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GEOLOGICA CARPATHICA, JUNE 2009, 60, 3, 263—267 doi: 10.2478/v10096-009-0018-z
Clay minerals from Weichselian glaciolimnic sediments of
the Sępopolska Plain (NE Poland)
JACEK DLUGOSZ
1*
, MIROSLAW ORZECHOWSKI
2
, MIROSLAW KOBIERSKI
1
,
SLAWOMIR SMOLCZYNSKI
2
and RYSZARD ZAMORSKI
3
1
Department of Soil Science and Soil Protection, University of Technology and Life Sciences, Bernardynska St. 6, 85-029 Bydgoszcz,
Poland;
*
jacekd@utp.edu.pl
2
Department of Soil Science and Soil Protection, University of Warmia and Mazury, Plac Lodzki 3, 10-957 Olsztyn, Poland
3
Department of Biochemistry, University of Technology and Life Sciences, Bernardynska St. 6, 85-029 Bydgoszcz, Poland
(Manuscript received February 22, 2007; accepted in revised form October 23, 2008)
Abstract: Glaciolimnic deposits sampled from three sedimentation reservoirs located on the Sępopolska Plain (north-
eastern Poland) were investigated. The material under study was deposited in the recession phase of the Pomeranian
phase of Vistula (Weichselian)
glaciation. The clay fraction was separated by centrifugation after preparation according
to Jackson. Mineralogical investigations were done by X-ray diffraction. The analysed deposits had a similar complex
composition of clay minerals. The main components were illites mixed with the illite/smectite mineral with percentages
< 10 % S. Another part were minerals of the illite/smectite type which had differentiated content of smectite layers
(mainly 80—90 % S). There were also chlorite minerals, probably as mixed layer minerals of the chlorite/vermiculite
type or HIV with a negligible amount of chlorite layers. The results indicated that all the deposits were of the same age
as well as similar deposited material and the samples are different from typical Pomeranian till and typical limnic
material of the same age. Small differences observed among the deposits of specific sedimentation reservoirs were
probably the result of later processes.
Key words: Late Pleistocene, north-eastern Poland, glaciolimnic sediments, clay minerals.
Introduction
Young glacial areas of northern Europe with diversified
surface features are covered with different materials, such
as till, limnic and fluvioglacial materials (Björck &
Möller 1987; Ringberg & Erlström 1999; Krzywicki
2002; Ber 2006). Apart from diversification due to the
deposition process those materials underwent transforma-
tions during the post-deposition period, which of course
affected their properties. It can be seen both in their mor-
phological, granulometric and petrographic properties, as
well as in the mineralogical composition of their clay
fraction. As has been proved by numerous researchers,
clay minerals contained in that clay fraction of limnic,
glacial and glaciolimnic materials can be an index for the
origin of those materials; as well as processes in which
they transformed during the post-deposition period
(Stankowska 1979; Peuraniemi et al. 1997; Ringberg &
Erlström 1999; Kalinenko 2001; Dlugosz 2002).
The objective of this study was to determine and compare
composition of clay minerals from glaciolimnic materials of
various sedimentation reservoirs. Another aim was to com-
pare the set of clay minerals of a glaciolimnic deposit with a
limnic and glacial deposit of the same age.
Material and methods
The study site is located on the Sępopolska Plain (north-
eastern part of Poland), a southern part of the Staropruska
Lowland. It is a basin 40—50 m high in the central part and
80—100 m near the edges (Kondracki 2000). The major part of
this area is covered with very diversified glacial till deposited
over the Pomeranian phase of the Vistula (Weichselian) glaci-
ation period (Ber 2006) and also fluvioglacial and limnic cre-
ated during the continental ice-sheet recession of the
Pomeranian and Holocene phases. On a large area of the
Sępopolska Plain, the top part of the glacial till becomes gla-
cial clay because of outer-layer variety that was deposited in
water through small short-lived water ponds. These ponds ex-
isted on the continental ice-sheet forefield as a result of lack of
possibilities of glacial water runoff (Slowinski 1975). The
thickness of these deposits usually reaches several meters.
Fig. 1. Localization of the investigated samples.
