PROTOCOLE 901
The Preparation and Characterization of an X-Type Zeolite
An Experiment in Solid-state Chemistry
Kenneth J. Balkus, Jr., and Kieu T. Ly
University of Texas at Dallas, Richardson, TX 75083-0688
Topics in solid-state chemistry are often neglected in
undergraduate laboratories partly because there are rela-
tively few experiments that capture the attention and
imagination of students. The advent of high-Tc supercon-
ductors that provide dramatic yet simple experiments (1)
has increased interest in solid-state materials. We have
been part of a movement to introduce solid-state chemistry
topics in the advanced undergraduate labs. We report an
undergraduate experiment based on the syntheiis and
charactrrrzat~ono f m X-twe -. zmlite (21.
The synthetic X-type zeolite has the faujasite structure
(3) shown below. Faujasite is the naturally occurring, but
rare, mineral. The general formula is M,i,(A102),(Si02)~9~.n
where n = 77-96 and x = valence of M. The faujasite
structure wnsists of ten cages connected by hexagonal
prisms or double six-ring (D6R)units. The P cages are oRen
called sodalite cages because the structure of the zeolite
sodalite (3) contains eight of these truncated octahedra
connected through the four rings. The vertices in Figure 1
represent either tetrahedral A1 or Si atoms with the 0
atoms omitted f ~ r ~ c l a r i t yThis
. structure transcribes a
sphere of about 12 Awhich we designate a s the supercage.
The 12 ring apertures to the a or supercage are about 7.4
A in diameter. These dimensions allow only certain mole-
cules to be adsorbed by the zeolite.
I n this experiment we will probe the pore size by moni-
toring the adsorption of various molecules. If we view
zeolite as a micropourous silicate in which the Si4+has been
partially substitued with A13t then we realize that for every
A13+there must be an equal number of positive charges
added for balance. The cations that compensate for the
cage
prism
Figure 1. Structure of zeolite X.
positive trivalent charge on Al can be virtually any electro-
positive element, from protons to lanthanides. These cat-
ions can he located throughout the structure. I n fact, there
are more cation sites than cations.
In this experiment we will prepare the sodium form ofan
X-tvoezenlite.Thesodium ionscan then brexchanged with
othk; metal ions such a s cobalt(I1).
We have found the X-type zeolite can be prepared during
a typical lab period and later characterized by infrared
spectroscopy, ion exchange, and adsorption.
Preparation of NaX
Many variables can influence zeolite synthesis: temper-
ature, pH, crystallization time, order of mixing, amount of
Si, Al, Na, and HzO. Zeolite NaX is a metastable phase,
meaning that other types of zeolites such a s P, A, or sodalite
may form if this recipe is not followed carehlly. The proce-
dure detailed below should produce highly crystalline NaX
within a normal lab period (2-4 h) without detectable
contamination from other phases.
The first procedure is to prepare sodium silicate and
sodium aluminate separately. The sources of silicon and
aluminum can vary, but we have found that silica gel
(Aldrich)and aluminumisopropoxide (Aldrich)are suitable
starting materials. Since this experiment requires working
under alkaline conditions, plasticware should be used.
I'olypropylene bottles shouldbe used for the rnstallizatiun
berausr 1hc.v are generdly autoclavnble. Sote: Polyethyl-
ene bottles $11 crick and leak.)
The sodium silicate is prepared by adding 3.0 g of silica
gel, 2.4 g of sodium hydroxide, and 6 mL of deionized water
to a 250-mL plastic beaker. This mixture is swirled until
the solids are completely dissolved. The sodium aluminate
solution is prepared simultaneously by adding 6.9 g of
aluminum isopropoxide, 2.4 g of sodium hydroxide, and 9
mL of deionized water to a 250-mL plastic beaker. The
mixture is stirred with gentle heating (below 80 ' C ) in a
water bathuntil the solids are dissolved (about 10 min) and
a clear gel is formed. A watch glass placed over the beaker
should prevent loss ofwntcr. (Note: The isopropanol furmed
during i h e hydrolysis of aluminum isopropoxide will evap-
orate or form droplets a t the surface. There is no need to
separate the alcohol from the gel.) When both solutions are
a t room temperature, the aluminate solution is added to
the silicate solution. An additional 27 mL of water is added
1
Volume 68 Number 10 October 1991 875
 PROTOCOLE 901
. , a,e,<- ?>,,>c . , < e , < - .!"
