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Fig. 5. Average crystals from the microscopic preparations; each prepara-
tion is represented by the mean length and the mean breadth of the crystals.
The numbers indicate the sequence of volume.
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SETTING EXPANSION OF GYPSUM 241
tions, since it was found that the majority of them could be
readily distinguished from each other by microscopic inspection
(cf. Fig. 10).
RESULTS AND DISCUSSION
The results of the measurements and of some of the calcula-
tions are collected in Table 5, while Fig. 5 shows the average
crystals in profile seen from the b face.
An examination of the measurements with the view of stati-
stical treatment showed in most cases no normal distribution, so
it was with some hesitation that the statistical calculations listed
in Table 5 were carried through (it can be noted, f. ex., that in
many cases the standard deviation amounts to more than one
third of the corresponding mean value). A mathematical analysis
of co-variations had to be abandoned owing to the abovemen-
tioned type of distributions.
I t must be warranted, however, to make a graphical analysis
of co-variations, though it must still be borne in mind that the
co-variants fail to form normal distributions.
The analysis shows that there is no correlation between on the
one hand the setting expansion, and on the other ( 1) the mean
length of the crystals, Fig. 6, (2) the end face area of the cry-
EXD. %
Fig. 6. The relation between the mean length (M) of the crystals and t he
setting expansion.
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212
E m %
KNUD DREYER JBRGENSEN
)O A
Fig. 5. The relation between the end face area of the crystals per unit
volume of dihydrate ( A) and the setting expansion.
stals per unit volume of dihydrate, Fig. 7, or (3) the sum of
breadth + breadth + length per unit rolunie of dihydrate.
The setting expansion was well correlated, however, both with
the number of crystals per unit volume of dihydrate (Fig. 8) and
with the end face periphery per unit volume of dihydrate (Fig. 9) .
In 1961 Jlrgensen described a hypothetical model to explain
setting expansion and expansion pressure of gypsum. The model
built on the assumption that an excess pressure would arise in
the liquid in the narrow slit between two growing crystals, and
that the magnitude of this pressure, and accordingly of the set-
ting expansion, would be (1) inversely proportional to the sum
of the slit peripheries present per unit volume of dihydrate, (2)
directly proportional to the viscosity of the liquid, and (3) di-
rectly proportional to the setting rate (rate of crystal growth).
The iiieasurements and calculations reported in the present work
have demonstrated that setting expansion and end surface peri-
phery*) are positively correlated, and there is nothing to indicate
that the degree of setting expansion is dependent on the viscosity
of the liquid or on the setting rate. So the abovementioned hypo-
--
*) This periphery will to a large degree determine the magnitude of the
slit periphery owing to the prevailing growth in length of the dihydratc
crystals.
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SETTING EXPANSION OF GYPSUM 243
Exp. Yo
0.5 E
20 4 1 60 80 100 120 140 160 N
Fig. 8. The relation between the number of crystals per unit volume of
dihydrate (N) and the setting expansion. Experiments with the same ad-
ditive in different concentrations are connected with lines. 1, gelatine. 2,
water of different temperatures. 3, NaNOs. 4, Rochelle salt. 6, NaCI. 6, Na2S04.
7, KrSOd. 8, NaZBd07. 9, sodium citrate.
thesis must no doubt be abandoned. An alternative possibility
is that crystal growth thrust and expansion may result from
thermodynamic movements on the boundary faces between two
united gypsum crystals. Undoubtedly such movements may cause
the molecules and ions of the solution to diffuse into the less
regular interfacial lattice and thereby expand it. A direct proof
of such an assumption cannot be furnished by the data presented
in this work, but for the present it seems the most plausible ex-
planation.
Any factor increasing the number of crystals will also increase
the number of boundary faces and thus the possibilities for
thermodynamic, expanding particle movements. The following
observations are therefore in good accordance with this hypo-
A
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244 KNUD DREYER J6RGENSEN
S
Fig. 9. The relation between end face periphery per unit volume of dihydrate
(S) and the setting expansion. The numbers indicate the same solutions
as in Figure 8.
thesis: (1) If the hemihydrate is crushed before spatulation the
number of dihydrate crystals in the set gypsum will increase,
and so will the expansion. (2) Spatulation prolonged beyond a
certain time will increase the number of crystals and at the same
time, the expansion. (3) Addition of foreign, chemically inactive
powders (here pumice) will give a greater number of interfaces
(here between gypsum and pumice) increasing with increased
fineness of the pumice powder, and a higher expansion will re-
sult. The positive correlation between the setting expansion and
the length of end face peripheries per unit volume of dihydrate
also supports the thermodynamic explanation since the proba-
bility for diffusion of particles into the interfacial lattice must
increase with its extent.
The experiment with addition of dihydrate powder (approx.