264
DLUGOSZ, ORZECHOWSKI, KOBIERSKI, SMOLCZYNSKI and ZAMORSKI
Four samples of glacial clay were collected for mineralogi-
cal analyses. The sampling sites were located near the fol-
lowing villages: Rownina Gorna – 54°10’48.3” N,
21°14’9.10” E (samples 1 and 2), Troksy – 54°03’16.4” N,
21°04’22.0” E (sample 3) and Silginy – 54°15’51.0” N,
21°12’22.0” E (sample 4) (Fig. 1). The samples represented
3 separate basins where the deposition took place. The sam-
pling was done at the depth of about 1 m where no influence
of pedogenic processes were observed. As for their texture,
we analysed it according to the USDA classification. The
samples represented different textures and were finally clas-
sified as: samples 1 and 3 – clay loam, sample 2 – silt clay
loam, sample 4 – clay. The full particle size data of the
analysed samples are given in Table 1. The pH of the sam-
ples varied little, and did not exceed the range 6.1—7.0 (Ta-
ble 1). All the samples were gleyed. This process was found
strongest in the case of sample 4.
The clay fraction (< 2 µm) for mineralogical investigations
was separated by the Beckman centrifuge after dispersion
with Na-ionite (Amberlite 120) (Gonet & Ciesla 1988). Prior
separation of the samples was done according to Jackson’s
method (Jackson 1975) that was used to get rid of peptizing
components (CaCO
3
, organic matter and free iron oxide).
The mineralogical composition of the clay fraction was as-
sessed by X-ray diffraction using the HZG – 4 instrument
with a CuK
α lamp and nickel filter. For this analysis, sam-
ples of specific fractions were saturated with Mg
2+
ions
(Mg), then solvated with ethylene glycol (Mg + EG), and K
+
ions. Next, the samples were heated to 300 and 550 °C.
These were oriented preparations obtained from a water sus-
pension by sedimentation. The results were used for qualita-
tive analysis, as well as the mixed layer minerals illite/
smectite structure as described by Srodon (1980, 1981,
1984). The fitting of the experimental data was done using
ORIGIN 7.0 software, which similarly to Lanson’s DECOM-
PXR software, is based on the Gauss and Lorentz functions
(Lanson & Velde 1992). The programme reconstructed single
peaks by fitting the envelope curve of overlapping peaks.
Results
The mineralogical analysis of the clay fraction (< 2 µm)
from the glaciolimnic materials under study, showed very
complex compositions with a great deal of similarity. The
main minerals were illite minerals which were mixtures of il-
lites and illites/smectites with a low content of smectite lay-
ers (up to 20 %). It was demonstrated as the calculated Ir
index (Ir = the intensity ratios of 001 and 003 reflections
Particle-size fraction (mm)
pH
Sample
number
2–1 1–0.5 0.5–0.25 0.25–0.1 0.1–0.05 0.05–0.002 <
0.002
Texture*
H
2
O KCl
1
0.0
7.0
14 3
6 32 38 CL
7.2
6.1
2
0.0
4.0
2
2
7
51
34
SCL
7.0
6.2
3
0.0
1.0
5
3
15
48
31
CL
7.5
6.9
4
0.0
0.0
0
1
2
19
78
C
6.8
6.1
* — texture according to USDA classification.
Table 1: Texture and pH of the investigated samples.
Fig. 2. X-ray diffractograms of the clay fraction of the analysed sam-
ples saturated with Mg
2+
and solvated with ethylene glycol (EG).
Fig. 3. X-ray diffractogram of the clay fraction of sample No. 3
(from Troksy) saturated with Mg
2+
and solvated with ethylene gly-
col (EG) in the range 3—11° 2
θ CuKα. Bold line represents the fit-
ted envelope curve, broken line – reconstructed picks, while fine
full line represents experimental data.
from the air-dried and glycolated samples) (Srodon 1984).
This was demonstrated as reflexes 1.00, 0.500 and 0.334 nm
in preparates saturated with magnesium ions (Mg
2 +
). They
265
CLAY MINERALS FROM WEICHSELIAN GLACIOLIMNIC SEDIMENTS (POLAND)
Fig. 4. X-ray diffractogram of the clay fraction of sample No. 2 (from
Rownina Gorna) saturated with Mg
2+
and solvated with ethylene gly-
col (EG) in the range 15—20° 2
θ CuKα. Description as in Fig. 3.
