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McDougall Potassiumargondatingarchaeology 1990
McDougall Potassiumargondatingarchaeology 1990
Author(s): I. McDougall
Source: Science Progress (1933-) , 1990, Vol. 74, No. 1 (293) (1990), pp. 15-30
Published by: Sage Publications, Ltd.
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Science Progress (1933-)
Introduction
The potassium-argon (K-Ar) isotopie dating method is widely used for
numerical age measurement of rocks, especially igneous rocks, which are
formed by cooling of magmas after emplacement or after eruption as lava
flows. This technique depends upon the accumulation in the rock of daughter
radiogenic argon (40Ar*) from the decay of parent radioactive potassium, the
isotope 40K. The K-Ar method is very useful for dating rocks in the range
from significantly younger than 100,000 years in favourable cases, to billions
(>109) of years. With appropriate samples and careful measurement, very
precise and accurate ages can be determined, often with uncertainties of as
little as 1% . In the Cainozoic, the last 65 million years (Ma) of geological
time, the K-Ar method arguably is the most important and versatile means
of numerical age determination presently available.
The basis for this review was a paper originally prepared for presentation
at an archaeological meeting; hence the title and emphasis. The K-Ar dating
method has applications in the archaeological context in those cases where
igneous rocks, including lavas or products of explosive volcanic eruptions
(pumices, tuffs etc.), are associated with stratigraphie sequences of interest.
It is intended to present here an outline of the principles of K-Ar dating,
15
Principles
The K-Ar dating method is based on the natural occurrence in the environ-
ment of the radioactive isotope of potassium, 40K, which has a half-life of
1250 Ma. This isotope, comprising about one atom in every 8600 atoms of
potassium, has a dual decay, with about 10.5% of the decays producing 40 Ar*
by electron capture, and the balance yielding ^Ca by ß~ decay (Fig. 1). The
calcium branch is not normally useful for age measurement because 40Ca is
the main isotope of this element in the environment. However, the argon
branch is particularly useful for numerical age measurement.
40k
electron capture / '
(10^3%)^. - ģ/
( ■$/ emission
(
)
'
.«?/>*
(89.5%)
'
emission /
Y ( ) y? '
40Ar -
The simplest case is that of a magma. The 40K present decays continuous
to 40 Ar*, which, however, will usually be lost by diffusion at the high preva
ing temperatures. This is because argon is a gas and thus will partition int
the gas phase. On cooling of the magma, perhaps after its eruption as a lav
the 40 Ar* will begin to accumulate within the rock when the temperature
decreases below that for closure with respect to argon diffusion in the
component minerals of the rock. This closure temperature for argon range
from about 500° to about 150°C in different minerals used for K-Ar datin
The 40 Ar atom is large enough that it remains trapped within the crystal lat-
ió I. McDougall
X ' Xe /
where tis the calculated age; X is the decay constant (5.543 x 1
the proportion of 40K atoms decaying per unit time; 'J' = 0.1
fraction of the 40K decays yielding 40Ar* , and 40 Ar* and 40K a
amounts of radiogenic argon and parent 40K within the sampl
time. The constants currently in use are those recommended b
Subcommission on Geochronology,31 based upon physical me
the 40K abundance and its decay. It will be evident from the e
determine a K-Ar age, the amounts of 40 Ar* and need to b
In the conventional K-Ar method, total potassium normally
on an aliquot of the sample by means of flame photometry, at
tion spectrometry or isotope dilution, and the amount of 40K
the 40K/K ratio is essentially constant in terrestrial materials.1
released by fusing a separate aliquot of the sample in a high v
and its amount is measured in a mass spectrometer, usually by
tion employing 38 Ar as a tracer. The proportion of the argon
genic also can be determined from the isotopie analysis. Provid
igneous rock is not subsequently disturbed by reheating, the K
likely to accurately measure the elapsed time since crystallizat
cooling.
