Exercise No.

1
3: Alkali and
Alkaline-earth Elements
Introduction
It is characteristic of the alkali elements that their cations do not form
insoluble chlorides, sulfides, carbonates, or phosphates. Therefore, in the
qualitative analysis scheme, they do not precipitate when successive
reagents are added but are left in the residual solution as unprecipitated ions.
They are usually identified by their flame spectra in the presence of HCl as a
volatilizing agent. Because the flame test is made after separation into all the
groups and the test is sensitive to the presence of even trace amounts of
elements, it is necessary to guard against the introduction of contaminating
amounts of alkali element when adding the precipitating reagents. For
example, not only is it inadmissible to add NaCl to precipitate the insoluble
chlorides but the HCl used instead must be checked for possible presence of
Na contamination. In the present scheme, only the most common alkali
elements (Na and K) are included.
As stated, cations of the alkaline-earth elements do not form insoluble
chlorides or sulfides. Except for beryllium, which is not included in the present
scheme, and magnesium, they do form insoluble carbonates and can thus be
separated from the alkali elements. Once the carbonates have been
precipitated, they can be dissolved again in an acetic acid buffer and the
alkaline-earth elements precipitated out consecutively, making use of
differences in the solubilities of the chromates and oxalates. Because the
difference with strontium is so slight, it is not included in the present scheme.

Learning Outcomes
1. Differentiate alkali from alkaline – earth elements through flame tests
and solubility.

Materials
• Laboratory Manual
• Bunsen Burner
• Hotplate and water bath
• Chemicals and Glasswares:
a. 50 mL beaker
b. Test tubes
c. Medicine droppers
For instructional purposes only • 1st Semester SY 2020-2021 25

d. Spatula
e. Nichrome wire
f. Barium chloride
g. Magnesium chloride
h. Calcium chloride
i. Sodium carbonate
j. Hydrochloric acid
k. Potassium nitrate
l. Ammonium carbonate
m. Ammonia
n. Acetic acid
o. Ammonium phosphate

Procedure

1. Test for alkali elements Na and K.

a. Get a piece of nichrome wire about 15 cm long and fashion
the end of it into a tiny loop. Stick the other end into a cork,
which will serve as a handle. Prepare a solution by dissolving
a few milligrams of Na2CO3 in a few milliliters of water and
adding 1 mL of 6M HCl. Dip the loop into the solution, and
hold it in the blue edge of a burner flame. Note the color.
b. Clean the wire by heating it strongly in the flame and dipping it
in a few milliliters of 6M HCl in a test tube. Heat again.
Repeat until the flame coloration reaches a low constant level.
Test a fresh portion of 6M HCl to see how much Na
contamination it has. In future tests, before reporting positive
presence of sodium, compare the flame tests of the unknown
with that given by the reagent HCl.
c. Observe the flame test for K by making up a solution of a
potassium salt, such as KNO3, with added HCl. Look at the
flame through a double thickness of cobalt glass. The glass
transmits the K flame color but filters out the Na color. Note
that the K flame is very transient and can easily be
overlooked.
d. Make up a solution by dissolving a very small amount of
Na2CO3 and KNO3 in a few milliliters of water. Add 1 mL of 6M
HCl, and test for the flame coloration. Repeat with a fresh
portion, looking through the cobalt glass at the very moment
the loop is introduced into the flame.

2. Reactions of alkaline-earth elements Mg, Ca, and Ba.

a. Because it is difficult to boil solutions in test tubes over open
flames without dispersing out the contents, it is
recommended that at the start of each lab you put some
water to boil in a beaker. You can use this throughout as a
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 26 Chem 157.1: Physical Chemistry I

boiling water bath into which you can place your tubes
whenever directed to heat or boil a solution.
CAUTION: Barium ion is toxic. Wash your hands after
handling.
b. In each of three labeled test tubes, place 0.5 mL (about 10
drops) of each of the solutions MgCl2, CaCl2, or BaCl2. If the
solution is acidic, add one drop of concentrated NH3 to make
it basic and then two drops of the ammonium carbonate
solution (which is 0.5 M (NH4)2CO3 and 1M NH3). Note any
carbonate precipitation.
c. To any of the above solutions in which a precipitate does not
appear, add four drops of 1M (NH4)2HPO4. The precipitate,
which forms, is an ammonium phosphate, having the formula
(M)NH4PO4, where M is the appropriate alkaline-earth cation.
d. Take each solution in which a carbonate has formed and
centrifuge (or filter). Test the supernatant liquid (or filtrate)
for completeness of precipitation by adding a few drops of the
ammonium carbonate solution. Combine any precipitate
formed with that originally obtained. Discard the supernatant
liquid. Add 3 M acetic acid dropwise to the precipitates to
dissolve them. Add half as many drops of 3M-ammonium
acetate to the solutions. Warm gently, and then add 1M
K2CrO4 dropwise until any precipitation of MCrO4 is complete.
Centrifuge and separate. Dissolve any MCrO4 formed in 6M
HCl, and test the resulting solution for flame coloration. (if a
white MCl2(s) precipitate forms in the 6M HCl, centrifuge,
separate, and dissolve the MCl2(s) in distilled water. Test the
MCl2 solution for flame coloration.)
e. In any of the above cases where MCrO4 did not precipitate,
add 3M NH3 dropwise until the solution is neutral or the color
has changed from orange to yellow, and then add about five
drops of 0.25 M (NH4)2C2O4. Heat to boiling and look for a
white precipitate of MC2O4.
3. Analysis of unknown possibly containing Na, K, Mg, Ca, Ba
a. On the basis of observations made in (1) and (2), fill out the
scheme or analysis shown below by writing formulas and
colors of all species formed.

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For instructional purposes only • 1st Semester SY 2020-2021 27

Guide questions and instructions on how to prepare

and submit the laboratory
1. Observe the following instructions in preparing and submitting the
laboratory reports:
A. Create the report in a Letter – sized paper.
B. Download the file entitled Laboratory Report Template and format
uploaded in Moodle classroom and process your report.
C. Do not forget to indicate your name, Course – Year and Time
Schedule.
D. Submit your laboratory reports in our Moodle e-learning page
under the specific exercise classwork. Your instructor will enroll
your names to access the page. Furthermore, reminders will also
be made when deadlines are approaching.
E. Deadline of submission of your laboratory reports will be indicated
in the e-learning page.

References

Cotton, Wilkinson and Gaus. (2002) Basic Inorganic Chemistry, 3rd ed. Wiley
Brown et al. (2002). Chemistry the Central Science.

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Vision: A globally competitive university for science, technology, and environmental conservation.
Mission: Development of a highly competitive human resource, cutting-edge scientific knowledge TP-IMD-04
V0 07-15-2020
and innovative technologies for sustainable communities and environment.
No.