Fig. 5. X-ray diffractogram of the clay fraction of sample No. 3
(from Troksy) saturated with Mg
2+
and solvated with ethylene gly-
col (EG) in the range 15—20° 2
θ CuKα. Description as in Fig. 3.
were shifted from 1.00 to 0.998 nm (001) and from 0.500 to
0.498—0.499 nm (002) in magnesium preparations solvated
with ethylene glycol (Mg
2+
+ EG) (Fig. 2). Another compo-
nent also found in the samples was highly concentrated swell-
ing minerals, such as smectites characterized by thinner layers
or mixed-layer minerals of the illite/smectite type containing
80—90 % of smectite layers. Swelling minerals occurred in the
clay fraction separated from all the analysed samples. Their
presence was recorded as reflexes 1.66—1.67 nm (Figs. 2, 3),
0.932 nm (Fig. 3), 0.559 (Figs. 4 and 5) and 0.279—0.281 nm
(Figs. 6 and 7) in the Mg
2+
+ EG preparations. In addition, re-
flexes indicating the existence of minerals from the illite/
smectite type of 80—90 % S in some of the investigated clay
fractions reflexes 0.521 nm (Fig. 5) and 0.262 nm (Fig. 6)
were recorded probably coming from illite/smectite minerals
of 20—25 % S (samples 1 and 3) as well as reflexes 0.506 nm
(Fig. 5) and 0.245 (Fig. 6) suggesting the occurrence in sam-
ples 1 and 2 of minerals of the illite/smectite type of 15 % S.
The third main component of the clay fraction for the sam-
ples under study was minerals containing vermiculite layers
with a small amount of chlorite minerals. A very small reflex
1.43 nm in the K
+
and K
+
300 (Figs. 7, 8) preparations indi-
cated a negligible amount of pure chlorites. The occurrence of
mixed-layer minerals containing chlorite layers was demon-
strated as reflexes recorded within the range 0.473—0.483 nm
in the Mg
2+
+ EG preparations (Figs. 2 and 4). Probably these
were mixed-layer minerals of the chlorite/vermiculite type
with a high but diversified amount of vermiculite or hy-
droxy-interlayered vermiculite (HIV) layers. The latter con-
clusion was based on the observation that the shift of the
Fig. 6. X-ray diffractogram of the clay fraction of sample No. 2 (from
Rownina Gorna) saturated with Mg
2+
and solvated with ethylene gly-
col (EG) in the range 30—35° 2
θ CuKα. Description as in Fig. 3.
Fig. 7. X-ray diffractograms of the clay fraction of the sample No. 3
(from Troksy).
266
DLUGOSZ, ORZECHOWSKI, KOBIERSKI, SMOLCZYNSKI and ZAMORSKI
reflex from the 001 band identifying that compounds in the
K
+
and K
+
300 preparations did not come to 1.00 nm in full,
allowing a broad reflex in the range 1.4—1.1 nm (Figs. 7 and
8) (Barnhisel & Bertsch 1989; Pai et al. 2004). An additional
observation supporting this conclusion was a lack of the re-
flex at 0.7 nm in the K
+
550 preparation. The broadening of
the reflex in those preparations was also caused by the
presence of minerals of the illite/smectite type in the clay
fraction because minerals of this kind undergo natural collap-
sation (Jackson 1963). There was no chance for the occurrence
of the chlorite/smectite type because in the Mg
2+
+EG prepara-
tions there were no reflexes of the 0.714—0.852 nm range
that corresponded to the 002 band minerals of this type. Ka-
olinites were present in all the samples as accessoric miner-
als, what was shown as a reflex at d = 0.234—0.238 nm and
the lack of the reflex at 0.7 nm in the K
+
550 preparation
(Fig. 9).
Discussion
Despite the origin of separate sedimentation basins, the
mineral composition of the clay fraction from the glaciolim-
nic material under study showed a high similarity. The main
components identified were mixed layer minerals of diversi-
fied structure as well as illites mixed with well-ordered min-
erals (IS) of the illite/smectite type (less than 10 % S).
Minerals of the illite/smectite type from various contents of
smectite layers (ranging 80—90 % S) as well as chlorite/ver-
miculite from the vermiculite layers, superiority dominated
in the group of mixed-layer minerals. In addition, the pres-
ence of partly-ordered minerals (IS/ISII) from the illite/
smectite type (20—25 % S) was observed in the material sam-
pled at Rownina Gorna and Troksy, as well as well-ordered
of the IS type (about 15 % S) in the deposit of Rownina Gor-
na. Only the clay fraction from Silginy did not contain min-
erals of the illite/smectite type with a low content of smectite
mixed layers. The latter composition was very clearly differ-
ent from the mineral composition of the glacial material (till)
from the Pomeranian phase of the Drawskie Lake District.