. ...*.
0 HOURS -., .".* I ,..... < ,, I .
2 HOURS
3 HOURS
4 HOURS
2000 1400 1000 BOO so0
wavmuuems(cm->)
Figwe 2 FT-IR speclra of zeol~fecrystal zatlon mlxtJre recordeo as
KBr pellets taken alter 0 2, 3 and 4 n.
to the gel and stirred with either a spatula or stir bar until
the mixture appears homogenous.
The gel may take on a variety of appearances, but the
- ".
initial eelatinous mixture will usuallv ouicklv form a sus-
pension of white solids. This mixture is quickly transferred
to a . ". ." screw cao bottle. sealed and laced in
oolwroovlene
an oven a t about 90 "C.
All students should place their samples in the oven at the
same time to minimize the fluctuation in temperature from
opening the oven door. The reaction time will depend on the
lab period. The best results are obtained a t 3 4 h, but
reasonably crystalline zeolites can be isolated after only 2
h. Alternatively, the crystallization can be followed by IR
spectroscopy to achieve the optimal yield (vide infra).
After 2 4 h the mixture is cooled to room temperature,
and the solution is neutralized by washing with much
water. This is best accomplished by transferring the mix-
ture to a beaker, then diluting with water, followed by
suction filtration and further washings. If the high-pH
zeolite solution is transferred directlv to a Buchner funnel
or frit, contamination may result from dissolution of the
oaoer or frit. The white zeolite crvstals mav be air-dried or
bvkdried until the next lab period wbkn the yield of
hydrated NaX zeolite may be calculated.
Characterization of NaX
Probably the best way to identify the zeolite phase and
evaluate the degree of crystallinity is by X-ray powder
diffraction. We followed this experiment using XRD and
found that highly crystalline NaX can be prepared after
only 2 h. More crystalline zeolites were obtained after 4 h.
Unfortunately, many undergraduate chemistry labs do not
876 Journal of Chemical Education
,~,, ,.,:,; have access to this technique. However, ifXRD is available,
" .. students should be referred to JCPDS file no. 38, 237 to
obtain a standard pattern for NaX (4).
The most reliable alternative is infrared s~ectrosco~v
which we can use to identify the zeolite and estima't;, the
(5).
crvstallinitv. Fimre 2 shows a series of s ~ e c t r recorded
a bv
a student durGg the preparation of zeolite X, using KF;
oellets. (Note: Excessive minding of samdes should be
avoided.) We are examininithe mid-IR region only because
the adsorbed water in the zeolite masks the OH reeion.
Without an expensive vacuum IR cell, very little informa-
tion can be obtained from this region. At 1 2 0 M 0 0 cn-'
there are many bands associated with different Si and A1
tetrahedra vibrational modes.
The spectrum for the initial amorphous aluminosilicate
gel (0 h) is a series of broad, featureless bands. There is a
correlation between this broadness and crystallinity: As
crystallinity increases, the bands become more narrow and
better defined. The 4 h spectrum is of a 100% crystalline
sample. A comparison with the starting gel reveals several
bands and shoulders have grown in. These have been
classified as external linkaees or structure-sensitive vibra-
W
tions. The appearance of th&e bands coincides withforma-
tion of the three-dimensional framework. The location of
these bands will shift to higher frequencies as the SiIAl
ratio of the product zeolite increases, but students can use
these spectra as a guide.
