Molecular and isotopic investigations of potteryand ‘charred remains’ from Sannai Maruyama andSannai Maruyama No. 9, Aomori Prefecture, Japan
Carl HERON,1,§ HABU Junko,2,3
Mio KATAYAMA OWENS,4 ITO Yumiko,5 Yvette ELEY,6,*
Alexandre LUCQUIN,6 Anita RADINI,6 Hayley SAUL,6
Cynthianne DEBONO SPITERI,1,** & Oliver E. CRAIG6
ABSTRACTThis paper presents a preliminary study of the analysis of organic residues of Early and Middle
Jomon pottery and ‘charred remains.’ Samples are taken from the Sannai Maruyama site and the
Sannai Maruyama No. 9 site in Aomori City, Aomori Prefecture in northern Japan. The following
questions are addressed in this study: (i) Do organic residues survive in association with pottery
vessels and charred remains? (ii) Can the residues be identiﬁed based on molecular and isotopic
criteria applied in other investigations? (iii) Are the residues associated with the charredremains common to the residues associated with the pottery vessels? (iv) How do these residues
contribute to our understanding of food processing and consumption? Results of our analysis
indicate that the lipid composition of the pottery extracts is remarkably similar although someof the sherds exhibited better preservation and a wider range of molecules were detected albeit
in lower abundance. There is a marked contrast with the composition of the lipid extracts of the‘charred remains.’ The lipid compositions of sample sets from Sannai Maruyama and Sannai
Maruyama No. 9 suggest aquatic resources in the pottery but with a plant contribution. The‘charred remains’ from Sannai Maruyama contain plant tissues most likely with a high starchcomposition such as nuts. Lipids were recovered from the majority of the samples.
KEYWORDS: lipid, molecular analysis, isotopic analysis, Jomon pottery, Sannai Maruyama

1 School of Archaeological Sciences, University of Bradford, Richmond Road, Bradford, West YorkshireBD7 1DP UK (C.P.Heron@bradford.ac.uk)
2 Research Institute for Humanity and Nature, 457–4, Motoyama, Kamigamo, Kita-ku, Kyoto, 603–8047 Japan
3 Department of Anthropology, University of California, Berkeley CA 94720–3710 USA (habu@berkeley.edu)
4 College of Natural Resources, University of California, Berkeley CA 94720–3100 USA (miokat@berkeley.edu)
5 Editing Section of the History of Aomori Prefecture, Aomori Prefectural Government, 1–1–1 Nagashima,
Aomori 030–8570 Japan (rhus0327@gmail.com)
6 BioArCh, Department of Archaeology, University of York, Heslington, York YO10 5DD, UK(oliver.craig@york.ac.uk)§ Current address: Department of Scientiﬁc Research, The British Museum, Great Russell Street, London
WC1B 3DG, UK* Current address: Center for Integrative Geosciences, University of Connecticut, Storrs, CT 06269 USA** Current address: Institut für Ur- und Frühgeschichte und Archäologie des Mittelaters, Eberhard Karls
Universität Tübingen, Schloss Hohentübingen, 72070 Tübingen, Germany
Category: Original Article Received: 13 June 2016; Accepted: 2 August 2016
JAPANESE JOURNAL OF ARCHAEOLOGY 4 (2016): 29–52

Carl HERON et al.

1.

