Society for American Archaeology

Separation of Bone, Charcoal, and Seeds by Chemical Flotation

Author(s): Connie Cox Bodner and Ralph M. Rowlett
Source: American Antiquity, Vol. 45, No. 1 (Jan., 1980), pp. 110-116
Published by: Society for American Archaeology
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110

AMERICANANTIQUITY

[Vol.45, No. 1, 1980]

Kubler, George
1948 Mexican architecture of the sixteenth century. Yale University Press, New Haven.
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1970 The history of the Incas, translated from the French by George Ordish. Schocken Books, New York.
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1975 Prehistoric principles of labor organization in the Moche Valley, Peru. American Antiquity
40:191-196.
Moseley, Michael E., and Luis Watanabe
1974 The adobe sculpture of Huaca de los Reyes. Archaeology 27:154-161.
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1974 Prehistoric earth mounds in the highlands of Ecuador: a preliminary report. Archaeological Investigations in the highlands of northern Ecuador. Department of Anthropology, University of New Mexico. Albuquerque. The Instituto Otavalefio de Antropologia, Otavalo, Ecuador.
Pozorski, Thomas
1975 El complejo de Caballo Muerto: los frisos de barro de la Huaca de los Reyes. Revista del Museo Nacional 41:211-251.
1976 Caballo Muerto: a complex of early ceramic sites in the Moche Valley, Peru. Unpublished Ph.D.
dissertation, Department of Anthropology, University of Texas, Austin.
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1936 Soils: their origin, constitution, and classification: an introduction to pedology. Thomas Murby and
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1962 Chavin art: an inquiry into its form and meaning. The Museum of Primitive Art, New York.
Samaniego Roman, Lorenzo A.
1973 Los nuevos trabajos arqueol6gicos en Sechin, Casma, Peru. Larsen ediciones, Trujillo.
Schaedel, Richard P.
1971 The city and the origin of the state in America. 39th International Congress of Americanists 1:15-33.
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1975 Origins of the state and civilization: the process of cultural evolution. Norton, New York.
Tello, Julio C.
1943 Discovery of the Chavin culture in Peru. American Antiquity 9:135-160.
1956 Arqueologia del valle de Casma. Culturas: Chavin, Santa o Huaylas Yunga y Sub-Chimi. Editorial San
Marcos, Lima.

SEPARATION OF BONE, CHARCOAL,AND SEEDS

BY CHEMICALFLOTATION
Connie Cox Bodner and Ralph M. Rowlett
Gravel, bone, carbonized seeds, and charcoal recovered from a 2,000 year old cereal pit were successfully
separated by chemical flotation. Specific gravities of each material were determined experimentally, and then
for each pair of materials to be separated (e.g., bone from gravel, seeds from charcoal), a solution with a
specific gravity intermediate between those of the two materials was used for flotation. Optimal sample sizes
and possible sources of error are discussed, as are criteria for selection of solutions. A procedure for
evaluating the effect of solutions and flotation practices on test seeds is also presented.

Flotation as a means for recovering botanical remains, charcoal, shell, bone, flint chips, and
other materials from archaeological contexts has become standard procedure for many projects
in recent years. Efforts have been directed towards developing customized versions of hand flotaConnie Cox Bodner and Ralph M. Rowlett, Department of Anthropology, University of Missouri-Columbia,
Columbia, MO 65201
Copyright ? 1980 by the Society for American Archaeology
0002-7316/80/010110-07$1.20/1

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111

REPORTS

tion systems, as well as machine flotation systems, for use in specific field and laboratorysituations (see Struever 1968; French 1971; Schock 1971; Jarmanet al. 1972; Stewart and Robinson
1973; Williams 1973; Minnis and LeBlanc 1976; and Watson 1976).
In each of these systems, the end product consists of a heavy fraction and a light fraction, each
of which must be further sorted on the basis of their constituent materials. Struever (1968) and
others have used chemically treated water to separate the light fraction into bone and plant remains. By using a solution of zinc chloride (ZnC12)at a specific gravity of 1.62, Struever has
reported a nearly 100% separation of these two particulartypes of material. However,even after
chemical flotation of this type, one is often faced with the tedious and time-consumingtask of
separating seeds from charcoal in the light fraction or burned clay from rock in the heavy fraction.
Such was the case in the flotation studies of the contents of a cereal pit fromthe Titelberghillfort site in southwestern Luxembourg(R.Rowlett et al. 1974; Thomas et al. 1975; Thomas et al.
1976; E. Rowlett et al. 1976). After the sample was separated into a heavy fraction and a light
fraction by means of a flotationmachine (Figure 1) similar to that reportedby Watson (1976:82),
the heavy fraction consisted of large quantities of gravel mixed with bone fragments and a few
potsherds, while the light fraction was made up of charcoal and carbonized seeds. It is worth
noting that the 2000-year-oldbone in this sample settled with the heavy fraction rather than
floating with the light fraction as Struever (168:354)reported happeningwith his samples.
It was postulated that the same principles which govern the ZnC12separation of bone from
plant remains could also provide the basis for the separation of other materials, if selected solutions of varying specific gravities were used. The fundamentalprinciple pertaining to chemical
flotation, and indeed to water flotation as well, is that any material will float in a solutionwith a
higher specific gravity than that of the material itself. Therefore, if a mixture of two materials