The 40 Ar/39 Ar dating technique, developed by Merrihue & Turner,29 is an
important variant of the K-Ar method. It provides much more information
than obtained by conventional K-Ar measurement, and enables evaluation
of some of the underlying assumptions. In this technique, the argon and
potassium effectively are determined on a single portion of the sample by
isotopie analysis in a mass spectrometer of the argon extracted from the
sample. The 40 Ar/39 Ar technique depends upon the conversion of a propor-
tion of the 39K to 39Ar by an (n,p) reaction during irradiation with fast
neutrons in a nuclear reactor. After irradiation the sample can be fused in the
extraction system and, subsequent to purification, the argon is analysed iso-
topically. The amount of 39 Ar present provides a measure of the 39K in the
sample, and as the 40K/39K ratio is essentially constant in the natural environ-
ment, the 40Ar*/39Ar ratio is proportional to the 40Ar*/40K, and hence age.
In practice we need to know the neutron dose the sample has received, and
this is obtained indirectly by analysing the argon released from a sample of
accurately known age that is irradiated together with the unknown in the
nuclear reactor. The 40Ar/39Ar technique has considerable advantages over
the conventional K-Ar dating method, as the age measurement is made on a
single split of the sample, thus overcoming inhomogeneity problems, and
smaller amounts of sample normally can be utilized. Furthermore, as the age
Potassium-argon dating 17
18 I. McDougall
V/Z/À/Z/Á V//////////A
o 4*rV
o Radiogenic arg
«
I I
• • I
o| I I r- F=*=
© i r
O)
« ' -i
- -- i-- 11 -i -1 1- i1- -1 1
i -- 11i -- 1
1 ii -- ii-
1 1
- i-
- 1
i II
1 Cî
d
rt
■ I
o 50 100 o 50 100
39ArK release (%) 39ArK release (%)
Increasing temperature :£>
Assumptions
As with all isotopie dating methods, a number of assumptions must be met if
a K-Ar or 40Ar/39Ar age measurement is to give a valid estimate of age, and
the most important of these are discussed below.
1. At the time of crystallization of the rock all pre-existing ^Ar* must
have been lost. If this is not the case, then the measured age will be greater
than the true age. For subaerially erupted volcanic rocks and shallow
intrusi ves this assumption generally is valid, but can be vitiated if xenoliths of
older rocks are incorporated in the magma.
Potassium-argon dating 19
Choice of samples
A very important aspect of K-Ar dating practice is the choice of appropriate
samples. As previously emphasized, the method is applied most successfully
to igneous rocks, although useful age information often can be obtained from
metamorphic rocks. Only in special circumstances is the method applicable
to the dating of the time of deposition of sedimentary rocks. In relation to
archaeology, application of the K-Ar method is mainly to igneous rocks or
their redeposited explosive volcanic products in the form of tuffaceous beds,
so that the discussion here will be restricted to such materials.
20 /. McDougall
Minerals that are suitable for K-Ar age measurement include leucite, high
temperature alkali feldspar (sanidine, anorthoclase), musco vite, biotite,
amphibole and plagioclase, listed approximately in order of decreasing potas-
sium content. Standard heavy liquid and magnetic methods are used to obtain
concentrates from the crushed sample, and it is desirable to aim for as high
purity as possible, preferably > 99% pure, at the coarsest grain size consistent
with obtaining material free of composites. It becomes increasingly difficult
to separate minerals as the crystal size decreases below about 100 |xm. Suitable
minerals may be separated from volcanic (or intrusive) rocks or their tuf-
faceous equivalents. Note, however, that tuffs, especially if reworked, may
contain old detrital material, which, if present in a sample being dated will
cause the measured age to be anomalously old. Thus, particularly careful
assessment of tuffaceous material is necessary to ensure that inclusion of
detrital minerals is avoided in the mineral separate; however, in some cases
detection of detrital contamination is very difficult. The measurement of
40 Ar/39 Ar ages on individual crystals, now possible by use of a laser micro-
probe, enables such questions to be directly assessed.