30 %> t o the hemihydrate powder in preparation of the slide
specinien gave fewer crystals than pure hemihydra te, while meas-
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SETTING EXPANSION OF GYPSUM 245
urements showed an increased setting expansion for such a
mixture. This apparent departure from the rule that expansion
and number of crystals are positively correlated may probably be
explained in the way that during the spatulation incident to ex-
pansion tests, a comminution of the dihydrate particles occurs
with resultant increase in the number of crystal nuclei.
Besides, the experiments seem to show (see Table 5) that dif-
ferent ions have a specific, different effect on expansion and
crystal number. Thus the effect of the alkali metal ions appears
to be correlated with their order in the periodic system (Li+ is
least effective, K+ and Rb+, most), and of the common anions
Sod-- has evidently a greater effect than NOS-, which again bas
a greater effect than C1-.
Summarized the results of the investigation show that the
various modifiers have a double effect since they influence both
nucleation and crystal proportions. Formation of nuclei, and ac-
cordingly the number of crystals, obviously affects the degree
of setting expansion; on the other hand, the influence of the
crystal proportion on the properties of the gypsum is rather un-
known.
ADDENDUM
In order to study the morphology of gypsum crystals in set
gypsum, test specimens were prepared from mixes made up of
25 g of hemihydrate and 25 ml of expansion modifier solution.
The test samples were examined by incident light by means of a
Leitz Ultropak with a magnification of 220. The purpose of the
investigation was to establish to what degree the crystals in these
preparations differed in appearance from the micropreparations
previously described. The crystal proportions could not be meas-
ured because no single crystals occurred. The crystals in the
various preparations were compared, by simple inspection, with
the crystals in a normal preparation obtained by mixing hemi-
hydrate with water. The same modifiers were used as those set
out in Table 5.
The results showed that only a few modifiers will distinctly
change the growth habits of the crystals (see Fig. 11). Thus, 4 n
NaCl gave very large and coarse crystals; 0.1 n sodium citrate,
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246
KNUD DREYER JflRGENSEN
Fig. 10 a.
flat and very short crystals, much the saiiie as in the iiiicroscopic
specimens; and prolonged syntulation resulted in very minute
crystals.
Certain substances, such as KeSOl and gelatine, produce very
considerable changes in the growth habits of crystals in the
micropreparations, where the relative amount of modifier is
much greater than in the spatulated preparations, but no visible
modifications of the crystals in the latter preparations. This
suggests that such substances disappear during the setting and
probably are built into the gypsum crystals. This incorporation
may take place in the way that molecules or ions of the modifier
are adsorbed on the growing crystal faces and enclosed by ele-
ments of the dihydrate lattice. The adsorption may occur to a
more or less marked degree on the various faces of a crystal
(selective adsorption), and will probably also be able to bring
about changes in the growth rate of the faces, and hence in the
proportions of the crystals.
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SETIING EXPANSION OF GYPSUY
Fig. 10 b.
247
Fig. 10 c.
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148
KS UD DREYER JBRCENSEN
Fig. 10 d.
Fig. 10 e.
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SETTING EXPANSION OF GYPSUM
Fig. 10 f.
Fig. 10 g.
18 - Acta odont. scand. Vol. 21.
249
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250
RS UD DIIETEIi J0RGESSES
Fig. 10 h.
Fig. 10. The effect of growth modifiers on gypsum crystals. Tllc crystals are
grown in distilled water (a), 1 11 Sac1 (b), 0.2 c/ o gelatine (c), 0.2 n
Rochelle s dt (d), 0.1 n sodium citrate (e), and 0.025 n borax Cf),
respectively. (6) shows syngenite crystals grown from hemihydrate in
0.5 II KzSO4. ( h) shows gypsum crystals grown in distilled \niter after mixing
a slurry of 25 ml water and 25 g hemihydrate for one minute.
Jlagnificatinn 150 X.
SZ'MJIARY
The present study was designed to examine whether a rela-
tionship exists between on the one hand the aiiiount of the set-
ting expansion of gypsum as varied, inter alia, by addition of dif-
ferent expansion modifiers, and on the other hand the morpho-
logy of the gypsuiii crystals.
After measurement of single crystals of gypsum in micropre-
parations (see Table 5 ) it could be demonstrated that the setting
expansion is positively correlated with the number of crystals
per unit volume of gypsuni, and with the sum of end face peri-
pheries, likewise per unit volume of gypsum. The expansion is
independent, on the other hand, of the mean length of the
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SETTING EXPANSION OF GYPSUM
Fig. 11 a.
Fig. 11 b.
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135
Fig. 1 1 e.
Fig. 11. Surfaces of gypsum after setting in distilled water (a). 1 n NaCl
solution (b), nncl 0.1 II sodium citrate solution (e), respectively.
Cltropnk, 650 X.
crystals, of the end face area of the crystals per unit volume of
gypsum, and of the sun1 of breadth -t breadth + length per unit
volume of gypsum.
I t is possible that the expansion is due to thermodynaiiiic move-
ments on the boundary faces between united gypsum crystals.
Such rnoreiiients iiiay give rise to diffusion of molecules and ions
into the interfacial lattice and thereby expand it.
