Short Note

Extraction of calcified Radiolaria and other calcified

microfossils from micritic limestone utilizing acetic acid
Seyed Mohsen Kariminia
Department of Geosciences, University of Texas at Dallas, P.O. Box 830688, Richardson, Texas 75083-0688
email: smk736@utdallas.edu

ABSTRACT: Micrite nodules are the only source of Radiolaria within the upper Tithonian to Aptian (Upper Jurassic-Lower Creta-
ceous) interval of Great Valley Supergroup (GVS), California Coast Ranges. Radiolaria recovered from GVS micrite nodules are either
calcified or pyritized. This paper describes a method of extracting well preserved calcified radiolaria from micrites utilizing acetic acid.
The same method resulted in the extraction of well preserved Upper Cretaceous planktonic foraminifera from indurated micrite within
the Khoy ophiolitic complex of northwestern Iran; from micrite in the Green Horn Formation, Pueblo Colorado; from indurated chalk in
the Austin Chalk, Dallas Texas, and from indurated micrite in Albian Duck Creek Formation of Texas. The preservation of extracted
radiolaria and planktonic foraminifera from the indurated micrites and chalk is excellent and is often comparable to that found in most
DSDP/ODP samples. Assumedly the clay content of the rock, and the chemical homogeneity of the calcified test are the principal rea-
sons for differential solution of the acetic acid.

TEXT-FIGURES 1-4
1-2. Surface of the rock sample etched with HCl, note the pits on the rock fragments surface, representing calcified radiolarian, and Planktonic
foraminifera dissolved faster than matrix. 3. Radiolarians at the rock surface after dissolving, and removing the disaggregated matrix with this method.
4. Planktonic foraminifera at the rock surface after dissolving, and removing the matrix with this new method.

micropaleontology, vol. 50, no. 3, pp. 301-306, text-figures 1-5, plates 1-2, 2004 301
Seyed Mohsen Karaminia : Extraction of calcified Radiolaria and other calcified microfossils from micritic limestone utilizing Acetic acid

INTRODUCTION Steps in microfossil extraction from micrites utilizing Acetic acid

Until recently it was impossible to extract calcareous
microfossils from micritic limestone. Studies by Lethiers and
Crasquin (1988), Lirer (2000) and Tur et al. (2001) demon-
strated that acetic acid could be utilized to extract calcareous
microfossils (e.g., planktonic foraminifera) from indurated
micrite. Hitherto, most calcareous microfossils in indurated
micrites had to be identified in thin section. During the summer
of 2002 the author independently developed a somewhat differ-
ent method of acetic acid extraction. This technique was born
from the frustration caused by trying to extract calcified
radiolaria from micrite nodules occurring in the Lower Creta-
ceous part of the Great Valley Supergroup (GVS), California
Coast Range (Kariminia, in progress Ph. D. dissertation, Uni-
versity of Texas at Dallas). In the past calcified radiolaria could
be extracted only from GVS micrites using the concentrated hy-
drofluoric acid method of Pessagno (1977).
1. Etch micritic limestone with diluted HCl (10%) for 1-3 min-
utes, and then rinse with water to determine the presence or ab-
sence of Radiolaria. Radiolaria could be recognized with a
binocular microscope from the pits on the ethched surface of the
sample (Figure 1). Utilizing an ultrasonic cleaner, the etched
material was then removed from the etched surface. This proce-
dure helped to accentuate the tests more clearly (Figure 3).
2. Crush the sample to 1-5 cm size.
3. Immerse the crushed sample in diluted acetic acid (75% ace-
tic acid, 25% water) for 8 hours within a beaker.
4.Rinse sample with water, and sieve through a set of #40, #80,
and #230 ASTM standard sieves.