Age measurements on whole rock samples of volcanics will reflect the argon
retention properties of the component minerals. Provided samples are well-
crystallized, and the potassium-bearing phases are unaltered, whole rocks are
excellent material for K-Ar dating, and commonly yield reliable ages. Lavas
that show more than incipient alteration, and/or contain glass can be less
satisfactory. Especially if glass is devitrified or altered, some of the ^Ar* is
likely to have been lost, leading to young apparent ages. In measuring whole
rock samples of lavas it is a wise precaution to remove large phenocrysts such
as olivine or pyroxene from them prior to dating, as such crystals may contain
some excess 40 Ar from the environment when they crystallized before the
eruption of the magma.
Volcanic glass, for example obsidian, can be used for dating if perfectly
fresh and undevitrified. Note, however, that owing to changes in glass as it
hydrates, devitrifies and alters, K-Ar ages can be anomalous,8 and should be
carefully assessed.
Age limits
As the K-Ar and 40 Ar/39 Ar methods rely upon the accumulation of 40Ar*
with time, it is technically easier to measure ages on old rocks; the limitations
arise in determining the radiogenic argon content of young samples. With
current techniques, properly applied, unaltered samples possessing a
reasonable potassium content, say > 0.5% , older than 0.5-1 Ma usually can
be measured with a precision of a few per cent utilizing samples of ^ lg.
However, the laser fusion approach to 40 Ar/39 Ar dating is dramatically
changing these requirements, in that much smaller samples can be measured.
In the archaeological context, we are likely to be dealing with the younger
Potassium-argon dating 21
22 /. McDougall
Potassium-argon dating 23
Fig. 3. Map of the Lake Turkana region , Turkana , and the Nachukui Formation ,
northern Kenya , indicating outcrop of the adjacent to the western shores of the lake ,
Koobi Fora Formation adjacent to the also are shown as they are correlations of
eastern shores of the lake. Outcrops of the the Koobi Fora Formation. Area that
Shungura Formation , to the north of Lake drains into Lake Turkana is left blank.
24 I. McDougall
Fig. 4. Generalized stratigraphy within the feldspars from pumice clasts in the tuffs
sedimentary sequence of the Koobi Fora are given , with the number of samples
Formation showing the main tuffaceous used in calculating each mean shown in
horizons. Average K-Ar and Ar/39 Ar parentheses after each age.
ages in million years (Ma) measured on
Potassium-argon dating 25
As the tuffs are of igneous origin, isotopie dating can be expected to yield
good estimates of the age of the eruptive episodes. Because the time between
eruption and deposition is likely to be extremely short, such ages should
closely approximate the time of deposition within the Turkana Basin. Never-
theless, direct dating of the KBS Tuff gave excessively old ages,16 demonstrat-
ing that an old detrital component was incorporated within the tuff, perhaps
not unexpectedly as reworking and transportation occurred subsequent to
eruption as volcanic ash. A solution to this problem was soon found, as it was
recognized that pumice clasts, which occur locally within some of the tuff
beds, are much less likely to have incorporated old detrital material within
them compared with the enclosing tuffs. These pumice clasts, also trans-
ported into the basin by water, are considered to be products of the same
explosive volcanic eruptions that produced the tuffs, confirmed by geo-
chemical fingerprinting in a number of cases. Phenocrysts of alkali feldspar
(anorthoclase), ideal material for K-Ar and 40 Ar/39 Ar dating, are present in
some of these pumices, and often can be separated quite free of detrital
contamination, especially if only the internal parts of a pumice block are
processed. Measurement of such juvenile feldspar normally would be
expected to yield an age reflecting the time since eruption and cooling.
Using this approach a comprehensive set of ages was determined on the
Koobi Fora sequence, as summarized in Fig. 4, after McDougall24 and
McDougall et al.25 The K-Ar age shown adjacent to a particular tuff horizon
is an average based upon measurements on high purity alkali feldspar con-
centrates separated from a number of pumice clasts, often from widely dis-
persed localities, within that tuff. Excellent agreement was found, as shown
by the small uncertainty (standard deviation) between the results from a
given level in virtually all cases. Such consistency provides considerable
confidence that the ages are geologically meaningful. Inspection of Fig. 4
shows that the measured ages decrease upward through the sequence, and
this consistency with the stratigraphy is taken as particularly strong evidence
that the ages can be accepted at face value. In addition, 40 Ar/39 Ar ages on a
number of the feldspars agree to within experimental error with the conven-
tional K-Ar ages. Most of the 40Ar/39Ar age spectra are similar to those illus-
trated in Fig. 5, yielding essentially flat patterns, indicating that the feldspars
have not been heated significantly subsequent to their crystallization, as no
evidence of argon loss is apparent from the spectra.
