LABORATORY MANUAL for
ANALYTICAL
CHEMISTRY
(Qualitative and Quantitative Analysis)
Compiled by Mrs. Rosario M. Oconer, MATCC
Reference: Qualitative Analysis by E.S. Gilreath
Activity #1
Analysis of Group I Cations
The Group 1 cation includes silver, lead and mercurous ions. They are precipitated
in their chloride forms. The insoluble chlorides are lead chloride, silver chloride, and
mercurous chloride. The analysis of this group is relatively simple. There are three steps
involved in the procedure. First, the group is precipitated with dilute HCl as insoluble
chlorides. Second, Lead chloride is removed from the precipitate by leaching with hot
water. and lastly, the separation of AgCl from Hg2Cl2 with ammonia water.
PROCEDURE:
1. Transfer solution to be analyzed (unknown sample) in a test tube and add 10 drops
of 3M HCl. Mix thoroughly and centrifuge. Test for complete precipitation by adding
another drop of 3M HCl. centrifuge and discard centrifugate. Precipitate remaining
in the test tube is washed with 10 drops of distilled water containing 1 drop of 3M
HCl. Stir, centrifuge and discard wash water.
2. White precipitate obtained in procedure #1 may be PbCl2, AgCl, and Hg2Cl2 Add
6-7 drops of distilled water and heat with stirring for 1 minute in a water bath.
Centrifuge quickly and transfer centrifugate into another test tube.
2A. TEST FOR CENTRIFUGATE
Centrifugate may contain Pb2+. Add 4 drops of K2CrO4. Yellow precipitate
confirms presence of LEAD ION.
2B. TEST FOR RESIDUE/PRECIPITATE
Residue may contain AgCl & Hg2Cl2. Treat residue with 10 drops of 3M
NH4OH, stir thoroughly and centrifuge. Transfer centrifugate into another test
tube. A blackening of the residue indicates the presence of the mercurous ion.
3. Centrifugate from 2B may contain Ag (NH3)2+. Acidify centrifugate with 3M HNO3.
Formation of a white precipitate confirms the presence of SILVER ION.
Residue from 2B may contain mercury. Wash with 10 drops of distilled water and
discard washings. Dissolve the precipitate in 2 drops of concentrated HNO 3 and
dilute with 5 drops of water. Add 1-2 drops of SnCl2 solution. White or gray
precipitate confirms the presence of MERCUROUS ION.
DATA SHEET
Name: ______________________________ Rating: _______________
Yr. & Sec.: ______________________ Group No. ____ Date: ________________
GROUP 1 CATIONS ANALYSIS
ACTIVITY 1
UNKNOWN NUMBER: ______________
PRESENT ABSENT
CHEMICAL CHEMICAL
NAME NAME
FORMULA FORMULA
Activity # 2
Analysis of Group III Cations
The cations of Group III are precipitated in a solution containing ammonia,
ammonium chloride, ammonium sulfide, consequently, the group precipitate is a mixture
of sulfides and hydroxides. The seven cations of this group are iron, cobalt, nickel, zinc,
manganese, and chromium.
The high concentration of sulfide ion necessary for precipitation of Group III
sulfides is obtained in an ammoniacal solution. This basic solution also produces the
precipitation of chromium and aluminum as hydroxides in Group III. Group III is divided
into two subgroups by the action of a strong base, in excess, upon a solution of the cations
of this group. Chromium, zinc, and aluminum hydroxides dissolve in excess KOH solution
to form a soluble group, whereas manganese, iron, nickel, and cobalt hydroxides
precipitate to form an insoluble group.
PROCEDURE:
FIRST DAY OF THE ANALYSIS
1. Transfer the unknown sample a test tube and add 4 drops of saturated NH4Cl; then
concentrated NH4OH drop by drop until the solution is basic. Add 10 drops of
thioacetamide solution and place in a boiling water bath for 5 minutes. Centrifuge and
discard centrifugate.
2. Treat the precipitate with 5 drops of concentrated HCl and stir. If all the precipitate
dissolves, it indicates the absence of Ni and Co. Add 3 drops of concentrated HNO3 and
heat in water bath for 5 minutes. Make the solution basic by adding 10 drops of 3F
KOH (test with litmus paper), then add about 0.2 g of solid Na 2O2 and stir. Heat in a
water bath for 3 minutes and centrifuge. Separate the centrifugate from the residue.
Wash residue with 10 drops of distilled water, stir and centrifuge. Separate the
centrifugate from the residue. Wash residue with 10 drops of distilled water, stir and
centrifuge. Add washings to the centrifugate previously obtained. Centrifugate may
contain aluminum, chromium, and zinc ions while the residue may contain iron,
cobalt, manganese, and nickel ions. Keep both test tubes (with centrifugate and
residue) inside the locker.
SECOND DAY OF THE ANALYSIS
3. Add 10 drops of saturated NH4Ac to the centrifugate obtained from procedure #2,
then 3M HAc until the solution is acidic (test with litmus paper). Now add 3M NH4OH
drop by drop until the solution is decidedly ammoniacal. Centrifuge. Separate the
centrifugate from the residue.