Introduction

As an example of early complex hunter-gatherer cultures, the Jomon culture (ca.
14,000–500 BC) on the Japanese archipelago has attracted the attention of many
prehistoric archaeologists (Habu 2004; Imamura 1996; Kobayashi 2004). Studies of
the Jomon culture can provide us with a unique opportunity to examine the causal
relationships between subsistence intensiﬁcation, population size, climate change andvulnerability of socioeconomic systems. In particular, the Middle Jomon (ca. 5300–4400
cal. BP) of northeastern Japan is known for an abundance of large settlements and theelaboration of pottery decoration. The subsistence base for these large settlements has
been a topic of debate. In this context, a key question is the importance of marine foodin Jomon diet and its changes through time in relation to changes in settlement size andresidential mobility. This question is also tied to a more theoretical question of whether
large, sedentary hunter-gatherer settlements in the temperate zone reﬂect the use of awide variety of food, or whether their subsistence activities have focused on a speciﬁctype of food resource (e.g., Habu 2014). Carbon and nitrogen stable isotope analysis ofJomon skeletal remains have helped us address these questions in terms of identifying
the importance of marine vs. terrestrial protein sources (e.g., Minagawa 2001; Minagawa& Akazawa 1992; Yoneda 2010; Yoneda et al. 2011), but this method is applicable only
when skeletal remains are well preserved. In the case of Japan where the soil is extremely
acidic, this means primarily at shell midden sites only.
This paper presents a preliminary study to approach this issue through the analysisof organic residues of Early and Middle Jomon pottery. Samples are taken from the
Sannai Maruyama site (ca. 5900–4400 cal. BP) and the Sannai Maruyama No. 9 site(ca. 5300–4400 cal. BP) in Aomori City, Aomori Prefecture in northern Japan. Eighteen
pottery vessel sherds and eight ‘charred remains’ were investigated. The charredremains are isolated ﬁnds and not associated with, or adhering to, pottery vessel sherds.
Nevertheless the curvature on these ﬁnds does indicate that they were once in contact
with a container although this may or may not be ceramic in nature. Sannai Maruyama
is the largest Jomon settlement site associated with more than 600 Early and Middle
Jomon pit-dwellings (Habu 2004: 108–132; Okada 2003). Sannai Maruyama No. 9 isanother Middle Jomon site in Aomori City (Aomori Archaeological Center 2007, 2008,2010). Approximately 500 m away from the Sannai Maruyama site, it is associated withwaterlogged middens. Figure 1 shows the locations of these sites.
The pottery chronology indicates that Sannai Maruyama was occupied from the
middle of the Early Jomon period (ca. 5900 cal. BP) to the end of the Middle Jomon
period (ca. 4400 cal. BP). The occupational span can be divided into 12 pottery phases.
© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

Figure 1.

Site locations

They are: Early Jomon Lower Ento-a through d, Middle Jomon Upper Ento-a through e,
Enokibayashi, Saibana, and Daigi 10 phases from the oldest to the latest.
Subsistence strategies of the Sannai Maruyama and Sannai Maruyama No. 9 sites
have been a topic of debate. Many scholars have suggested the possibility that chestnut(Castanea Crenata) was the staple food of the Sannai Maruyama residents from theLower-Ento-b to Upper Ento e-phases, although an abundance of chestnut pollen is moreevident in the Early Jomon layers. Due to uneven preservation conditions within the site,
reports of faunal remains from the Sannai Maruyama site are primarily from the ﬁrst
two phases of the site occupation: Lower-Ento-a and b phases (c. 5900–5600 cal. BP)(see Habu 2004). An abundance of grinding stones, presumably plant food processing
tools, is particularly noticeable from the Upper-Ento-b to e phases (ca. 5200–4900 cal.
BP) (Habu 2004, 2008). The Sannai Maruyama No. 9 site, which is dated to the Middle
Jomon period, is known for an abundance of buckeye (Aesculus turbinata; also known
as horse chestnut) remains from its waterlogged midden. Chestnut remains are also
© Japanese Archaeological Association

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Carl HERON et al.

recovered from the same midden, and the relative frequency of these two taxa changed
through time. No faunal remains have been reported from this site. Given these lines ofevidence, we expect that the foodways of the residents of these sites may have changed
signiﬁcantly through time.
The potential for the analysis of organic residues from pottery vessels of the Jomon
culture has been demonstrated in a number of recent publications (e.g., Craig et al. 2013;
Horiuchi et al. 2015; Lucquin et al. 2016). The following questions are addressed in thisstudy: (i) Do organic residues survive in association with pottery vessels and charredremains? (ii) Can the residues be identiﬁed based on molecular and isotopic criteria
applied in other investigations? (iii) Are the residues associated with the charred remains
common to the residues absorbed in the pottery sherds? (iv) How do these residues
contribute to our understanding of food processing and consumption at the sites?

2.