In Figure 2 the main asymmetric stretch is a t 982 m-'
with a shoulder at 1053 cm-'. The symmetric stretches
occur at 748 and 670 m-' with a weak shoulder at 689 cm-'.
The band a t 560 cm-' is associated with the double 6 rings
that connect the sodalite cages. A TO4 bending vibration
400 occurs at 456 m-'.
If an impurity phase did hystallize, it should be fairly
easy to identify by IR. The key area to monitor is the
double-ring region. Common phases that might appear as
impurities include zeolites P and sodalite which both lack
double-ring structural units (3).Therefore, there should be
no IR bands near 560 em-' for these phases. Zeolite P has
a characteristic band at 600 cn-'; sodalite, at 660 cm-'. If
-
zeolite A were an imouritv the double-rinevibration would
A
shift to a lower wave number (about 550-cm-') relative to
of D ~ units.
R
-
X-tvoe zeolites because it has double four-ring units instead
Ion-Exchange Properties
One of the characteristic properties of zeolites is their
ability to ion-exchwe cations. The combinationof Si4+and
A13+ results in a deficiency of positive charge which is
balanced by exchangeable cations. In a simple test we can
determine if the above product has ion-exchange capabili-
ties.
In a 250-mL Erlenmeyer flask dissolve 0.1 g of cobalt
chloride in about 100 mL of deionized water. Then add 1g
of the product zeolite and stir until the pink solution is
decolorized.Times will vary, but heating greatly facilitates
this process, so complete exchange can be accomplished in
less than anhour. After filtration, wash with water and test
the washings for NaCl with a AgN03 solution.
If the zeolite is pink and if the filtrate is colorless but
contains NaC1, the product has ion-exchange properties.
Ideally two Na+ions will exchange for every COZ+,as shown
in eq 1. In reality a stoichiometric exchange is unlikely
because different cobalt species are possible. For example,
a Cl- or OH- ligand might be coordinated to the metal ion,
with one Na+ exchanged, to maintain electroneutrality.
One can imagine how this ion-exchange property could
be exploited commerciallyto soften water or to remove toxic
or radioactive metal ions from water.
2
 PROTOCOLE 901
Adsorption Properties
If the Co(I1)-exchanged zeolite is allowed to air-dry, it
remains a pink powder, but if the students heat the zeolite
crystals they will eventually turn blueviolet. This change
in color results from dehydration of the zeolite and
illustrates t h e adsorption properties of zeolites. A
suprisingly large amount of water can he adsorbed by
X-type zeolites: Thermogravimetric measurements indi-
cate as much a s 25% by weight. This hydrophilicity is
related to the large internal surface area and the polarizing
ability of the zeolite cages.
Given these strong adsomtion urouerties we can now
probe thedimrnsion;bfthe zholite pores by varyingth~size
of the adsorbinr! molecule. The ahovo strurture of zeolite X
would indicatethat molecules smaller than about 7.4 A Acknowledgment
should he adsorbed. We can use the kinetic diameter (2)to
decide if a molecule will fit through the zeolite pores. For
example, water has a kinetic diameter of 2.65 A, benzene,
5.85 A. We already know water is adsorbed, but we can test
to see if benzene is adsorbed.
Place about 50 mg of dehydrated zeolite into a 1/2-dram
vial or small test tube. Then carefully weigh the vial avoid-
ing fingerprints and place it inside a larger vial. Place both
vials uncapped into a larger vial or beaker that can be
covered tightly. Place a few milliliters of benzene into the
largest vial and cover. After a n hour or so remove the vial
containing the zeolite and weigh.
3
A weight change indicates that benzene was adsorbed
and the pmduct must have pores with diameters of 6 A or
more. This experiment can be repeated with other mole-
cules provided they have significant vapor pressure. Given
the uniform pore distribution of zeolites one can see how
these materials wuld be used a s molecular sieves to adsorb
or exclude molecules by size.