TEST FOR THE RESIDUE
Residue may be aluminum hydroxide. Wash with 10 drops of water and discard
washings. Add 3M HCl drop by drop until residue dissolves. Add 3 drops of saturated
NH4Ac and 3 drops of aluminon reagent, then make decidedly ammoniacal with 3M
NH4OH. Allow the mixture to stand for 2 minutes, then centrifuge. Separation of a red
precipitate confirms the presence of ALUMINUM IONS.
TEST FOR CENTRIFUGATE
Add 1M Ba(Ac)2 to the centrifugate until precipitation is complete, (around 15 drops).
Centrifuge and separate the centrifugate from the residue. And continue the test as
follows:
FOR THE RESIDUE FOR THE CENTRIFUGATE
Add 10 drops of 3M HCl to the Acidify the centrifugate with 3M HAc
residue and warm for 1 minute in and add 5 drops of thioacetamide
water bath. Centrifuge and discard solution and place in boiling water
the white residue. Place 2 drops of bath for 5 minutes. Formation of a
centrifugate upon a piece of filter white precipitate confirms presence
paper and add 2 drops of H2O2. of ZINC ION.
Formation of a blue color which
fades rapidly confirms presence of
CHROMIUM ION.
THIRD DAY OF THE ANALYSIS
4. Precipitate from Procedure #2 may contain the hydroxides of iron, cobalt, nickel, and
hydrated manganese dioxide. Wash with 10 drops of water and discard washings.
Dissolve the precipitate in 5 drops concentrated HCl. Dilute the resulting solution to
approximately 25 drops and divide into four portions. Follow the procedure below to
test for the presence below to test for the presence of each iron.
FIRST PORTION:
Add 0.2 g of solid sodium bismuthate. Stir well and centrifuge. Reddish-purple color
in supernatant liquid confirms presence of MANGANESE ION.
SECOND PORTION:
Test for ferric ion by adding 2 drops of 3M NH4CNS. Appearance of deep red
coloration confirms presence of FERRIC ION.
THIRD PORTION:
Add solid NaF with stirring until undissolved NaF remains. Let 10 drops of alcoholic
NH4CNS run down the side of the test tube containing this portion. Appearance of
blue-green color at the junction of the 2 liquids confirms the presence of COBALT
ION.
FOURTH PORTION:
Add solid NaF with stirring until undissolved NaF remains. Make the solution basic
with 3M NH4OH, then add 4 drops of dimethylglyoxime. Formation of a red precipitate
confirms presence of NICKEL ION.
DATA SHEET
Name: ______________________________ Rating: _______________
Yr. & Sec.: ______________________ Group No. ____ Date: ________________
GROUP 3 CATIONS ANALYSIS
ACTIVITY 2
UNKNOWN NUMBER: ______________
PRESENT ABSENT
CHEMICAL CHEMICAL
NAME NAME
FORMULA FORMULA
Activity # 3
Analysis of Group V Cations
Group V Cations is sometimes called the soluble group and includes sodium,
potassium and ammonium ions. The salts of these cations, with few exceptions are quite
soluble. This accounts for the fact that there is no precipitating agent for the group. It is
necessary to test for the ammonium ion upon a portion of the original solution used in the
beginning of the analysis. If a strong base such as KOH or NaOH is added to a solution
containing ammonium ions and the solution is warmed, the escape of ammonia gas
results. The ammonia gas which escapes maybe recognized by its odor or by its action
upon moist red litmus paper.
The most reliable qualitative tests for sodium and potassium ions in low
concentrations are their identifying flame spectra. An intense yellow flame persisting for
several seconds confirms the presence of sodium ions. The presence of potassium ions
is indicated by a pale violet flame.
PROCEDURE:
1. Test for Sodium and Potassium Ions
Transfer one-half of the unknown sample to an evaporating dish and add 1 drop of
concentrated HCl. Perform flame test as follows:
Clean a platinum wire until it gives no color to a non-luminous flame. Dip end of the
wire in the above solution and return wire to the flame. Intense yellow flame persisting for 5
seconds confirms presence of SODIUM ION.
In the absence of sodium ions, presence of potassium ions imparts a pale violet color
to flame when viewed with the naked eye. If yellow flame of sodium is present it will be
necessary to view flame through a filter of cobalt glass. Repeat above test and examine flame
through a cobalt glass. Reddish-violet flame persisting for about 2 seconds confirms presence
of POTASSIUM ION.
2. Test for Ammonium Ion
Place the other half of the unknown sample into a small beaker and add 5 drops of
distilled water. Make solution alkaline with 3M KOH. Immediately cover the beaker with a
watch glass to which adheres a strip of moistened red litmus paper on the convex side. Warm
the solution gently for 1 minute. Even shading of litmus paper from red to blue confirms the
presence of AMMONIUM ION.
DATA SHEET
Name: ______________________________ Rating: _______________
Yr. & Sec.: ______________________ Group No. ____ Date: ________________
GROUP 5 CATIONS ANALYSIS
ACTIVITY 3
UNKNOWN NUMBER: ______________
PRESENT ABSENT
CHEMICAL CHEMICAL
NAME NAME
FORMULA FORMULA