The samples

Sannai Maruyama and Sannai Maruyama No. 9: Potsherds (Figure 2)

Two potsherds excavated from the Sannai Maruyama No. 9 site (J1−J2) and sixteen
pottery sherds excavated from the Sannai Maruyama site (J3−J18) were selected for thisanalysis.
J1 and J2 are from the Sannai Maruyama No. 9 site. Both of them were collectedin summer 2007 from the block soil sample that had been collected in 2006 from thewaterlogged midden at the site by Aomori Archaeological Center (Aomori ArchaeologicalCenter 2008). The midden layers from which these sherds were excavated are dated to theﬁrst half of the Middle Jomon period, from the Upper-Ento-b phase to the Upper-Ento-ephase. AMS dates obtained from these midden layers range from ca. 5200 to 5000 cal.
BP (Ito & Habu 2015).
The 16 potsherds excavated from the Sannai Maruyama (J3−J18) come from threedifferent contexts. J3−J13 were obtained in Summer 1997 from the 6th Excavation
Area of the site, a waterlogged midden at the northwestern edge of the site (Cultural
Affairs Section of the Agency of Education of Aomori Prefecture 1998b). J3 is dated
to the Middle Jomon Upper-Ento-b phase (ca. 5200 cal. BP). J4−J13 are dated to theLower-Ento-d phase, the last pottery phase of the Early Jomon period dated to ca.
5500–5300 cal. BP. J14-17 are Middle Jomon potsherds, and were excavated at the timeof the 30th Excavation in Summer 2006 (Cultural Affairs Section of the Agency of
Education of Aomori Prefecture 2008). This was a re-excavation of the 6th Excavation
area. These potsherds were recovered at the time of the removal of the backﬁll of the1997 excavation. Because Middle Jomon large postholes are reported from this area, it ismost likely that these potsherds were originally associated with a Middle Jomon feature© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

Figure 2.

Photos of potsherd samples (J1−J18)

dug into the Early Jomon layers. J18 was found from the test excavation area of the
Sannai Maruyama site in summer 2007. The sherd came from a small-pit, most likely
dated to the latter half of the Middle Jomon period. Among all the samples, this was the
only one that comes from a non-waterlogged depositional context.

Sannai Maruyama: ‘Charred remains’ (Figures 3 and 4)

At Sannai Maruyama, charred remains that look like ‘foodcrusts’ (the charred deposits
occasionally observed on pottery vessel surfaces) were recovered through wet-sieving ofsoil samples obtained from waterlogged middens. These were recovered in isolation and© Japanese Archaeological Association

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Carl HERON et al.

Table 1.

Pottery sherds from Sannai Maruyama No. 9 (J1−J2) and Sannai Maruyama (J3−J18)

Sample No.
I=interior;
E=exteriorContext & original
sample No.

Collection
date

Phase

Jomon Subperiod

Depositional
context

J1I

Sannai Maruyama No.
9, SX-10, Block 2,
Layer 2a8/4/2007

Upper-Ento?

Middle Jomon

J2I

Sannai Maruyama No.
9, SX-10, Block 2,
Layer 2d-3

8/4/2007

Upper-Ento?

J3I

Sannai Maruyama,
6th Excavation Area,
North Wall

7/29/1997

J4I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 40Sherd a

J4E

Sherd Condition

Sampledescription

Waterlogged

Potsherd, unwashedand stored in Ziploc
after recovery

Interior
surfacedrilling

Middle Jomon

Waterlogged

Potsherd, unwashed inaluminium foil, then
ZiplocInterior
surfacedrilling

Upper-Ento-b

Middle Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

7/25/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 40Sherd a

7/25/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Exterior
surfacedrilling

J5I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 40Sherd b

7/25/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J6I

Sannnai Maruyama,
6th Excavation Area,
North Wall, Cut 40Sherd c

7/25/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J7I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 41

7/25/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J8I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 47Sherd a

7/28/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J9I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 47Sherd b

7/28/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J10I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 47Sherd c

7/28/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J11I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 47Sherd d

7/28/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

Table 1. Pottery
Continued
sherds from Sannai Maruyama No. 9 (J1−J2) and Sannai Maruyama (J3−J18)
Sample No.
I=interior;
E=exteriorContext & original
sample No.

