subsection, (a), (b), (b), etc. of interest. Find the set of observations
that are closest to yours. The MAJOR OBSERVATION(S) column leads
you to the set of observations and inferences you are looking for.
Observations and inferences should be written briefly and logically.

3) The table of contents and list of reagents should be used to search


for any reagent. The table summarizing precipitation reactions (page
58) should be consulted whenever a precipitate is formed with a
reagent which is not found in the table of contents and the index of
reagents.

4) For some reagents, the cations (or anions) (active ingredients) are
interchangeable (e.g. KOH instead of NaOH or MgCl2 instead of
MgSO4). This is based on the fact that for some reactions, the source
of the anion or cation reacting does not matter.

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5) If in doubt with a set of observations, used the inferences of
previous or next experiments to clarify your doubts.

6) If more than one reagent is used to carry out a particular test of


which the combination of reagent is not tabulated in the reference
book and of which each addition gives rise to observable changes, the
reference may be made independently, i.e. each reagent reference
may be made separately, and the references combined.

7) The first test is usually a preliminary test for either cation or anion
or for a compound. The inference may concern a number of
possibilities which must all be reported (the first test may also be a
flame test or special test to reveal, directly, a cation, anion or
compound).

8) Further tests, in the case where the first test gives a number of
possibilities are generally aimed at reducing these possibilities to one
or a few of them. This is why many inferences concerning a cation, for
example, must be related. This however does not apply squarely to
mixtures of double salts.

9) The substance is thus, finally identified after a progressive and


subjective acceptance of correct intermediate answers.

Some Logical Examples

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1st inference: M or N or L;

2nd inference: N or L or D present;

3rd inference: N or G present

The first inference must include M, N and L. The second inference


can only include N and L, but not D, since D was not a possibility in the
first inference. The third inference must be written only on N since G
was not a possibility in any of the previous inferences.

Thus, N is the cation or anion or compound we are looking for.

*Second logical example*

1st inference: A or B or C or D present.

2nd inference: A or E present.

3rd inference: C or F present.

Substance may contain A and C, e.g two cations in a double salt,


(NH4)2SO4.FeSO4.

Check to see that the observations on A and C in this set of tests are
not very similar. If they are very similar, substance can either be A or
C. Decide logically.

*EXAMPLES OF EXPERIMENTAL REPORTS*

Example 1

You are provided with an organic compound, R. Carry out the following
experiments on R and record the observations and inferences on the
spaces provided.

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a) Place a little of substance R on an inverted crucible lid and ignite
from above.

OBSERVATION

Sample R (liquid) burns readily with a low luminous non-sooty flame.


No residue.

What is the Inference?

Answer:

INFERENCES

Substance has a low C:H ratio. Probably a lower saturated aliphatic


organic compound present.

NB: Since substance burns with a low luminous flame, it will be


irrelevant monitoring non-luminous-flame, ie writing that: substance
burns readily with a non-luminous or low luminous.

b) Place a little of substance R in a small dry beaker and add PCl5.

OBSERVATIONS

Sizzling sound. White pungent steamy fume of air, evolved, fumes


turns moist blue litmus paper red.

Inference?

Answer:

INFERENCES

Acidic HCl gas evolved. –OH group present. Substance is an aliphatic


alcohol or carboxylic acid. Equation!

NB. Since substance is a liquid and did not burn with a sooty flame or
with the smell of burnt sugar,(or paper) in test(a) it means the
compound could not be a carbohydrate or aromatic compound. Ie

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these possibilities have been eliminated. (refer to reactions with this
reagent for a clearer picture)

c) To about 1cm3 of R in a test tube, add 1cm3 of dilute H2SO4 acid


follow by 1cm3 of potassium dichromate solution and heat. Preserve
solution for test (d) below.

OBSERVATIONS

Orange mixture gives green solution on heating.

Inference?

Answer:

INFERENCES

Compound reduces Cr6+ or Cr3+(green). R is therefore a reducing


agent, hence redox reaction. R is an alcohol.

NB. Since carboxylic acids cannot be oxidized; it follows that R can


only be an alcohol. R can also not be a tertiary alcohol since these are
not oxidized.

d) To the solution from (c), add 3cm3 of water follow by aqueous


sodium hydroxide, and then add 1cm3 of iodine solution and warm.

OBSERVATIONS

Light yellow suspension (or precipitate) with antiseptic smell formed


on warming as grey-green precipitate. The precipitate dissolves after
addition of sodium hydroxide.

Inference?

Answer:

INFERENCES.

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Yellow precipitate of iodoform (tri-iodomethane). Grey-green
precipitate is Cr(OH)3.

CH3CHOH + I2/OH- -->( CHI3 + COO-.

Methyl carbinol group present. R was oxidized to a ketone. Thus, R is


secondary alcohol.

NB: Finally note how the conclusion has been arrived at. A tertiary
alcohol would not have been oxidized. A primary alcohol on the other
hand would have been oxidized directly to a carboxylic acid, hence no
formation of iodoform.

Exercise :

You are provided with a salt, W carry out the following experiments on
W and record the observations and inference in the space provided.

a) Divide sample W into two portion. Place the first portion in a test
tube and add concentrated sulphuric acid.

OBSERVATION

White pungent steamy fumes evolved. Fumes turned moist blue litmus
paper red in air.

Inference?

INFERENCE.

Acidic HCl gas evolved. W is a chloride. Equation!

NB: In air, colorless HCl absorbed moisture and becomes white.

b) To 2cm3 of the solution of W, add a pure sodium hydroxide.

OBSERVATION

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White precipitate form, insoluble in excess reagent.

Inference ?

INFERENCE

Insoluble metal hydroxide M(OH)x precipitated. Hydroxide not


amphoteric. Cd2+, Mg2+, Ca2+ or Ba2+ present.

NB: The four possibilities (under inference) MUST all be mention here
because no preliminary test is there to permit us to eliminate any

c) To 2cm3 of the solution of W, add aqueous magnesium sulphate.

OBSERVATION

No change (no observation).

INFERENCES?

INFERENCES

Mg2+ present (or confirmed)

NB: W can thus contain only Mg2+ since only it sulphate of all the
cations listed in (b) above is soluble. Precipitation would have been
observed if any of the other cations listed in test (b) were present.

Question

Suggest an identity for substance W

Answer : mgcl2

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