PLATE 1
All illustrations are scanning electron micrographs of Upper Jurassic and Lower Cretaceous Radiolaria from the Great Valley Supergroup,
California Coast Ranges, Glenn and Paskenta Counties, California. Illustrations demonstrate preservation differences of extracted
Radiolaria using this method of sample preparation versus concentrated hydrofluoric acid (HF) technique described in Pessagno (1977b).
Note that only calcified and pyritized Radiolaria exist for ~ 1000 miles along strike in Upper Jurassic and Lower Cretaceous (Berriasian to
Aptian) portions of the Great Valley Supergroup. Scale in upper right = number of µm cited for each illustration.

1 Complexapora kozuri Hull. Calcified radiolaria ex-
tracted from limestone nodule using new method.
Buchia piochii Zone Grindstone Creek, Glenn
County, California. Scale = 167 µm.
2 Pantanellium sp. Calcified radiolaria extracted from
limestone nodule using new method. Note excellent
preservation. Buchia piochii Zone Grindstone Creek,
Glenn County, California. Scale = 50 µm.
3 Pantanellium corriganensis Pessagno. Pyritized
specimen extracted from limestone nodule using HCl.
Sample NSF 1019 of Pessagno (1977b). Lower Creta-
ceous: lower Hauterivian to lower Barremian. Scale =
250 µm.
4 Cecrops septemporatus (Parona). Pyritized specimen
extracted from limestone nodule using HCl. Sample
NSF 1019 of Pessagno (1977b). Lower Cretaceous:
lower Hauterivian to lower Barremian. Scale = 200
µm.
5 Parvicingula citae Pessagno. Calcified specimen ex-
tracted from limestone nodule using HF. Sample NSF
845 of Pessagno (1977b). Lower Cretaceous: lower
Hauterivian to lower Barremian. Scale = 128 µm.
6 Parvicingula sanfilippoae Hull. Calcified radiolarian
extracted from limestone nodule using new method.
Scale in upper right = 100 µm.
7 Ristola cretacea Baumgartner. Calcified radiolarian
extracted from limestone nodule using new method.
Sample from Buchia piochii Zone, Grindstone Creek,
Glenn County, California. Upper Jurassic: upper
Tithonian. Note better preservation with new method
of sample preparation; compare with preservation of
R. cretacea (Figure 8 below. HF method of sample
preservation). Scale = 139 µm.
8 Ristola cretacea Baumgartner. Calcified radiolarian
extracted from limestone nodule using HF method of
sample preparation. Sample from Buchia uncitoides
Zone, Grindstone Creek,Glenn County,California
Lower Cretaceous: Berriasian. Scale = 147 µm.
9 Minocapsa sp. Calcified radiolarian extracted from
limestone nodule using new Kariminia method. Note
excellent preservation. Buchia piochii Zone, Grind-
stone Creek, Glenn County, California. Scale = 109
µm
10 Mita sp. cf. M. magnifica Pessagno. Calcified
radiolarian extracted from limestone nodule using this
method. Calcified radiolarian extracted from lime-
stone nodule using new method. Note excellent pres-
ervation. Buchia piochii Zone Grindstone Creek,
Glenn County, California. Scale = 83 µm
11 Caneta sp. Calcified radiolarian extracted from lime-
stone nodule using the new method. Note excellent
preservation. Calcified radiolarian extracted from
limestone nodule using new method. Note excellent
preservation. Buchia piochii Zone Grindstone Creek,
Glenn County, California, Scale = 92 µm.
12 Parvicingula sp. Calcified radiolarian extracted from
limestone nodule using new method. Note excellent
preservation. Calcified radiolarian extracted from
limestone nodule using new method. Note excellent
preservation. Buchia piochii Zone Grindstone Creek,
Glenn County, California. Scale = 76 µm.

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Seyed Mohsen Karaminia Plate 1

micropaleontology, vol. 50, no. 3, 2004 303

Seyed Mohsen Karaminia : Extraction of calcified Radiolaria and other calcified microfossils from micritic limestone utilizing Acetic acid

TEXT-FIGURE 5
Comparison of this method and previous methods introduced by Tur et al. (2001), and Lirer (2000).

