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Journal of Archaeological Science: Reports
journal homepage: www.elsevier.com/locate/jasrep
Best practices for calibrating and reporting stable isotope measurements in
archaeology
Paul Szpak
a,⁎
, Jessica Z. Metcalfe
b
, Rebecca A. Macdonald
b
a
Department of Anthropology, Trent University, 1600 West Bank Drive, Peterborough, ON K9L 0G2, Canada
b
Department of Anthropology, The University of British Columbia, Vancouver, BC V6T 1Z1, Canada
ARTICLE INFO
Keywords:
Isotopes
δ-Values
Calibration
Standards
Precision
Accuracy
Analytical uncertainty
ABSTRACT
The use of isotopic measurements in archaeological research has increased rapidly over the past ~ 25 years,
owing largely to the proliferation of the instruments required to produce these measurements relatively quickly
and cheaply. Unfortunately, the understanding of how to adequately calibrate and report these isotopic data has
not kept pace. We surveyed nearly 500 archaeological research papers published within the past 25 years that
presented original isotopic data. We found that, generally, the majority of studies do not provide adequate
information regarding how isotopic measurements were calibrated, nor how analytical uncertainty (precision
and accuracy) was assessed. We review and present recommendations for data analysis, calibration, and
reporting to aid archaeological researchers who use isotopic measurements and practices. We present a simple
method for quantifying standard analytical uncertainty using data that would be provided by most laboratories.
1. Introduction
Isotope ratio mass spectrometry (IRMS) is used widely in archae-
ological
1
studies to address a variety of questions. Beginning in the late
1990s, the direct interfacing of rapid and automated combustion
techniques (e.g., elemental analyzers connected via continuous-flow
to IRMS systems) for analyzing bulk organic materials decreased
analytical costs and dramatically increased the number of analyses that
could feasibly be performed in a given study. Prior to that time
relatively few isotopic studies had been conducted in archaeology,
and each study produced at most a few dozen measurements. In recent
years, an abundance of studies has been conducted, producing thou-
sands of measurements (Fig. 1). Given the now widespread availability
of technology to produce isotopic measurements quickly and cheaply, it
is important to examine how these measurements are being reported.
This is particularly important in archaeology as the researchers
primarily responsible for disseminating the results in publications are
often not directly involved in obtaining the raw measurements and
transforming them into calibrated δ-(delta) values. Moreover, results
obtained from commercial laboratories may lack the relevant details or
be difficult to interpret with respect to analytical uncertainty, particu-
larly for scholars with a limited understanding of isotope ratio mass
spectrometry. A decade ago, Jardine and Cunjak (2005) commented on
the increase in laboratories providing isotopic measurements and
recognized the potential of a widening knowledge gap between IRMS
operators and ecologists disseminating these data. We have noticed a
similarly widening knowledge gap in archaeology, particularly as it
relates to the reporting of analytical methods and uncertainty. While a
number of studies have attempted to examine within- and among-
laboratory variation in isotopic measurements, the emphasis has been
on sample preparation specifically (e.g., Guiry et al., 2016; Jørkov
et al., 2007; Sealy et al., 2014), or more generally on measurements
produced by different laboratories (e.g., Pestle et al., 2014). Little
attention has been paid to the effects of data calibration or the
quantification of measurement accuracy, precision, and overall uncer-
tainty.
The purpose of this paper was fourfold. First, we sought to evaluate
the reporting of stable carbon and nitrogen isotopic measurements and
their associated uncertainties in the archaeological literature. To do
this, we performed a review of relevant literature, focusing on data
reporting, calibration methods and quality control (accuracy and
precision). The results of this survey suggested that a review of methods
and strategies for reporting isotopic data would be useful to archae-
ologists utilizing IRMS in their research. As such, the second purpose of
the paper was to review data reporting and quality control methods and
present them in a manner accessible to researchers who are reporting
isotopic measurements but not generating the measurements them-
selves. Third, on the basis of our literature survey and review of
http://dx.doi.org/10.1016/j.jasrep.2017.05.007
Received 31 October 2016; Received in revised form 24 April 2017; Accepted 1 May 2017
⁎
Corresponding author.
E-mail address: paulszpak@trentu.ca (P. Szpak).
1
For the purposes of this discussion, we use the terms ‘archaeological’ and ‘archaeology’ as catch-alls for isotopic studies in both archaeology and physical anthropology.
Journal of Archaeological Science: Reports 13 (2017) 609–616
2352-409X/ © 2017 Elsevier Ltd. All rights reserved.
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