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Potassium—argon dating in archaeology

Author(s): I. McDougall
Source: Science Progress (1933-) , 1990, Vol. 74, No. 1 (293) (1990), pp. 15-30
Published by: Sage Publications, Ltd.

Stable URL: https://www.jstor.org/stable/43423874

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Sci. Progress
Oxford (1990) Potassium-argon dating in
74, 15-30
archaeology
I. McDougall
The potassium-argon (K-Ar) isotopie of the basis of the K-Ar dating
dating method can provide precise tnethod and the underlying assump-
and accurate numerical ages on suit- tions, concludes with an example of
able rocks , especially igneous rocks, its application to the Plio- Pleistocene
over a wide range of age from less stratigraphie sequence in the Tur kana
than 100,000 years old, with no older Basin, northern Kenya. By dating
limit . Together with its variant, the alkali feldspars separated from
40 Art39 Ar technique, the K-Ar pumice blocks in tuffaceous beds,
method is very useful for the numer- excellent age control has been
ical age calibration of stratigraphie obtained for the wealth of vertebrate
sequences, including those containing fossils, including hominids, as well as
archaeological or fossil material, in archaeological material that has
cases where appropriate rocks for been found in the sequence.
dating are present. This brief review

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,

Dr McDougall is a Senior Fellow in the Research School of Earth Sciences, the


Australian National University, Canberra ACT, Australia.

15

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together with discussion of the practical applications and limitations of the
method. The treatment is far from exhaustive; for more detailed information
the reader is referred to works by Dalrymple & Lanphere,10 Faure13 and
McDougall & Harrison.26

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 -

Fig. 1. Diagram showing decay


electron emission.

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

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tices indefinitely at temperatures normally encountered at or near the Earth's
surface. However, loss of argon by diffusion will occur if the rock sub-
sequently experiences elevated temperatures, for example during a meta-
morphic event.
The basic equation for calculation of age is:

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

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is proportional to the 40Ar*/39Ar ratio, derived from isotopie ratio measure-
ments in the mass spectrometer, a precision of better than 0.2% often can
readily be achieved.
A 40 Ar/39 Ar age measured by directly fusing an irradiated sample will
normally yield a value that is indistinguishable from a conventional K-Ar
age. However, the main advantage of the 40 Ar/39 Ar method is that the argon
may be released by heating the sample in the vacuum system in stages,
starting the procedure well below the temperature of fusion. In this step-
heating or incremental heating technique, the argon released at each
temperature is analysed isotopically, and an age calculated for each gas frac-
tion. Thus, a series of apparent ages is obtained from a single irradiated
sample. The method relies upon the diffusion characteristics of the argon
isotopes from the crystal lattice. The results normally are plotted on a diagram
showing the age measured for each fraction against the proportion of 39Ar
released. If such an age spectrum shows a series of ages that are essentially
indistinguishable from one another, it is concluded that the sample has
remained undisturbed since crystallization, with a uniform spatial distribu-
tion of argon across the crystals (Fig. 2a). In cases where the age spectrum is
more complex (Fig. 2b), it is commonly possible to state that the sample has
been thermally disturbed after crystallization, and inferences may be drawn
as to when the disturbance occurred and whether this has caused some loss or

gain of 40Ar*. It may also be possible to determine the original crystallization


age from an age spectrum on a sample that has been thermally disturbed.
Thus, the 40 Ar/39 Ar method is a powerful technique, increasingly used in
geochronological studies, often in conjunction with conventional K-Ar dating,
to obtain a much firmer basis for evaluating the thermal history of a sample.
Samples ranging from a few mg for old (say >500 Ma) minerals to about
1 g of mineral for young rocks (say <5 Ma old) are used for 40Ar/39Ar dating
by means of the incremental heating technique. Argon extractions are
commonly done utilizing a resistively heated furnace system directly on-line
with the mass spectrometer. Heating of a sample by a laser beam to release
gas, followed by isotopie analysis of the argon in the mass spectrometer, has
significantly widened the application of the 40 Ar/39 Ar dating technique.28,33
The laser microprobe opens up a whole new range of possibilities for total
fusion 40 Ar/39 Ar dating of extremely small samples, including single crystals,
or for dating geologically complex or heterogeneous samples. Recently, Layer
et al.2{) have shown that by defocusing the beam from a continuous laser it is
possible to heat a single crystal in stages at successively higher temperatures
to produce a 40 Ar/39 Ar age spectrum. It is becoming increasingly apparent
that there are significant advantages in using a laser microprobe in 40Ar/39Ar
dating. These include the high spatial resolution achievable, the small sample
size required, and the ability to undertake multiple analyses, which enables
full advantage to be taken of the high precision capabilities of the 40 Ar/39 Ar
dating method.