B
G
H- __~

KEY:
A
B
C
D

Water Intake Valve

E
55 Gallon Drum
Metal Stand
F
Shower Head
G
H
Soil Trap

Bucket Insert with

Screen Bottom
Overflow Pipe
Water Outlet Valve

Figure 1. Schematic diagram of the flotation machine used in this study.

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112

AMERICANANTIQUITY

[Vol.45, No. 1, 1980]

with significantly different specific gravities is put into a solution whose specific gravity is intermediate between those of the materials to be separated, then separation can be achieved.
At the time our work was carried out, we were unaware of similar work done by Teteryuk and

his associates in the U.S.S.R.some years earlier (J.M. Adovasio, personal communication).Using
the principle outlined above, Teteryuk has successfully separated classes of spores from one

another in genetically homogeneous groups by using Thoulet's solution (potassium triiodomercurate [II]) in varying concentrations, and hence varying specific gravities. The separation is
accomplished by repeatedly adjusting the specific gravity of the solution, centrifuging, and drawing off groups of spores suspended in solution by means of a pipette. Although the technique has
some potentially serious drawbacks (i.e., Thoulet's solution is very volatile and toxic, and the pro-

cedure is extremely time-consumingand tedious),its merits are obvious.Adovasio(personal communication)reports satisfactory results after adapting Teteryuk's procedure to archaeological

materials other than pollen and spores.

PROCEDURE
In our particular situation, we wanted to separate bone fragments from gravel in the heavy
fraction, and seeds from charcoal in the light fraction. It became necessary to determine the
specific gravities of each of these components before a suitable flotation solution could be

selected.
Samples of each of these materials were collected by hand from the two fractions. Optimal
sample sizes by weight were as follows: seeds 1.5-2.5 g, charcoal 2.5-4.5 g, bone 2-4.5 g, gravel
10-20 g. The density of each material was determinedby first placing a weighed, dry sample in a
clean, dry, weighed 25 ml graduatedcylinder.The cylinderwas then filled with water to the 25 ml
mark and weighed again. Subtractingthe combinedweights of the dry cylinder and the dry sample from the weight of the cylinder filled with sample and water yields the weight of the water

necessary to fill the cylinder. Since the specific gravity of water is approximately1.00 g/ml, the
weight of the water in the cylinder in grams is equal to the volume of the water in the cylinder in
milliliters. By subtracting the volume of the water from the total volume of the cylinder (i.e., 25
ml), the volume of the sample can be determined. The weight of the dry sample divided by the

volumeof the same is equal to its specific gravity in grams per milliliter.A sample calculation appears in Table 1.
Table 1. Calculationof Gravel's Specific Gravity.
Weightof clean, dry 25 ml graduatedcylinder:
Weightof gravel sample:
Weightof cylinder,gravel, and water to 25 ml:
Weight of water:

66.2133 g
10.6800 g
97.1544 g
97.1544 g
-66.2133
- 10.6800

20.2611 g
Volume of water:
Volume of sample:

20.2611 ml
25.0000 ml
-20.2611

4.7389
Specific gravity of gravel:

10.6800 g
4.7389 ml
= 2.25 g/ml

Water must fill all spaces not taken up by the sample in order for the weights and therefore the

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REPORTS

113

Table 2. Specific gravities (in g/ml)of Seeds, Charcoal,Bone and Gravel from the Titelberg,Luxembourg.