Collection
date

Phase

Jomon Subperiod

Depositional
context

J12I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 47Sherd e

7/28/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J13I

Sannai Maruyama,
6th Excavation Area,
North Wall, Cut 47Sherd f

7/28/1997

Lower-Ento-d

Early Jomon

Waterlogged

Potsherd, washed thenstored in Ziploc

Interior
surfacedrilling

J14I

Sannai Maruyama,
30th Excavation,
backﬁll-Sherd a7/2006Upper-Ento

Middle Jomon

Waterlogged

Unwashed, stored in
Ziploc after recovery

Interior
surfacedrilling

J15I

Sannai Maruyama,
30th Excavation,
backﬁll-Sherd b

7/2006Upper Ento

Middle Jomon

Waterlogged

Unwashed, stored in
Ziploc after recovery

Interior
surfacedrilling

J16I

Sannai Maruyama,
30th Excavation,
backﬁll-Sherd c

7/2006Upper-Ento

Middle Jomon

Waterlogged

Unwashed, stored in
Ziploc after recovery

Interior
surfacedrilling

J17I

Sannai Maruyama,
30th Excavation,
backﬁll-Sherd d7/2006Upper-Ento

Middle Jomon

Waterlogged

Unwashed, stored in
Ziploc after recovery

Interior
surfacedrilling

J17E

Sannai Maruyama,
30th Excavation,
backﬁll-Sherd d7/2006Upper-Ento

Middle Jomon

Waterlogged

Unwashed, stored in
Ziploc after recovery

Exterior
surfacedrilling

J18I

Sannai Maruyama,
Test excavation, Test
Trench 6, ‘post hole?’
top

8/8/2007

Un-known

Middle Jomon

Dry

Unwashed, wrappedin aluminium foil,then in a paper
envelope placed inplastic box

Interior
surfacedrilling

Sherd Condition

Sampledescription

not adhering to pottery or other vessel surfaces. That noted some displayed smooth andcurved surfaces suggesting the possibility that they had originally been in contact withsome form of container. Impressions in some of these charred remains suggest someform of basketry. Eight samples of these charred remains were selected for analysis withthe aim of determining if the lipid residues from the pottery share a common origin withthe lipids extracted from these charred remains. Photos and drawings of these samples
are shown in Figures 3 and 4. All samples were ﬁrst water-screened, then dried andstored in Ziploc plastic bags. Given their unique form, we assume that these are different
from so-called ‘Jomon cookies’ and other solid forms of charred food remains that havebeen reported from Jomon sites in central Japan.
All of these samples were found by site technicians at the time of sorting organic
remains within the water-screened samples, and were provided by the Preservation Ofﬁce© Japanese Archaeological Association

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Carl HERON et al.

Figure 3.

Photos of samples of the charred remains (J19−J26)

Figure 4.

Drawings of samples of the charred remains (J19−J26)© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

Table 2.

‘Charred remains’ from Sannai Maruyama
Jomon
Sub-period

Depositional
context

Lower- Ento-a

Early Jomon

Waterlogged

Sannai Maruyama, T-tower, VII F-74-4,
Layer VIa, Specimen “b”

Lower- Ento-a

Early Jomon

Waterlogged

J21

Sannai Maruyama, T-tower, VII F-74-4,
Layer VIa, Specimen “c”

Lower- Ento-a

Early Jomon

Waterlogged

J22

Sannai Maruyama, T-tower, VII F-74-4,
Layer VIa, Specimen “d”

Lower- Ento-a

Early Jomon

Waterlogged

J23

Sannai Maruyama, T-tower, VII F-74-4,
Layer VIa, Specimen “e”

Lower- Ento-a

Early Jomon

Waterlogged

J24

Sannai Maruyama, T-tower, VII F-74-4,
Layer VIa, Specimen “f”

Lower- Ento-a

Early Jomon

Waterlogged

J25

Sannai Maruyama, T-tower, VII F-74-4,
Layer VIa, Specimen “g”

Lower- Ento-a

Early Jomon

Waterlogged

J26

Sannai Maruyama, Northern Valley,
F-30274, 4 mm

Lower-Ento-a or b

Early Jomon

Waterlogged

SampleContext and original sample No.

J19Sannai Maruyama, T-tower, VII F-74-4,
Layer VIa, Specimen “a”

J20

Phase

of the Sannai Maruyama site to the East Asian Archaeology Laboratory of the Universityof California for further analysis. Samples J19−J25 were originally excavated from Layer
VIa of the Transmission Tower (Cultural Affairs Section of the Agency of Education of
Aomori Prefecture 1998a), a waterlogged midden layer dated to the Lower-Ento-a phaseof the Early Jomon period (ca. 5900–5650 cal BP). J26 is from a waterlogged midden
called “the Northern Valley” (Cultural Affairs Section of the Agency of Education of
Aomori Prefecture 2014), which is dated to the Lower-Ento-a to Lower-Ento-b phase of
the Early Jomon period (ca. 5900–5500 cal BP).

3.