18 I. McDougall

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a b

Margin Centre Margin Margin Centre Margin

V/Z/À/Z/Á V//////////A

o 4*rV
o Radiogenic arg
«

© 39ArK (from 39K) '* 39Arļ<


c ~~ ~~ -----------
o
0

I I
• • I

Margin Centre Margin Margin Centre Margin

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 :£>

Fig. 2. Schematic diagrams showing case in which partial loss of radiogenic


model 40 Ar/39 Ar age spectra. Top diagramargon has occurred from the crystal sub-
portrays an idealized crystal in cross sequent to its initial crystallization.
section , the middle diagram in each panelA maximum age for the time of the
shows the concentration of radiogenic reheating is given by the 40 Ar/39 Ar age for
argon and neutron-induced 39 Ar K acrossthe gas released in the first step of the
the crystal , and the lower diagram experimenty and a minimum age for the
illustrates the 40 Ari39 Ar age spectrum primary crystallization of the crystal is
expected from measurement of argon provided by the apparent age measured on
extracted in successive steps at the gas released at the highest temperature.
progressively higher temperature from the Thickness of bars in model age spectra
idealized crystal, (a) The case of a crystal
indicates nominal uncertainty in the
undisturbed subsequent to initial individual ages.
crystallization and rapid cooling, (b) The

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

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2. The sample being dated must have remained a closed system since
crystallization. In other words, there must be no loss or gain of potassium or
^Ar*, other than by radioactive decay of 40K. Failure of this assumption is
perhaps the most common cause of incorrect ages, often because of thermally
activated loss of 40 Ar* by diffusion, leading to ages that are too young.
3. Any non-radiogenic argon present in the sample must have the isotopie
composition of atmospheric argon, or the appropriate composition must be
identified and used in the calculations. There is 0.94% by volume of 40 Ar in
the atmosphere; this relatively high abundance is because 40 Ar continually is
being added to the atmosphere from the outgassing of magmas and by release
from rocks as they are weathered. Invariably there is a proportion of non-
radiogenic argon in the gas extracted from a sample, and this must be properly
corrected for. It is stressed that the radiogenic 40 Ar generated in situ from
decay of 40K in the sample is identical to the non-radiogenic 40 Ar. In the case
of terrestrial rocks this non-radiogenic 40Ar normally can be allowed for by
measurement of another argon isotope, 36 Ar, present in the gas extracted
from the sample. This is because the 40 Ar/36 Ar ratio in atmospheric argon is
constant at 295.5, so that the amount of atmospheric 40 Ar can be determined
by multiplying the amount of 36 Ar by 295.5. The 40 Ar* is then obtained by
difference, following subtraction of the atmospheric 40 Ar from the total 40 Ar.
In most circumstances the correction for the non-radiogenic 40 Ar in terrest-
rial rocks, using the assumption that it is of atmospheric composition, works
extremely well.
In each study undertaken it is of the utmost importance to take steps to test
these basic assumptions. This is best done empirically by measuring ages on a
suite of rocks or minerals in known relation to one another in the area under

investigation. The consistency or otherwise of the results, together with know-


ledge of the geology of the area, usually permits assessment of the appropriate-
ness of the assumptions, and provides the basis for conclusions as to the
reliability and meaning of the measured ages. A single conventional K-Ar age
can be quite misleading because there is little basis for testing whether the
underlying assumptions have been met. A 40 Ar/39 Ar age spectrum
determination, on the other hand, often enables some assessment to be made
of the reliability and meaning of the results, but, again, several measurements
are highly desirable.

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.

Experience shows that it is essential to make careful pétrographie examin-


ation of all samples prior to dating to determine whether they are suitable for

20 /. McDougall

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age determination. Such examination provides a basis for determining which
potassium-bearing minerals can be separated or whether the sample might be
measured as a whole rock if it is too fine grained to undertake mineral separa-
tion.

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

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part of the geological time scale, from several million years ago to the present,
and thus the younger limit for the application of the K-Ar dating method is
of considerable interest and relevance. This younger limit, however, is not
clearly defined, as it depends upon factors which vary from sample to sample.
Thus, a sanidine feldspar with 10% K will generate twenty times more 40 Ar*
per unit time than a sample of plagioclase with 0.5% K. Other things being
equal, it will be obvious that a sample of much younger age will be measurable
by using sanidine than plagioclase, simply because of the differences in the
rate of generation of 40 Ar*. In fact the younger limit of applicability of the
K-Ar and 40 Ar/39 Ar methods is determined by the ability to distinguish and
measure a small component of 40 Ar* above a much larger atmospheric argon
component that originates from the sample itself and from the argon extrac-
tion line.