Material

Run No. 1

Run No. 2

Run No. 3

Seeds
Charcoal
Bone
Gravel

0.60
0.80
1.37
2.25

0.66
0.83
1.87
1.97

0.64
0.82
1.62
2.23

Mean Specific
Gravity
0.63 + 0.03
0.82 + 0.02
1.6 + 0.2
2.1 + 0.1

calculations to be meaningful. All air bubbles should be tapped out of the cylinder before the final
weighing. In addition, samples of sizes smaller than those listed as optimal yielded erratic specific
gravities, whereas samples of at least the size range listed gave relatively uniform results. The
specific gravities of these materials are listed in Table 2.
Table 2 shows that the specific gravity determinations varied to a greater extent for the bone
and gravel samples than for the seeds and charcoal. There are several possible explanations for
this circumstance. First, both the gravel and the bone fragments were heterogeneous in nature.
Variation in bone density arises from differential preservation, interspecies differentiation, or
differences between and among types of bone (i.e., long bones, mandibles, ribs, etc.). Sampling error could have been a factor as well, as the larger pieces of bone and gravel could not fit into the
graduated cylinder and were therefore excluded from the samples. However, the agreement of
specific gravity determinations among the three runs was reasonably good and proved to be sufficient for our purposes.
Next, solutions of the proper specific gravities were selected to provide the desired separation
of the particular materials. Figure 2 presents the scheme for separation. A solution of specific
gravity between 1.6 and 2.1 separated bone from gravel, and a solution of specific gravity between 0.63 and 0.82 served to separate carbonized seeds from charcoal.
Several important criteria need to be considered when selecting a solution for flotation studies
of this kind. The ideal solution would be one which is (1) neither extremely acidic nor basic, (2) not
toxic, (3) not damaging to the materials floated, and (4) not flammable, but which is (5) commonly
available, and (6) relatively inexpensive. Compromises can, of course, be made; for example, if the
work is to be done in the laboratory under the hood, then flammable liquids are more acceptable
than if the work had to be done in a hot desert field situation.
I ORIGINAL SOIL
Flotation

HEAVY FRACTION
(GRAVEL, BONE) I
Solution
between

GRAVEL_

of
1.6
g/ml

density
and 2.1

SAMPLE j

Machine

LIGHT FRACTION
(CHARCOAL, SEEDS)

Solution
between

of density
and 0.82
0.63
g/ml

iCHARCOAL7

LSEEDS j

Figure 2. Scheme for partitioning heavy and light flotation fractions on the basis of the density of
chemical flotation solutions and the specific gravities of archaeological materials.

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114

AMERICANANTIQUITY

[Vol.45, No. 1, 1980]

Any solution being considered for flotation must be tested with regard to its effect upon the ar-

chaeological materials, particularly the botanical remains. Of course, it is unrealistic to risk the
destructionof an entire seed sample in the search for a safe solution.We have successfully used
common bird seed and garden seed which have been carbonized by slow roasting in an oven (500?
F for several hours) for such tests. If a solution does not damage these test seeds, then it will probably be safe for the archaeological sample. If, on the other hand, a solution dissolves or in some
other way destroys the test seeds, nothing is lost and a very important bit of information is gained.
We left our test seeds in the various solutions for three days to be certain about the nature of the
solutions in this regard. Table 3 lists several possibilities for boththe dense (S.G. 1.6-2.1 g/ml) and
the light (S.G. 0.63-0.82 g/ml) solutions, along with their approximate current prices. They have

been selected on the basis of the criteria listed above.

used for the Titelberg material were ferric sulfate (Fe2[S04]3 xH20) for
from gravel, and either ethyl ether ([C2H5]20) or acetone (CH3COCH3) for
from charcoal. The "recipe" for a Fe2(SO4)3exH20 solution with a speciic
1.6 and 2.1 g/ml was derived in the following manner. Varying weights of
xH20 were each dissolved in a fixed volume of water, and the specific gravity of the
Fe2(S4)3
solution was measured using a picnometer. The specific gravity determinations were then plotted
The solutions
separating bone
separating seeds
gravity between

against the ratio of weight of Fe2(S04)3* xH2Oper milliliterof water (Figure3). Interpolationsor
extrapolations can be made using this graph to arrive at the estimated proportion of
Fe2(S04)3 xH20 to water, and then these amounts can be multiplied by whatever factor is

necessary to yield the desired quantities of solution.For example, a solutionwith a specific gravity between 1.3 and 1.4 g/mlwould require some 0.45 g of Fe2(S04)3* xH2Oper milliliterof water
or 450 g per liter. Such graphs can easily be made for any solution used. Both the acetone and
ethyl ether were used without dilution.
RESULTS
The results obtained using this flotation procedure were remarkablysatisfactory. For sorting
bone from gravel, the separation was clean and complete for all practical purposes. When incomplete separation occurred, it might be attributed to the factors of heterogeneity and sampling

Table 3. Possible Solutionsfor ChemicalFlotationStudies.