Conclusion
The synthesis of an X-type zeolite is a relatively simple
experiment in solid-state chemistry. I t allows the students
to prepare a commercially important material and thenuse
its physical properties a s a probe of molecular structure.
The synthesis of this zeolite fmm such simple starting
materials is fascinating, and it is fun to realize that ion-ex-
change and selective adsorption studies easily relate the
synthetic product to the interesting three-dimensional
structure of Figure 1.
We thank the Robert A. Welch Foundation and the donors
of the Pretroleum Research Fund administered by the
American Chemical Society for financial support.
Literature Cited
1. Forerample,seeJue~gen~gen,F.H.;EUls.A.B.:DiecLmann,G.H.:Perkins,R.I. JCham.
Edue. 1987.64.851.
2. For an overview of zeolites, see Breck, D. W. &di& Molecuior Siew6; Wiley: New
York, 1974.
3. Meier,W.M.;Olson,D.H.AllasofZ~di~SL~ucfunTyp~s;Butteteorth:London,1988.
4. Pmddd D~ffficfionPila lhorganjr): JCPDS-International Centre for Diffraction
Data: Swarthmare. PA.
5. Flanken, E. M. in Zeolite Chemistry ond Cafalys&;ACS Monograph No. 171,1976,
SO.
Volume 68 Number 10 October 1991 877
 PROTOCOLE 901
The Preparation of Pure Zeolite Nay and Its Conversion
to High-Silica Faujasite
An Experiment for Laboratory Courses in Inorganic Chemistry
Fritz Blalier and Emst Schumacher
Institute for lnorganic. Analytical and Physical Chemistry, University of Bern, Freiestrasse 3, CH-3012 Bern. Switzerland
Every student of chemistry meets the fascinating proper-
ties of molecular sieve zeolites during his or her career. We
encounter them as drying agents, selective gas adsorbents,
ion exchangers, chromatographic media, catalysts, or cata-
lyst supports (I).A large number of interesting experiments
can be performed with the many varieties of commercial
zeolites, e.g., Linde A, X, and Y (2).However, the prepara-
tion of these highly organized porous crystalline systems
remains a mystery tomost users. This does not change dras-
tically when the synthetic and patent literature is examined
(3).
There are many motives for synthesizing zeolites in the
laboratory: Commercial zeolites have unknown chemical pu-
rity and are often crystallographically not well character-
ized. All commercial zeolites are contaminated by heavy
metals, mostly iron, which produce all sorts of artifacts if one
studies EPR spectra of sorbed free radicals (4). Last but not
least: One takes great satisfaction from successfully synthe-
sizing one of these enigmatic substances and from proving
that i t is monophasic, conforms to a specific type of crystal-
lographically well-defined zeolite species, and s h o w all the
expected properties even better than the commercial prod-
uct. Since the architectural variations for assembly of zeolite
structures from the prototype "bricks" ( 5 ) are not yet ex-
hausted by far, it iseven possibleto discover systematically a
new phase with unusual adsorptive properties, e.g., built-in
chiral discrimination.
The published synthesis procedures are mostly uncom-
meuted recipes. Only meager information is given regarding
reaction steps, reaction paths or mechanisms. The impor-
tant reaction parameters are not clearly described, which
creates the reader's impression that the process can hardly
be reproducible. However, recent investigations with novel
tools have led to a better understanding of the reaction
conditions, e.g., MAS (magic angle spinning) NMR of 27Al
and 29Si, light scattering and photon correlation spectrosco-
py of the phase nucleation steps, and computer simulations.
The results allow one to infer what happens and how t o
control the conditions for a specific synthesis. But predic-
tions of how t o proceed for creating new zeolites are still
unreliable (3).
Plannlng a Synthesis
Systematic studies of zeolite preparation involve careful
consideration of the following important areas:
the nature and composition of the reactants and the formation of
precursor species,
nucleation kinetics and crydtal growth,
phase transformations,temperature, and pressure factors.