The combined results illustrate that in favourable circumstances a high
precision is attainable and that quite fine-scaled numerical age definition is
possible. The alkali feldspars dated in this study all had moderate potassium
contents in the range of 3.7-5.8% , and even for the youngest samples, the
proportion of 40 Ar* compared with the total 40 Ar was as great as 0.7, using
samples of mass ~2 g for the argon extractions. Thus, in this study, the
26 I. McDougall
younger limit was not even closely approached. Calculations show that it
would be possible to measure ages on comparable feldspars from rocks as
young or younger than 30,000 years with a precision of a few per cent, with
up to 10% of the argon radiogenic.
Overall, these results demonstrate that the sequence at Koobi Fora was
deposited over an interval between about 4.1 and 0.7 Ma ago in the Pliocene
and early Pleistocene, with evidence for significant hiatuses in the sedimen-
tary record. For example, a time gap of -0.6 Ma is indicated between the
deposition of the Chari and Silbo Tuffs in the upper part of the sequence.
It should also bę noted that the sediments were deposited on a local base-
ment of Neogene volcanic rocks. A sample of well-crystallized, unaltered
basalt from a lava flow beneath the earliest sediments of the basin yielded an
age of 4.35 ± 0.05 Ma, consistent with the age control provided by the dating
of the tuffs.
The age of the KBS Tuff of 1.88 ± 0.02 Ma is similar to, but more precise
than that obtained by conventional K-Ar age measurement by Drake et al.n
on alkali feldspar and also volcanic glass from pumices at this level, and
Gleadow19 reported an average age of 1.87 ± 0.04 Ma from fission track
measurements on zircon separated from pumices in the KBS Tuff. Thus, the
age of this horizon, the subject of much controversy previously, would now
seem to be particularly secure.
The age determinations from the Koobi Fora tuffs have yielded an inter-
nally consistent set of measurements, from which we have great confidence
that they are geologically meaningful. Much of the important archaeological
and palaeoanthropological material recovered from the Koobi Fora sequence
came from the interval from just below the KBS Tuff to the Chari Tuff, that
is from sediments in the age range 1.9-1.4 Ma in the latest Pliocene to early
Pleistocene.
F. H. Brown, together with co-workers, has been able to utilize the tuff
beds in the Turkana Basin sequences to facilitate correlation between the
three presently known main regions of outcrop of the Plio-Pleistocene
sediments. This has been summarized recently by Feibel et a/.14 who have
Potassium-argon dating 27
careful mapping in the field and appropriate chemical analyses of glass from
tuffs in the sequence, it normally is possible to provide a precise age to a new
find.
These bones are interpreted to be those of a male 1.68 m tall, who was about
12 years old when he died. The fossils were excavated from a siltstone that
immediately overlies a tuff correlated with the Okote Tuff Complex of the
Koobi Fora Formation. Feldspar from pumices in the Okote Tuff Complex in
the Koobi Fora region yielded an average K-Ar age of 1.64 ± 0.03 Ma.25 At
Nariokotome, the equivalent of the Chari Tuff of the Koobi Fora Formation
lies 34 m stratigraphically above the hominid level. The Chari Tuff has an age
of 1.39 ± 0.02 Ma (Fig. 4). Thus, the evidence shows that the Homo erectus
skeleton is slightly younger than the 1.64 Ma age of the tuff of the Okote Tuff
Complex and significantly older than the Chari Tuff, so that an age of 1.6 Ma
is derived for the time of deposition. This illustrates the power of geochrono-
logical studies combined with a thorough knowledge of the stratigraphy. It is
worth noting, in passing, that the Okote Tuff Complex contains numerous
archaeological sites from which stone tools in abundance have been found.
