In the Laboratory
Properties of Zeolite A Obtained from Powdered Laundry Detergent
An Undergraduate Experiment
Alison L. Smoot and David A. Lindquist
Department of Chemistry, University of Arkansas at Little Rock, Little Rock, AR 72204
Until recently, sodium tripolyphosphate (Na5P 3O10) was
the preferred builder in laundry detergents. Since phos-
phates stimulate growth of algae in wastewater they have
been replaced in most laundry detergents by the sodium
form of zeolite A (Na-A) (1). Zeolite A acts as a water soft-
ener by cation exchange of its sodium ions for calcium and
magnesium ions. The utility of zeolites extends far beyond
water softening. Zeolites are used in immense quantities as
catalysts for petroleum cracking and isomerization reac-
tions (2). Other applications include their use as desiccants,
selective adsorbents, and ion exchange materials.
In this experiment students are introduced to the
myriad properties of zeolites using Na-A from detergent.
The appeal of this experiment is the study of a useful and
versatile material obtained from a common household prod-
uct. As an extension to the experiments described here one
may synthesize Na-A to compare its properties with those
of the commercial material (3).
Na-A has a high ion exchange capacity because it is an
aluminum-rich zeolite containing approximately equal
numbers of aluminum, silicon, and sodium atoms with an
empirical formula of NaAlSiO4 . The composition of zeolite
A can be varied considerably to form silicon-rich material
by using lesser quantities of aluminum during synthesis.
Silicon-rich compositions have lower ion exchange capacity,
so they are not used in detergents.
The framework of zeolites is based on a simple motif of
tetrahedrally coordinated aluminum and silicon atoms con-
nected by bridging two coordinate oxygen atoms. Figure 1
is an illustration of the cubic unit
cell of zeolite A (4). Each vertex in
the figure represents an aluminum
or silicon atom and each line repre-
sents an Al–O–Si or Si–O–Si link-
age. There are several types of zeo-
lites, but all have the common fea-
ture of a network of internal pores.
The size and geometry of the pores
in a specific zeolite are defined by
the crystal structure. The diameter
of the eight-member ring entrance Figure 1. Zeolite A unit cell.
to the pores in zeolite A is 4.1 Å (2).
The zeolite framework is neutral in charge if composed
solely of silicon and oxygen. However, the zeolite framework
adopts one negative charge for each aluminum incorporated
into the structure, since aluminum has a formal charge of
3+ whereas silicon is 4+. Additional cations are needed to
accommodate the increasing charge with increasing alumi-
num content. In the case of Na-A, these additional cations
are sodium ions residing in the pores. Sodium ions can be
readily exchanged for other cations small enough to fit into
the pores (i.e., <4.1 Å in diameter).
Some Experiments Using Zeolite A
Extracting Na-A from Detergent:
Powdered laundry detergents specifying “aluminosili-
cates” on the ingredients list are those containing Na-A.
Vol. 74 No. 5 May 1997 • Journal of Chemical Education
Since zeolite is the only insoluble component of detergent,
it is isolated by filtering a solution of the detergent followed
by washing of the zeolite with water. The zeolite crystals
used in detergents are very small (≈1 µm), so a fine filter
paper should be used. The weight percentage of Na-A in the
detergent may be determined. Since the zeolite is hygro-
scopic, the powder should be heated to about 400 °C before
weighing.
Water Softening Property of Na-A
The water-softening property of Na-A can be demon-
strated by shaking a large stoppered test tube half-filled
with tap water, 0.25 g of zeolite, and a very small drop of
liquid dish soap. The height of the suds layer formed in the
test tube will be greater than in a similar tube containing
soapy water but no zeolite. The zeolite acts as a softener by
exchanging the hard Ca2+ and Mg2+ ions of the tap water
for Na+.
Desiccant Properties of Na-A
Na-A is hygroscopic, absorbing approximately 20 wt%
of water. This is quantified by first weighing a few grams of
zeolite in a crucible after drying overnight at 400 °C. The dry
zeolite in the crucible then is placed in a humid environment
and weighed again when the mass has equilibrated.
Ion Exchange Properties of Zeolite A
Detergent zeolite has an approximate empirical for-
mula of NaAlSiO4. If Na-A is placed in a solution rich in
Ca2+ ions, then ion exchange yields a zeolite formula of
Ca0.5AlSiO4 . The degree of exchange can be quantified by
determining the decrease in Ca2+ solution concentration af-
ter ion exchange.