At least six different zeolites (NaA, NaX, Nay, PI,P2,
CHA) and "mixtures" are obtained in hydrothermal pro-
cesses using the same set of reactants (SiOa, Al, Al2(SO4)8,
NaOH, and HzO) under different reaction conditions (3,6);
on the other hand pure N a y can be obtained by several
procedures. Because subsequent crystal separation is impos-
sible, 100% yield of amonophasicproduct has to be achieved.
4
Zeolite N a y is a synthetic faujasite with an SilAl ratio of
2.4 f 0.8.We eive a simole. reoroducible method. adanted
(n,
f r o m ~ a s a h a r a eal.
t for its preparation from analytically
Dure chemicals. The ~rocedureis based on the senaration of
nucleation and growth processes. Nucleation of ;he desired
seed ia induced in a clear solution with hieh NaOH concen-
tration. The dissolution of aluminum and silica in concen-
trated solutions of NaOH begins with the following reac-
tions:
+
-
or 2 I A l l t 20H- + 6H,O 2[AI(OH)J + 3H,
SiO, NaOH -Na[SiO,OH] dissolved (2)
Condensation leads to the formation of dimeric, trimeric,
and finally oligomeric anions, which are already the struc-
tural subunits of the zeolite. Equation 3 suggests a first
--
condensation step:
Al(OH),- + Na[SiO,OH] Na[(OH),A1+SiOOH] + OH-
+
or Al(OH),- [BO,OHl- [(HO),Al-O-SiOOHI- + OH-
(3)
The surrounding cations compensate the charge of the an-
ionic network and serve as template agents for the three-
dimensional arrangement. All the secondary building units
(SBU) of zeolites have been probed by high resolution FT-
NMR of 27Aland 29Siin the liquid phase, a method that is
powerful enough to discriminate aluminosilicate species
havinguo to 10 Sior A1 atoms (8).The formation of colloidal
particies-is indicated by the decrease of visible light trans-
mittance of the nucleation solution during the aging process.
.. ..
A simple spectrophotometer is adequatefor these measure.
ments. Both methuds combined give strong evidence for the
formation of aggregates with about one unit cell dimension
from the smaller structwal subunits in the clear nucleation
solution.
The clear nucleation solution is mixed with a precipitated
eranular sodium-alumina-silica eel in the ratio 15. Mixine
Gf the two systems (probably) lea& t o a steady state equilib':
rium between dissolution of the a m o r ~ h o u eel
s and further
*
crystal growth. Crystallization a t 92 2 OC needs 24-72 h.
The nucleation solution is decisive for the zeolite obtained,
and small changes of the composition, aging time, or tem-
perature cause remarkable effects on the zeolite crystalliza-
tion process.
Zeollte Nay: Experlmenial Procedure
For all theswpa w be described below laboratory glassware has to
be avoided. Polyethylene or polypropylene flasks with tight screw
caps have to b~ applied. Why?!
Nucleation
Solution A (eq 1) is prepared by dissolution of 1.35 g (0.05 mol)
metallic A1 (99.999%obtained from Alusuisse) in a solution of 15.0g
(0.375 mol) best purity NaOH in 35 mL distilled water. Solution B
(eq 2) is produced by dissolving 15.0 g (0.25 mol) dry SiOn(Fluka No.
Volume 67 Number 6 June 1990 519
 PROTOCOLE 901

60780) in 15.6 g NaOH in 35 mL distilled water. Both solutions are

*
mixed in polyethylene flasks in an oil thermostat at 42 3 'C and
aged for 90 10 min at the same temperature. This is the "nucle-
ation solution" wherein the formation of seed structures takes place
as has been proved withlight-scatteringexperiments (7).The nucle-
ation solution should he clear after the given time of aging. If some
turbidity is left, the concentration of sodium hydroxide has heen too
low or sodium carbonate is a contaminant,
The Aiuminosilicete Gel
Solution C is 31.5 g (0.05 mol) Alz(S0A (Merck p.a.1 dissolved in
125 mL water, and solution D consists of 30.0 g SiOz and 16.0 g
NaOH dissolved in 75 mL HzO. Then D is slowly poured into C
under vigorous stirring while the granular sodium-alumina-silicate
gel precipitates,which is subsequently washed with cold water. The
washed gel is transferred to a polypropylene flask and water is
admitted to 180 g total weight.