Chemical
S.G. = 0.79 g/ml)
Acetonea (CH3COCH3,
Bromoformb(CHBr3,S.G. = 2.89 g/ml)
Calciumbromide(CaBr2)
Cupricnitrate (Cu(N03)2* 3H20)
Cyclohexane(C6H12,S.G. = 0.78 g/ml)
Ethylether anhydrousa
((C2H5)20, S.G. = 0.72 g/ml)
Ferric chloride (Fe2C13)
Ferric sulfate (Fe2(S04)3?xH20)
Potassiumtriiodomercurate(II)b
(HgI2? KI)
Sodiumdichromate(Na2Cr207 2H20)
Zinc chloride (ZnC12)

Price
$4.75/gallon
$17.35/kg
$8.50/lb
$3.94/lb; $15.40/5 lb
$7.50/gallon;$24.00/5 gallons
$2.75/lb; $11.75/5 lb
$3.20/lb; $34.80/12 lb
$2.75/lb; $18.00/25 lb
$37.80/lb
$2.25/lb; $20.00/25 lb
$2.62/lb; $21.50/25 lb

Note. Maximumspecific gravities for saturated solutions of inorganic salts must be determined experimentally.
a Highlyflammable.
b Shouldbe used with a hood.

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115

REPORTS

0
1.0
E

o
-

0.9-

/
>

0.8-

OCX~

-0.7

0
x

0.6 /

?2

0.5i

u-

0.4-

0.3-

c)

/
/

_0.2.0
R

/
0.1-

1.1

1.2

1.3

1.4

1.5

1.6

Specific Gravity in grams/milliliter

Figure 3. Specific gravity plotted against the number of grams of Fe2(S04)3 xH20 dissolved in 1.0
ml of water.
error, as discussed earlier. Even allowing for these problems, chemical separation proved much
faster than that done totally by hand.
With respect to the seed-charcoal separation, two unanticipated phenomena were observed.
As soon as the sample was poured into the ether or acetone, the charcoal sank immediately, as
was expected. However, the large seeds began to sink soon thereafter instead of floating on top as
expected. After these large seeds were retrieved, some very tiny seeds, the presence of which had
not been detected up to this point, were left floating on top. These were easily retrieved and
stored separately from the larger seeds and charcoal.
It should be noted that Fe2(S04)3*xH20 , like ZnC12, is very hygroscopic. This means that
materials which have been floated in this solution must be thoroughly rinsed with clean water, or
they will never dry completely. Materials which have been floated in acetone or ether are readily
dried by simple evaporation of the solvent from the archaeological materials.

CONCLUSIONS
Through the use of selected solutions of varying specific gravities, certain archaeological
materials can be separated from each other quickly and efficiently. While we realize that such a
procedure is not necessary in those situations where there is a limited number of easily separable
kinds of materials, we believe it can be advantageous for the heterogeneous mixtures that often
compose the heavy and light fractions isolated by more traditional flotation methods. Of particular significance is the detection by this technique of previously unobserved materials.

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116

AMERICANANTIQUITY

[Vol.45, No. 1, 1980]

Although the possibility of damage to the more fragile components has been cited as a major
drawback of chemical flotation (Jarman et al. 1972:39), we observed no degradation of the archaeological materials after periods of several hours. Obviously caution must be exercised while
manipulating chemical reagents, but we believe that the benefits of their use in procedures such
as that outlined here are sufficient to justify the extra time and effort necessary to do so.
Acknowledgments. The Titelbergsettlements research project was supportedby National Science Foun-

dation grants BNS76 00011 during 1975-1978 and GS 39835 from 1973 to 1975. The project was initiated by

Universityof MissouriResearch Councilgrants in 1971 and 1972. The flotationmachinewas built by Michael
J.Reagan,Departmentof Anthropology,Universityof Missouri-Columbia.
Figures 1 and 3 were drawn by Guy
Prentice of the Universityof Illinois-UrbanaFAI-270ArchaeologicalMitigationProject.
We thank Dr. George M. Bodner of Purdue University,Dr. James W. Porter of the University of IllinoisUrbana, and Dr. JamesAdovasio of the Universityof Pittsburghfor their constructivecommentsand suggestions regardingthis paper.
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