Materials and methods

Prior to GC-MS (gas chromatography-mass spectrometry), drilled pottery samples (2 g) or
powdered charred remains (10–20 mg) were weighed into scintillation vials and covered
with 10 mL of AnalaR grade dichloromethane/methanol (2/1 v/v ratio), ultrasonicated for
2×15 minutes, and then centrifuged for 5 minutes at 2000 rpm. The supernatant wasdecanted using a disposable Pasteur pipette, and placed in a Hach tube. The extraction
process was repeated three times to ensure maximum lipid extraction. The solvent was© Japanese Archaeological Association

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Carl HERON et al.

then evaporated under a gentle stream of nitrogen and mild heating to retain the lipid
extract. The extracts were either methylated or silylated. Methylation was achieved
using 100 µL boron triﬂuoride in methanol (14% w/v), and heating the mixture for 20
minutes at 70°C. The reaction was quenched using two drops of deionised water andextracted using 3×1 mL aliquots of hexane. The samples were then dried under nitrogenand redissolved in dichloromethane. Silylation was achieved by adding three drops of
BSTFA (N,O-bis(trimethylsilyl)triﬂuoroacetamide) with 1% TMCS (trimethylchlorosilane)to each of the dried lipid extracts and heated at 60°C for 15 minutes. The samples wereonce again evaporated to dryness under a gentle stream of nitrogen and redissolved indichloromethane.
Prior to GC-C-IRMS (gas chromatography-combustion-isotope ratio mass spectrometry),
lipids were extracted from the sherds and charred remains in one-step with acidiﬁed
methanol. Methanol (1 and 4 mL respectively) was added to homogenized charred remains(10–30 mg) or sherds (1 g) and the mixture ultrasonicated for 15 min. The solvent was thenacidiﬁed with concentrated sulphuric acid (200 or 800 mL respectively). The acidiﬁed
suspension was heated in sealed tubes for 4 h at 70°C and then cooled, and lipids wereextracted with n-hexane (3x). Dissolved sulphur was removed by treatment with activatedcopper turnings. The samples were analysed directly by GC-C-IRMS as described below.

Bulk isotope analysis

Bulk carbon and nitrogen isotope analysis was undertaken on the charred remains(1–2 mg). The samples were dried and weighed into tin capsules. C and N isotope
analyses were performed on a Europa 20-20 mass spectrometer ﬁtted with a Roboprep
combustion unit. All samples were determined in duplicate.

Gas Chromatography-Mass Spectrometry (GC-MS)

Analysis was carried out on an Agilent 7890A Series GC connected to a 5975C Inert
XL mass selective detector. The splitless injector and interface were set at 300°C and
325°C respectively, and helium was used as the carrier gas at constant inlet pressure. Theoven temperature was initially kept at 50°C for 2 minutes, then ramped to 325°C at 10°C
min−1 and held for 10 minutes. The GC column, a 30 m×0.25 mm, 0.25 µm HP-5MS 5%
Phenyl, 95% dimethylpolysiloxane phase fused silica column, was directly inserted into
the ion source. Electron impact (EI) spectra were obtained at 70 eV with full scan fromm/z 50 to 800.

Gas Chromatography-combustion—Isotope Ratio Mass Spectrometry(GC-C-IRMS)

The stable carbon isotopic compositions of individual lipids were determined in© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

duplicate using a Delta V Advantage isotope ratio mass spectrometer (Thermo Fisher,
Bremen, Germany) linked to a Trace Ultra gas chromatograph (Thermo Fisher) witha ConFlo IV interface (Cu/Ni combustion reactor held at 1000°C; Thermo Fisher).
Samples were diluted in hexane and 1 mL was injected onto a DB-5MS fused silica
column (30 m×0.25 mm×0.25 mm; J&W Scientiﬁc). The temperature programme was
1 min at 45°C min−1 to 295°C and 15 min at 295°C. Ultra-high purity grade helium
was used as the carrier gas (at a ﬂow rate of 1.4 mL min−1). The ion intensities of m/z
44, 45, and 46 were monitored and the 13C/12C and 18O/16O ratios of each sample peakwere automatically computed (Isodat version 3.0; Thermo Fisher) by comparison witha standard reference CO2 gas of known isotopic composition, which was repeatedly
measured with each sample. All results are reported in per mil (‰) relative to VPDB
international standard. Replicate measurements of each sample and a mixture of FAMEs
with δ13C values traceable to international standards (Indiana F8 standard; obtained
from Arndt Schimmelmann, Indiana University, Bloomington, IN, USA) were used todetermine instrument precision (<0.3‰) and accuracy (<0.5‰). The values of unknown
samples were corrected for methylation by comparison with standard C18 : 0 and C16 : 0 fatty
acids of known isotopic composition, which were methylated with each batch of samples
using identical reagents and procedures.