5. Return sample remaining on sieve #40 to the diluted acid for cessing time varies from 30 minutes for shales up to eight hours
another 8 hours treatment. for micrites.

6. Gently rinse the residue with abundant water, and dry in
oven.
Plates 1 and 2 illustrate the tests extracted with this modified
method. All figures are scanning electron microphotographs,
representing excellent preservation of the tests.
Ultrasonic cleaning of the sieved residue (Lirer 2000) helps to
remove sediments from delicate structures of foraminifera spec-
imens (e.g. umbilical apparatus of Upper Cretaceous planktonic
foraminifera). To prevent destroying the extracted calcified
radiolarians ultrasonic cleaning of the residue should be limited
to one or tow seconds.

DISCUSSION The reaction of undiluted acid and carbonate sample takes sev-
The time length for treating a given sample depends on the clay eral days up to two weeks. Accelerating the process by heating,
content of the sample and its induration. In this method the pro- mentioned in some other studies, is because of utilizing concen-

PLATE 2
All illustrations are scanning electronic micrographs of Upper Jurassic, Lower and Upper Cretaceous radiolaria and planktonic
foraminifera from the indurated micrites within the Khoy ophiolitic complex of northwestern Iran, Greenhorn Formation of Pueblo,
Colorado, and Duck Creek Formation of Texas. Scale in upper right = number of µm cited for each illustration.

1,2,9 Umbilical and lateral views of Favusella washitensis
Carsey extracted from indurated limestone. Upper
Albian, Duck Creek Formation, Texas. Scale: figure
1= 88 µm, figure 2 = 142 µm, figure 9 = 88 µm.
3,4 Whitinella sp. Greenhorn Formation, Pueblo, Colo-
rado. Scale : figure3 = 144µm, figure4 = 165.5 µm,
figure9 = 129 µm.
5 Ticinella sp. Duck Creek Formation, Texas. Scale =
160 µm.
6 Schackoina sp. Khoy Ophiolitic Complex, N.W. Iran.
Scale = 109 µm.
7 Ticinella sp. Greenhorn Formation, Pueblo, Colorado.
Scale = 155 µm.
8 Racemiguembelina sp. Khoy Ophiolitic Complex,
N.W. Iran. Scale = 190 µm.
10 Globotruncana linneiana (d‘Orbigny) in acidified
surface of the rock sample, before rinsing and extract-
ing. Note the differential dissolution of rock matrix
compared to the foraminifera. Khoy Ophiolitic Com-
plex, N.W. Iran. Scale = 175.5 µm.
11-13 Lower Cretaceous calcified radiolaria in acidified sur-
face of the rock sample, before rinsing and extracting.
Note the differential dissolution of rock matrix com-
pared to calcified radiolaria. Figure 11: Pantanellium

304
Seyed Mohsen Karaminia Plate 2

micropaleontology, vol. 50, no. 3, 2004 305

Seyed Mohsen Karaminia : Extraction of calcified Radiolaria and other calcified microfossils from micritic limestone utilizing Acetic acid
trated acetic acid (Tur et al 2001, Lethiers et al 1988). With this
method time span can be reduced to30 minutes to 8 hours by
diluting acetic acid to 75% and processing at the room tempera-
ture. Text figure 5 compares this modified method and those of
Tur (2001), and Lirer (2000). Other studies lack the illustrations
of extracted microfossils and are not discussed herein.
ACKNOWLEDGMENTS
This work was supported in part by NSF EAR0074120 awarded
to Dr. Emile A. Pessagno, Jr. I would like to thank Dr. Emile
Pessagno for his continuous support, and critical reading of
manuscript. I thank Dr. James Carter, Dr. Ignacio Pujana, and
Mrs. Narjes Sabety for their aid in technical phase. I wish to ex-
press my appreciation to Dr. Ignacio Pujana and Ms. Dragana
Nebrigic for reviewing the manuscript.
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Manuscript received May 17, 2004
Manuscript accepted May 17, 2004