Examination of the crystals in preparations of spatulated set
gypsum showed that only exceptionally are their structure and
shape affected by the expansion modifiers.
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SETTING EXPANSION OF GYPSUM
253
HfiSLJMfi
ETUDE SUR LEXPANSION DE PRISE DU PLATRE
Le but de cette dtude est dexaminer sil existe un rapport
entre les deux facteurs suivants: limportance de lexpansion de
prise du plltre pendant ses variations obtenues entre autre par
addition de divers modificateurs dexpansion dune part, et la
morphologie des cristaux de plltre dautre part.
Aprks avoir mesurk des cristaux de platre isoles sur des pre-
parations microscopiques (voir tableau 5) il a 6th possible de
mettre en evidence que lexpansion de prise du plltre est en cor-
relation positive avec le nombre de cristaux par unite de volume
de plltre et avec la somme des peripheries des faces terminales,
calculee de mQme par unite de volume de plltre. Lexpansion est
par contre independante de la longueur moyenne des cristaux,
de la superficie des faces terminales des cristaux par unite de
volume de platre et de la somme: largeur + largeur + longueur
par unit6 de volume de plltre.
I1 est possible que lexpansion soit due B des mouvements ther-
modynamiques sur les faces de jonction des cristaux soud6s entre
eux; de tels mouvements peuvent faire diffuser des molecules et
des ions dans le rkseau plus ou moins irregulier des faces de jonc-
tion, et provoquer ainsi son expansion.
LCtude de la morphologie des cristaux dans des prdparations
de plltre glche et pris a montre quelle ne se trouve quexcep-
tionnellement influencde par les modificateurs de lexpansion.
ZUSAMMENFASSUNG
OBER DIE ABBINDEEXPANSION VON GIPS
Der Zweck dieser Untersuchung war zu untersuchen, inwieweit
ein Zusammenhang besteht mischen einerseits der Griisse der
Abbindeexpansion von Gips, so wie diese u. a. durch Zusatz von
verschiedenen Expansionsreglern variiert, und andererseits der
Morphologie der Gipskristalle.
Durch Messung von Einkristallen von Gips in Mikropriparaten
(siehe Tabelle 5) wurde ermittelt, dass die Abbindeexpansion
positiv korrelat ist mit der Anzahl von Kristallen pro Raumein-
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251 KSCD DRETEH JgIIt i ESSES
heit Gips uiid iiiit der Suiiiiiie ron Endflachenperipherien, eben-
falls pro Rauriieinheit Gips. Dagegen ist die Espansion unab-
hiingig ron der ;\litlellQnge der Kristalle, von deiii Endflachen-
mass der Kristalle pro Rauiiieinheit Gips und ron der Suiiiine
Breite + Breite + LQnge pro Rauiiieinheit (;ips.
Es ist miiglich, dass die Expansion auf therinodgnainische Be-
wegungen in den Grenzflachen zwischen zusaiiiinengewachsenen
Cipskrist:illen zuruckzufiihren ist ; solche Bewegungen kiinnen
eine Diffusion ron Molekeln und Ionen in das weniger regelinas-
sige Grenzflachengitter hinein niit sich fuhren und so dasselbe
expandieren.
Die Untersuchung der Morphologie der Kristalle in Praparaten
von ausgeriihrtein, abgebundenem Gips ergab, dass sie nur aus-
nahmsweise yon Espansionsreglern beeinflusst wird.
REFERENCES
dndrems, H., 1951 : The production, properties and uses of calcium sulpliate
plasters. British Building Congress, division 2, part F, 135-144,
London.
J grgenoen, K. D. h d. S. Porner, 1959: Study of the setting of plaster. .I. dent.
Rcs. 38: 491-499.
J Crgensen, K. U., 1960: The hygroscopic setting expansion of gypsum. Bcta
odont. wand. I f f : 461-475.
-*- 1961: Setting expansion of gypsum. I n J. H. Ue Roer et al. (editors)
Reuclivify of Solids. Proc. 4th inlern. symp. on the reactivity of solids.
Amsterdam. Elsevier Publishing Co.
Mathis, E. H., 1919: A study of the behaviour of plaster of Paris as an in-
vestment in the process of vulcanizing dental rubber. .J. nat. dent. Ass.
6: 132415.
AfcCurtney, E. R. & A. E. Alesander, 1958: The effect of additives upon the
process of crystallisat ion. J. Coll. Sci. 23: 382-3W.
Tschepelewetzki, JI. L. & B. B. J ewslina, 1938: Dynamik des Krystalwachs-
turns und die Veranderungen ilirer ausscren Form am Beispiel des
Gipses und Calciumkarbonats. Reviewed i n Chem. Zentralblatt fO9:
IVeIser, If. B. & F. B. .Iforeland, 1932: The setting of plaster of Paris. J. Phgs.
1307-1308.
Chem. 36: 1-30.
Address: Kpbenhauns TandltPqchdjskole
1G0, Jagtuej, Kbbenhctvn 8
Denmnrk
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