Starch granules and phytoliths

To investigate the presence of plant remains, starch granules, phytoliths (silica bodies)and plant tissues were extracted from samples taken from six charred remains. The
extraction procedures followed established protocols by Saul et al. (2012). Charredremains ranging from 4.79 mg to 9.12 mg were ﬁrst treated with 3% H2O2; 10 mL for
15–30 min and then manually disaggregated. The samples were then centrifuged (1000x;
3 min). Then the supernatant was reduced to 2 mL, and the residues washed three times
with UltraPure water. Residues were then made up to 1 mL suspensions. The supernatant
was mounted on microscope slides and left to dry at room temperature. Finally a drop ofglycerol was placed at top of the dried residues and a glass cover slip placed above it toallow any starch granules or phytoliths present in the mixture to be observed in rotatedplanes. The mounted slides were examined using an inverted polarising microscopeﬁtted with a digital camera. All silica bodies and starches were counted by scanning themounted specimen in a grid pattern at a magniﬁcation of 630x.

4. Results
Bulk isotopic analysis

The results are shown in Table 3. The %nitrogen in the charred remains is consistently© Japanese Archaeological Association

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Carl HERON et al.

Table 3.

Bulk carbon isotope determinations undertaken in duplicate on the charred remains

Sample%C

δ13C (‰)%N

δ15N (‰)

C/N ratio

J19
J20
J21
J22
J23
J24
J25
J26

51.1
54.5
53.7
49.7
53.7
61.7
53.4
53.8

−24.7
−24.8
−25.5
−24.8
−25.1
−25.9
−25.0
−25.2

1.3
1.3
1.5
1.2
1.2
1.3
1.5
1.1

−1.8
−1.1
0.6
0.2
−1.6
−1.7
−1.5
1.1

47.3
50.4
40.7
48.1
52.1
57.1
40.5
56.7

low (1.1–1.5%) with much higher %carbon (49.7–61.7%). The δ13C values range from
−24.7 to −25.9‰. Such values could indicate terrestrial C3 plants or animals consuming
C3 plants. The very high (>40) C/N atomic ratios compare well with the C/N ratios ofcharred modern starchy foods cooked in pottery vessels including acorns and chestnuts(Yoshida et al. 2013, Figure 4). This study also showed that cooking acorn, chestnut andhorse chestnut in pottery vessels resulted in relatively small shifts in δ13C values within±2‰. The C/N ratios for terrestrial animal tissues and marine foods were all below 22.
Interestingly the δ13C values given by the starchy foods in this study are between −22
to −30‰, which is consistent with the values reported in here. Values for modern C3nuts, corrected according to the Suess effect, have been reported with δ13C values of−25.4±1.6‰ and δ15N values of 1.2±2.4‰ (n=16; Shimojo reported in Yoneda et al.
2004, 103).
Figure 5 plots δ15N values against atomic C:N ratio for the charred remains from
Sannai Maruyama. These data are compared with charred deposits (n=70) recoveredfrom pottery vessel surfaces from Torihama (Fukui Prefecture, Incipient, Initial and
Early Jomon contexts) and examples of charred plants dating to the Incipient Jomon(Kudo 2014). The Torihama samples have been shown, by GC-MS and GC-C-IRMS
analysis, to be dominated by lipids consistent with aquatic sources, both marine andfreshwater (Lucquin et al. 2016). In contrast, the Sannai Maruyama remains, with low
δ15N values and high C:N ratios, are consistent with plant tissues as evidenced by thecomparison with examples of charred plant remains from Incipient Jomon contexts andby comparison with literature values.