This lake region is known for showing a high content of illite
minerals in the clay fraction without vermiculite minerals,
accompanied by a very small percentage of smectite layers
(Dlugosz 2002). Glaciolimnic material from south-eastern
Sweden deposited in the late Weichselian glaciation period
investigated by Ringberg & Elström (1999) also contained a
clay fraction composed of a high percentage of illite without
traces of vermiculite layers, whereas, material of the glacial
till from northern Finland analysed by Peuraniemi et al.
(1997) and by Soveri & Hyyppä (1966) (glacial clay of
southern till from Finland) demonstrated a high content of
vermiculite of chlorite layers. However, the comparison of
the percentage from smectite layers in the studied material
showed that it was similar to glacial deposits of the Poznan
and Leszno phase of the Weichselian glaciation period
(Stankowska 1979; Dlugosz 2002). The results indicated that
the main minerals in the composition of the clay fraction of
the deposits under study are the residues of the parental ma-
terials of that sediment. The lack of effects of post-sedimen-
tary processes was confirmed by a poor acidity of the
investigated material, which does not promote the develop-
ment of vermiculite layers. These minerals are formed over
the process of the leaching of alkaline ions at much lower pH
(4—5) (Vincente et al. 1977; Katarhansis 1988; Matsue &
Wada 1989). Another reason that these minerals did not oc-
cur in glaciolimnic sediments was a lack of oxidoreductive
conditions, necessary for their creation because these condi-
tions provide the Fe
3+
ions composing them (Vincente et al.
1977; Douglas 1989). That is why mixed-layer minerals con-
taining vermiculite layers found in the clay fraction of the
glaciolimnic deposits under study could be chlorited vermic-
ulites developed during weathering of biotite in the sequence
biotite
→ vermiculite → chlorited vermiculite (Barnhisel &
Bertschel 1989) or minerals of the chlorite/vermiculite type
could be an intermediate product in the transformation of de-
trite chlorites to smectites (Senkayi et al. 1981). However,
mixed-layer minerals of the illite/smectite type can already
be the product of diagenesis of glaciolimnic material. During
Fig. 8. X-ray diffractograms of the clay fraction of sample No. 4
(from Silginy).
Fig. 9. X-ray difractograms of the clay fraction of analysed samples
saturated with K
+
and heated to 550 °C.
267
CLAY MINERALS FROM WEICHSELIAN GLACIOLIMNIC SEDIMENTS (POLAND)
this process illites occurring in the sediment underwent de-
potassication, which could be promoted by the reaction of
pH 6—7 assayed in that sediment (Ismail 1970; Crawford et
al. 1983).
Conclusions
The results showed a high uniformity of the clay fraction
in the glaciolimnic material from the deposit basins under
study. The composition of the clay fraction of those deposits
indicated that it was formed mainly from the glacial material
(till) of the Poznan phase of the Weichselian glaciation. The
remaining part was constituted of the very fine limnic mate-
rial of the Pomeranian phase. A small variability among the
samples of specific basins was caused by the processes form-
ing smectites during the post-sedimentation period. Howev-
er, the assessed composition of the clay minerals suggested
an origin of the investigated materials different from typical
Pomeranian glacial till as well as typical limnic material
from the same age. However, it should be clearly stated that
our conclusion for these differences needs further study on
the mineralogical composition of the clay fraction of miner-
als, both from this type and typical glacial till and limnic
clay from the Staropruska Lowland.
Acknowledgment: The study was supported by the Polish
Ministry of Science and Higher Education, Grant No.
2776/B/P01/2007/33.
References
Barnhisel R.J. & Bertsch C.J. 1989: Chlorites and hydroxy-interlay-
ered vermiculite and smectite. In: Dixon J.B. & Weed S.B.
(Eds.): Minerals in soil environments. Soil Sci. Soc. Amer.,
Madison, Wisconsin, 729—788.
Ber A. 2006: Pleistocene interglacials and glaciations of northeast-
ern Poland compared to neighbouring areas. Quat. Int. 149,
12—23.