The Ca2+ solution for exchange is prepared by dissolv-
ing approximately 15 g CaCl2·H2 O in 200 mL of distilled
water. The solution is standardized by chelometric titration
of Ca2+ with ethylenediaminetetraacetic acid (EDTA) (5). Ti-
tration procedures are found in most standard analytical
chemistry texts.
Exchange then is performed using 100 mL of the stan-
dardized CaCl2 solution to which is added approximately 6
g of accurately weighed Na-A dried overnight at 400 °C be-
fore weighing. The mixture then is stirred for 30 min and
the zeolite powder allowed to settle. An aliquot of the solu-
tion is titrated as before and the degree of ion exchange in
the zeolite determined. For example, 6 g of Na-A (NaAlSiO4)
will accommodate approximately 0.021 mol of Ca2+, corre-
sponding to a formula of Ca0.5AlSiO4 after exchange.
Zeolite HA as a Dehydration Catalyst
Zeolite A will catalyze the dehydration of an alcohol to
form an alkene. To make the zeolite catalytically active it is
converted to its acid form (H-A). The Na+ ions in Na-A are
first exchanged for NH4 + ions by stirring a mixture of a few
grams of zeolite in an ammonium chloride solution (10 g
NH4 Cl in 40 mL H2 O) for one hour. The supernatant solu-
tion is discarded and the zeolite filtered and washed. The
NH4 + exchanged zeolite then is heated overnight in air at
569
In the Laboratory
400 °C to drive off ammonia and make the protonated form
of zeolite according eq 1.
400 °C
NH4+-A → H+-A + NH3
A few grams of zeolite (H-A) are placed in the middle
section of a length of Pyrex glass tubing and held in place
with a loose plug of glass wool on each side of the powder.
Using rubber tubing, one end of the glass tube is connected
to the outlet of a bubbler containing a tertiary alcohol such
as neopentyl alcohol. The inlet of the bubbler is connected
to a nitrogen cylinder. The downstream end of the catalyst
tube is connected to the inlet of a second bubbler contain-
ing mineral oil. To run the reaction, a slow flow of nitrogen
gas is passed through the apparatus while the catalyst is
maintained at about 300 °C. The catalyst can be heated in
a tube furnace or by wrapping the glass tube with a resis-
tively heated electrical tape. The alkene is collected as a so-
lution in the mineral oil bubbler. Progress of the reaction is
noted by the sharp odor of alkene at the outlet and the wa-
ter layer forming in the bottom of the oil bubbler. The dehy-
dration of neopentyl alcohol to 2-methyl-2-butene is shown
below (eq 2).
CH3 CH3
300 °C / N2
CH3CH2 C OH
H+-A
CH3CH2 C + H2O
CH3 CH3
570 Journal of Chemical Education • Vol. 74 No. 5 May 1997
The alkene is characterized by the infrared spectrum
of the oil solution. The salient feature is the olefinic C–H
out-of-plane wagging vibration at 801 cm{1. The C=C stretch
at 1660 cm{1 is very weak. Primary and secondary alcohols
(1) may also be dehydrated by H-A, though not as easily as ter-
tiary alcohols owing to the stability of the tertiary
carbocation intermediate. Most catalytic reactions using
zeolites are designed to take place within the zeolite pores.
The neopentyl alcohol molecule is too large to enter the H-
A pores, but the surfaces of the zeolite crystals are suffi-
ciently active for dehydration.
Acknowledgment
We wish to thank the Student Undergraduate Re-
search Fund (SURF) administered by the Arkansas Sci-
ences Information Liaison Office (SILO) for financial sup-
port of this work.
Literature Cited
1. Zeolites as Catalysts, Sorbents and Detergent Builders; Karge, H.
G.; Weitkamp, J., Eds.; Elsevier Science: Amsterdam, 1989.
2. Hölderich, W.; Hesse, M.; Näumann, F. Angew. Chem. Int. Ed. Engl.
1988, 27, 226–246.
3. Meise, W.; Schwochow, F. E. Advances in Chemistry 121; American
Chemical Society: Washington, DC, 1973; pp 169–178.
4. Broussard, L.; Shoemaker, D.P. J. Am. Chem. Soc. 1960, 82, 1041–
1051.
5. Harris, D.C. Quantitative Chemical Analysis; W. H. Freeman: San
(2) Francisco, 1982; p 284.