Finally, some of the tuffs in the Koobi Fora sequence have been identified
by geochemical fingerprinting in deep sea sedimentary cores recovered from
the Gulf of Aden, and from which estimates of age may be obtained through
biostratigraphy and magnetostratigraphy. 14,30 These age estimates fit well
with the directly determined time scale for the sequence at Koobi Fora.
It is rare to have such thick stratigraphie sequences containing igneous-
derived rocks appropriate for comprehensive geochronological studies of the
kind summarized here. However, another example of considerable signifi-
cance comprises the sequence in the Hadar area of Ethiopia from which
hominid fossils assigned to Australopithecus af arenš is have been found.
Dating this sequence by the K-Ąr method using feldspars separated from
tuffaceous beds and whole rock samples of basalt interbedded in the section
has encountered some difficulties.1,32 Nevertheless, there is little doubt from
28 /. McDougall
Conclusions
The K-Ar and 40Ar/39Ar isotopie methods are particularly useful for age
measurement of young igneous rocks. Where igneous rocks suitable for
dating are interbedded with sedimentary sequences it is possible to obtain
precise and accurate numerical ages that can provide information on the
deposition age of the associated sediments and their contained fossils and
artefacts. Measurements often can be made on samples covering the age
range down to 100,000 years, and even on samples as young or younger than
10,000 years in favourable circumstances. Great importance is attached to
proper sample selection if reliable and consistent results are to be obtained.
Measurement of multiple samples from the same horizon and on samples
from different levels in the stratigraphie sequence are desirable to enable
consistency of the results to be tested. Such consistency checks are vital for
evaluation as to whether the assumptions underlying the methods have been
fulfilled. Finally, it will be evident that the principles and practices of K-Ar
and 40 Ar/39 Ar dating of sequences of archaeological significance do not differ
materially from those used in determining ages in geological successions that
do not contain archaeological or palaeonotologically important materials.
References
1. Aronson J.L., Schmitt T. J., Walter 9. Dalrymple G.B. (1968) Earth Planet.
R.C., Taieb M., Tiercelin J.J., Sci. Letts 3, 289.
Johansen D.C., Naeser C.W. & 10. Dalrymple G.B. & Lanphere M.A.
Nairn A.E.M. (1977) Nature 267, (1969), Potassium-Argon Dating.
323. W.H. Freeman Co., San Francisco
2. Brown F.H. (1982) Nature 300, 631. 258pp.
3. Brown F.H. & Cerling T.E. (1982) 11 Drake, R.E., Curtis G.H., Cerling
Nature 299,212. T.E., Cerling B.W. & Hampel J.
4. Brown F. , Harris J . , Leakey R. & (1980) Nature 283, 368.
Walker A. (1985) Nature 316, 788. 12. Evernden J.F. & Curtis G.H. (1965)
5. Cassignol C. & Gillot P.-Y. (1982) Current Anthropology 6, 343.
In: Numerical Dating in Stratigraphy13. Faure G. (1986) Principles of Isotope
(ed. by G.S. Odin), p. 159. J. Wiley, Geology. 2nd Edition. J. Wiley, New
New York. York.
6. Cerling T.E. & Brown F.H. (1982) 14. Feibel C.S., Brown F.H. &
Nature 299, 216. McDougall I. (1989) Amer. J.
7. Cerling T.E., Brown F.H. & Physical Anthropology 78, 595.
Bowman J. R. (1985) Chem. Geol. 15. Fitch F.J., Hooker P.J. & Miller J. A.
(Isot. G eosci.) 52, 281. (1976) Nature 263, 740.
8. Curtis G. H., Drake, R.E., Cerling 16. Fitch F.J. & Miller J. A. (1970)
T.E., Cerling B.W. & Hampel J.H. Nature 226, 226.
(1975) Nature 258, 395. 17. Fitch F.J. & Miller J. A. (1976) In:
Potassium-argon dating 29
30 /. McDougall