In practice it is found that the non-radiogenic 40 Ar, normally of atmos-


pheric argon composition, varies over more than two orders of magnitude
from about 10" 10 mol/g to 10~12 mol/g 10,22,26 in samples used for K-Ar dating.
Taken together with the large range of potassium content in rocks and
minerals, this makes it difficult to uniquely specify a younger age limit for
application of the method. Typically, unaltered whole rock volcanic samples
have low atmospheric 40 Ar associated with them (1-5 x 10" 12 mol/g), and
prismatic minerals such as sanidine, especially if the surface has been cleaned
in dilute HF in the laboratory prior to argon extraction, can have atmos-
pheric 40 Ar as low as 10" 12 mol/g, but ranging up to -10" 11 mol/g. In
contrast, platy minerals such as biotite typically have much greater atmos-
pheric ^Ar associated with them, averaging -10" 10 mol/g. Thus, in
measuring ages on young rocks, sanidine with its high potassium content is
probably the most useful mineral, but its occurrence is restricted to certain
silicic volcanic rocks. Whole rock volcanic samples, often with potassium
contents in the range of 0.5 to several per cent, are particularly satisfactory
because of their low atmospheric argon contents. Biotite, although a
relatively high potassium mineral (-7%), is much less appropriate for dating
very young samples owing to its high atmospheric 40 Ar content.
If the proportion of ^Ar* relative to the total ^Ar is greater than 10% , an
age normally can be expected to be determined with a precision in the order
of 1% standard deviation. However, as the proportion of 40 Ar* decreases
relative to total ^Ar, error magnification sets in, such that if only 2% of the
40 Ar is radiogenic, the error in the age measurement is likely to approach
50% , increasing dramatically as the ^Ar* decreases toward zero. Thus, the
younger limit of application of the K-Ar dating method depends upon the
ability to detect and measure a small proportion of ^Ar*, and it will be
evident that those samples with the lowest atmospheric 40 Ar contents will be
most favourable in this respect.
To bring these various factors together, we can now consider the amount
of 40 Ar* generated per unit time. Thus, alg sample of sanidine feldspar with
10% K and of age 10,000 years, will contain 1.7 x 10" 13 mol 40Ar*; this
amount can be measured satisfactorily in a modern mass spectrometer used
for argon analysis. Taken together with an atmospheric ^Ar blank of say
5 x 10" 13 mol from the extraction line and atmospheric 40Ar of 10" 12 mol/g

22 /. McDougall

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from the sample itself in favourable cases, the proportion of 40 Ar* would be
10.8%. This indicates that in principle a sanidine of age 10,000 years can be
measured with an uncertainty of a few per cent.
Dalrymple9 demonstrated in 1968 that in fact sanidine from rhyolites about
10,000 years old are indeed measurable by the K-Ar method. In contrast, a
biotite with 7% K and 10" 10 mol/g of atmospheric 40Ar, that is 1 Ma old, will
only have -12% of 40 Ar*, so that it is clear how much less favourable this
mineral is for dating young rocks. The younger limit for whole rock volcanic
samples varies widely depending upon the actual atmospheric 40 Ar content
and the K content of the sample, but is likely to be in the range 20,000
years- -200,000 years, for a precision of 10% or better in the measured age.
Such a precision should be obtainable where the percentage of radiogenic
^Ar compared with the total ^Ar in the gas extracted from the sample is
-3%.
In an unusual approach to the isotopie measurement of Ar in a mass
spectrometer, Cassignol & Gillot6 demonstrated a precision of better than
10% for an age in cases where only 1% of the total 40 Ar was radiogenic. This
was achieved by particularly careful standardization of the mass spectrometer
as a manometrie, as well as isotopie ratio, measuring device, allowing
elimination of the 38 Ar tracer normally used. Measurements made by them
on sanidine, leucite and the groundmass of a number of volcanic rocks from
the Phlegrean Fields and Mount Vesuvius near Naples, Italy, yielded K-Ar
ages ranging from 38 000 ± 1000 years (4.5% of the^Ar recorded as radio-
genic), to 4000 ± 500 years (1% of the 40 Ar recorded as radiogenic), showing
the high age resolution available when dealing with favourable samples.
These data were shown to be consistent with the geological record, and with
the available radiocarbon ages from this area. It should be stressed, however,
that with a sample containing a low proportion of radiogenic argon, the
assumption that the non-radiogenic argon has an atmospheric argon isotope
ratio becomes critical; if this assumption is not valid, then the calculated (or
model) age can be grossly in error.
These examples illustrate why it is difficult to place a unique younger limit
as to the age of samples that can be successfully dated by the K-Ar and
40 Ar/39 Ar methods, but that with appropriate samples it is possible to
measure ages on rocks younger than 100,000 years with good precision, and
in the case of particularly favourable high potassium samples with low
atmospheric argon, ages of less than 10,000 years can be determined with
acceptable precision.