Wex apparaNs tor Hw Mment of zeolltes wlth SlC14vapor: (I) and (4) cold
The Ctystai Growth Process traps, (2)ooldtrap with breakseal ampule, (3)reactlonvessel, (5)RoNlex 1919
The formation of zeolite crystals from the small snbunita formed ccnnenlons, (6)breakseal ampule with SiC14,(7) iron bar.
in the nucleation solution occurs in a gel with defined molar compo-
+
sition: 30 g of the nucleation solution (A + B) are added to (C D),
and, after mixing well, the gel is distributed in two flasks,which are
kept in a drying oven at (92 r 2 "C). The composition in mole % of (I =
+ + 1')'"
An(hZ kZ
the reactant eel is now: HgO: 88.45%.NaOH: 5.70%.SiO?: 5.26%.Al: 2 sin 8
~ ~~
~.~~ is controlledh;~-ravdiffraction after 24 h bv
0.59%.~rvst&ization
~ ~,
where n = 1, 2, 3,. . . , a = unit cell length, X = X-ray
taking the samples directly from ;he Re:; as urually20-30 h is
sufficient for complete reaction, the gel is filtered and washed with waveleneth. and B = Braze anele. Both elementarv cell oa-
boiling water as soon as the X-ray analysis shows a crystalline rametersare ohtained wiihhigh precisionso that t<eshrink-
product. The result is zeolite Nay of high purity with an average ape of the unit cell of the Si-exchanged zeolite can be used to
crystal diameter of approximately 0.9 pm. estimate the SiIAI ratio with help of literature data (9). The
difference of 2% between the two unit cell constants is
Hlgh-Slllca Zeollte caused by the different bond lengths dsi.0 = 1.61Aand d~1.0
In a second exoeriment the svnthesized zeolite Y (SilAl- = 1.69 A. MID-IR spectroscopy from 300-1400 em-' is also
2.5) is converted to high-silica'faujasite with ~ i l ~ l ' r a t of
io well suited to the orobine of structural alterations in zeolite
-100 or even more. if it is treated with silicon tetrachloride frameworks. T h e bands i f both zeolites show a 1:l correla-
vapor (9) a t 450 OC: T h e reaction
xSiC1, + Na5,(Al0,),,(SiOz),,, - Na,,(AlO,),,-,(Si0~),36tl
+ rNaCI+ zAlC13 (4)
tion with each other and band assignments should be made
(9). T h e higher ordering of the lattice atoms and the unit cell
contraction lead to sharper absorption bands and shifts of
approx. 8%to higher frequencies in the modified form. For
is a substitution of the lattice Alnl of the zeolite by SiN with reproducible X-ray diffraction and (optional) thermogravi-
a n almost c o m ~ l e t emaintenance of the crvstal structure. metric analysis standardized humidity conditions are neces-
.&l3 volatilizes from the zeolite phase and condenses on the sary, e.g., by keeping the zeolites in a desiccator over a
elass surface: NaCl or nonvolatile NaA1C14 is leached with saturated MgClz solution. X-ray diffraction and IR analysis
water. show that the crystal structure is well preserved and that
only a small part of the degree of crystallinity is lost during
Experlrnental the exchange reaction.