Björck S. & Möller P. 1987: Late Weichselian environmental histo-
ry in south-eastern Sweden during the deglaciation of the
Scandinavian ice sheet. Quat. Res. 28, 1—37.
Crawford T.W. Jr., Whitting L.D., Begg E.L. & Huntington G.L.
1983: Eolian influence on development and weathering of
some soils of Point Reyes Peninsula, California. Soil Sci. Soc.
Amer. J. 47, 1179—1185.
Dlugosz J. 2002: Differentiation of the composition of clay miner-
als in fine clay fraction (< 2 µm) of Alfisols formed from gla-
cial till. ATR, Bydgoszcz, 1—104 (in Poland).
Douglas L.A. 1989: Vermiculites. In: Dixon J.B. & Weed S.B.
(Eds.): Minerals in soil environments. Soil Sci. Soc. Amer.,
Madison, Wisconsin, 635—674.
Gonet S.S. & Ciesla W. 1988: Methods for disperging soil samples
for studies of clay fraction. Prace komisji Nauk PTG, Warsza-
wa 103, 17—299 (in Poland).
Ismail F.T. 1970: Biotite weathering and clay formation in arid and
humid regions. Soil Sci. 109, 287—261.
Jackson M.L. 1963: Aluminum bonding in soils. A unifying princi-
ple in soils science. Soil Sci. Soc. Amer. Proc. 27, 1—10.
Jackson M.L. 1975: Soil chemical analysis – advanced course. 2nd
edition. Published by the author, Madison, Wisconsin, 1—895.
Kalinenko V.V. 2001: Clay minerals in sediments of the Arctic
seas. Lithology and Mineral Res. 36, 362—372.
Katarthansis A.D. 1988: Compositional and solubility relationships
between aluminum-hydroxyinterlayered soil – smectites and
vermiculites. Soil Sci. Soc. Amer. J. 52, 1500—1508.
Kondracki J. 2000: Regional geography of Poland. PWN, Warsza-
wa, 46—58 (in Poland).
Krzywicki T. 2002: The maximum ice sheet limit of the Vistulian
Glaciation in north-eastern Poland and neighbouring areas.
Geol. Quart. 44, 165—188.
Lanson B. & Velde B. 1992: Decomposition of X-Ray diffraction
patterns: a convenient way to describe complex I/S diagenetic
evolution. Clays and Clay Miner. 40, 629—643.
Matsue N. & Wada K. 1989: Source minerals and formation at par-
tially interlayered vermiculites in dystrochrepts derived from
Tertiary sediments. J. Soil Sci. 40, 1—7.
Peuraniemi V., Aario R. & Pulkkinen P. 1997: Mineralogy and
geochemistry of clay fraction of till in northern Finland. Sed.
Geol. 111, 313—327.
Ringberg B. & Erlström M. 1999: Micromorphology and petrogra-
phy of late Weichselian glaciolacustrine varve in southeastern
Sweden. Catena 35, 147—177.
Senkayi A.L., Dixon J.B. & Hossner L.R. 1981: Transformation of
chlorite to smectite through regularly interstratified intermedi-
ates. Soil Sci. Soc. Amer. J. 45, 650—656.
Słowański W. 1975: Commentaries to geological map of Poland.
Wyd. Geol., Warszawa, 50—52 (in Poland).
Soveri U. & Hyyppä J.M. 1966: On mineralogy of fine fractions of
some Finnish glacial tills. State Inst. Technical Res., Finland
Publ. No. 113, 1—31.
Srodon J. 1980: Precise identification of illite/smectite by X-ray
powder diffraction. Clays and Clay Miner. 28, 401—411.
Srodon J. 1981: X-ray identification of randomly interstratified il-
lite/smectite in mixture with discrete illite. Clay Miner. 16,
297—304.
Srodon J. 1984: X-ray powder identification of illitic materials.
Clays and Clay Miner. 32, 337—349.
Stankowska A. 1980: Stratigraphic and regional variation of glacial
tills in Poland in the light of clay minerals investigations. In:
Stankowski W. (Ed.): Tills and glacigene deposits. Zesz. Nauk.
UAM, Poznan 20, 57—65.
Vincente M.A., Razzaghe M. & Robert M. 1977: Formation of alu-
minum hydroxy vermiculite (integrate) and smectite from mica
under acidic conditions. Clay Miner. 12, 101—112.