Geochronology of the Turkana Basin, northern


Kenya
To illustrate and amplify some of the points already made concerning the
application of the K-Ar and 40 Ar/39 Ar methods to the dating of sequences of
archaeological significance, results obtained on rocks exposed in the Turkana
Basin, northern Kenya, may be reviewed briefly. In terms of the approach
used in this work, the pioneering study by Evernden & Curtis12 on the geo-
chronology of the sequence at Olduvai Gorge, Tanzania, was of particular

Potassium-argon dating 23

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significance, as they demonstrated how the K-Ar dating method could be
successfully applied to such sequences.
The Pliocene to Pleistocene sediments exposed in the Turkana Basin, and
especially in the Koobi Fora region, adjacent to the eastern shores of Lake
Turkana (Fig. 3), have been the focus of intensive study since their potential
importance to palaeoanthropological and archaeological research was
recognized by R.E. Leakey in 1967. Because of the great abundance of
vertebrate fossils, including hominids, as well as stone tools, that have been
recovered from the Koobi Fora sequence, and correlative sequences else-
where in the Turkana Basin (Fig. 3), there has been much interest in estab-
lishing a numerical time scale for deposition of these sediments. More than
400 hominid fossils have been reported from the Turkana Basin sequences
(Feibel et al.14), and include many important fossils assigned to the genera

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

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Homo and Australopithecus , which provide information on the evolution of
humankind. In the Koobi Fora region, most of the hominid fossils have been
found in the upper half of the stratigraphie sequence, in the interval from just
below the KBS Tuff to near the top (Fig. 4). Much controversy has sur-
rounded attempts to measure the age of horizons within the Koobi Fora
Formation, and, in particular, the age of the KBS Tuff,8'11;15-17'23'24-27 but it
is not necessary or appropriate to deal with these problems here except in
passing. An interesting account of the controversy associated with the
numerical dating of the KBS Tuff and its bearing on the time scale of evolu-
tion of hominids is given in the book by Lewin.21
The sequence at Koobi Fora, shown in Fig. 4 after Brown & Cerling3 and
Cerling & Brown,6 consists mainly of flatlying sands, silts and clays deposited
in lacustrine, deltaic and fluvial environments similar to those observed in the
Turkana Basin today. Most of the detrital material comprising the sediments
was brought into the basin by drainage from the north via the ancestral Omo
river. Isotopie dating of the detrital sediments themselves is not particularly
useful, except to indicate that much of the material was derived from erosion
of older rocks, which commonly yield early Palaeozoic (-450 Ma) ages.

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

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Within the sequence, however, numerous tuffaceous beds are found, the
products of contemporaneous explosive eruptions of silicic (rhyolitic)
volcanoes thought to have been located somewhere in southern Ethiopia.
The ash from these eruptions blanketed the landscape, including the ancestral
Omo drainage, to be transported by water and deposited soon after in the
Turkana Basin in a manner similar to that for the normal detrital sediments.

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

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Fig. 5. 40 "Ari39 Ar age spectrum for step at the level of one standard deviation
feldspar from a pumice clast in the Silbo shown by thickness of bar. Temperature
Tuff Data plotted against fraction 39 Ar (°C) at which gas released indicated for
released. Uncertainty of the age for each each step.

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

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documented the correlations between the Koobi Fora Formation, the
Shungura Formation which crops out just to the north of Lake Turkana, and
the Nachukui Formation, adjacent to the western shores of Lake Turkana
(Fig. 3). The correlations depend upon the distinctive chemistry of the
volcanic glasses comprising the individual tuff beds, and the invariant order
of the tuffs in the sequences. Thus, the geochronology developed in one area
can be used elsewhere in the Turkana Basin. Feibel et al. 14 show that there
are now 20 horizons within the overall sequence that have been dated
precisely by the K-Ar method. The stratigraphie and geochronological
framework is now so well defined that new palaeontological or archaeological
finds commonly can be assigned an age to better than 0.1 Ma or even better
than 0.05 Ma, without the need for further geochronological measurements.
This is achievable provided that the stratigraphie level from which a sample
was recovered can be determined within the tuffaceous bed framework. With

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.

A good example of this approach is the age of 1.6 Ma assigned to the


remarkable set of bones announced by Brown et al.4 that comprise a nearly
complete skeleton of Homo erectus , recovered from sediments adjacent to
the western shores of Lake Turkana at a site known as Nariokotome III.

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

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the available results that most of the sequence is older than 2.9 Ma, although
there is conflicting evidence as to how far back in time it extends. However,
the Sidi Hakoma Tuff, near the base of the succession in the Hadar region
has been correlated geochemically with the Tulu Bor Tuff of the Koobi Fora
Formation (Brown2), for which we interpolate an age of -3.4 Ma, see also
Sarna-Wojcicki et al .30

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.

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