SiClr is previously distilled into breakseal tubes; each tube should
contain approx. 5 mL of liquid SEl+ On the basis of the tube
content one estimates the stoichiometric quantity of Nay to weigh Conclusions
into the reaction vessel 3 (figure) from eq 4. For complete AlISi
exchange a 10-20% excess of SiCln is recommended. Pedagogically valuable characterizations and interpreta-
The Pyrex apparatus is connected as indicated in the figure, and tions are possible with the zeolite conversion experiment:
the breakseal tube is attached to the cold trap 2. The zeolite is
sufficientlydried in a flow of pure Nz(g)(2 bat 450 O C after predry- Determination of the cubic unit cell constant by powder X-ray
ing in an oven). Cold trap 1is cooled with liquid Nz. The breakseal diffractometry;a reference substance, e.g., sodium chloride, is to
ampule is opened with the iron bar 7 and a magnet. Cold trap 4
might be cooled with liquid nitrogen, or, if not, the gas flow (approx.
1mL1s) is led into a NaOH solution to remove the unreacted SiCL.
. he used for precise determination.
The size of the unit cell is connected with the bond lengths.
IR spectroscopy is sensitive for hond lengths in macromolecular
The SiCL input is regulated by the gas flow or the ampule aperture. systems, and highly symmetric structural subunits are proved.
The complek reaction takes appron. 4 h, and then the oven tem. The zeolites prepared are adequately identified by X-ray
prrature is slowly diminished from 450 'C to 200 ' C in 1 h; the
oroduct is washed with0.01 M HCIor NH.CIsolutronand hot water, diffractometry and solid state IR. Scanning electron micros-
hried at 110 "C, and investigated with IR spectroscopy (1-3% in copy, determination of adsorption isotherms for different
KBr) and Debye-Schemer powder X-ray diffraction. substances, and thermogravimetric analysis are additional
tools to reveal the large physicochemical differences be-
Results and lnterpretatlon tween the two zeolites. Most important are the hydrophobic
The DebyeScherrer diffraction pattern allows one to de- nature. Brdnsted aciditv of the H+ form. adsorotion heats.
termine the unit cell parameters of both zeolites N a y and and therefore catalytic-properties. ore over,
t h e synthe:
the modified high-silica form. T o every diffraction line sized zeolite N a y is free from paramagnetic impurities and
Miller indices (h. . . k.. 1). can be assiened. Thev are found to be therefore adequate for research purposes. EPR measure-
either odd or even and not of &xed parity, e.g., (331) or ments of small metal clusters in zeolites are possible even if
. .. but not (321). This moves the presence of a face-
(242). very weak signals result from the metallic particles (4).
centered cubic lktice (spacegroup ~ 3 d k )From . the diffrac- All experiments have been checked by the students of the
tion anele B we extract the elementary cell length according second-year course in inorganic chemistry a t the University
to ~ r a g g ' law
s (9--11): of Bern.
5
520 Journal of Chemical Educatlon
 PROTOCOLE 901

Acknowledgment
.
.... - . . --
H.stud. surf. SC;. c n i . 1~81,24,107-128.~ar~are~ar,
3. ~echart, R.M. s l u d surf. sei. cot

We thank the SNF grant no. 2.273.86 and the Kommission

zur F6rderung der Wissenschaftlichen Forschung, grant No.
146111211,for financial support, W. M. Meier, Giline Har-
vey, B. Lathy for introduction in the art of zeolite synthesis;
R. Giovanoli, M. Faller, R. Steiner, and Beatrice Frey for X-
ray service and scanning electron microscopy.
Literature CRed
10. Berry, R.8.; dice. S. A,:
Ross,J. ~hya&iChernistry; Wiley: N m Yark. 1980.
11. Buerger. M. J.; Azaroff. L. V . The Pouder Method in X - m y C r y a f d o ~ r a p h y :
1. Bmck, D. W . Zeolitr Molecular Siouas: W h y :NelvYork, 1974. McGrsw-Hill: New York, 1958.
2. ~ ~ w..
~Y.;r j ~i r n a .k~ ward,&
.: ~ i E~S.
. N*W Deu.ropmantainzootite seiowe
Technology; Elsener: Amtfcrdam. 19%.

6
Volume 67 Number 6 June 1990 521