Gas Chromatography-Mass Spectrometry (GC-MS)

It has been demonstrated, largely by experimental means, that both quantitative andqualitative changes in lipids occur during pottery use and burial (Evershed 2008a). These
data suggest an overall depletion in lipids over time. Qualitatively, loss of triacylglycerols© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

Figure 5. Plot of δ15N values vs. atomic C:N ratio showing the charred remains from Sannai
Maruyama compared with ‘ foodcrusts’ (n=70) recovered from pottery vessel surfaces from
Torihama (Fukui Prefecture; Incipient, Initial and Early Jomon contexts) and examples of charred
plants dating to the Incipient Jomonby hydrolysis and unsaturated n-alkenoic acids by oxidation are commonly observed
although the rate of change is dependent on the burial environment. Clear differences
are observed between degraded food lipids absorbed in pottery vessel sherds and lipids
extracted from the associated sedimentary matrix (e.g., Heron et al. 1991). Most lipid
compounds in foods and sedimentary matrices are hydrophobic and immobile althougha minor contribution of soil lipid to the extracts from the pottery sherds and the charredremains cannot be ruled out entirely. The range of lipid marker compounds detected inarchaeological residues must be evaluated carefully to identify the most likely origin.
The presence of molecules derived from thermal alteration of lipids (ω-(o-alkylphenyl)alkanoic acids) and sugars (levoglucusan) reinforces the view that archaeological residues
are consistent with food processing, such as cooking. Further evaluation of the foodsource is obtained by compound speciﬁc carbon isotope analysis of the most abundantn-alkanoic acids in the residues.

Sannai Maruyama ‘charred remains’—methylated extracts

Gas chromatography-mass spectrometry was undertaken on methylated solvent extracts© Japanese Archaeological Association

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Carl HERON et al.

Table 4. Lipid composition of residues extracted from the charred remains (methylated extracts)
Samplen-alkanoic acids

n-alkenoic acids

Dioic acids

ω-(o-alkylphenyl)alkanoic
acids

J19
J20
J21
J22
J23
J24
J25
J26

C14 : 0–C28 : 0
C14 : 0–C22 : 0
C14 : 0–C26 : 0
C14 : 0–C22 : 0
C14 : 0–C20 : 0
C14 : 0–C24 : 0
C14 : 0–C24 : 0
C14 : 0–C28 : 0

C18 : 1
C18 : 1
C18 : 1
C18 : 1
C18 : 1
C18 : 1
C18 : 1
C18 : 1

C16 : 0–C22 : 0
C16 : 0–C22 : 0
nd
nd
trace
nd
nd
nd

C18
C18
C18
C18
C18
C18
C18
C18

nd—not detected

Figure 6. Extracted ion (m/z 105) chromatogram highlighting C18 ω-(o-alkylphenyl)alkanoic acidisomers (peaks labelled *) in sample J20 (charred remains). The peaks labelled 16, 18, 20 and 22
correspond to n-alkanoic acids with n carbon atoms respectivelyof the charred remains (Table 4). The major components in each sample are saturated nalkanoic acids. Although dominated by hexadecanoic (C16 : 0; palmitic) and octadecanoic(C18 : 0; stearic) acids, a wider range of n-alkanoic acids is present from tetradecanoic acid
(C14 : 0) up to octacosanoic acid (C28 : 0) in two cases. Unsaturated n-alkenoic acids are
restricted to a trace of octadecenoic acid (C18 : 1). Long-chain dioic (dicarboxylic) acids
were detected in three samples. Sterols are absent as are isoprenoid acids such as phytanic© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

acid. No n-alkanols or dihydroxyalkanoic acids were detected. The methylated extractsof all samples also show clear evidence for the presence C18 ω-(o-alkylphenyl)alkanoic
acid isomers (Figure 6). The mechanism underlying the formation of these compounds
as a result of thermal action on n-alkenoic acids has been addressed in detail in Evershed
et al. (2008). A wider range (from C16 –C22) of these molecules has previously beenreported as constituents of heated marine and freshwater organisms in pottery vessels ofarchaeological date and form from unsaturated fatty acids present in the fresh tissue lipid(Evershed 2008b; Heron et al. 2010; Craig et al. 2011, 2013). Only C18 ω-(o-alkylphenyl)alkanoic acid isomers were detected in the charred remains and, together with the absenceof any isoprenoid acids, it suggests that the charred remains do not comprise a marine or
freshwater contribution. The detection of C18 ω-(o-alkylphenyl)alkanoic acid isomers onlyis likely to derive from a source dominated by C18 alkenoic acids (C18 : 1, C18 : 2 and C18 : 3).
This supports a plant source and is consistent with the bulk isotope data.

Sannai Maruyama ‘charred remains’—trimethylsilylated extracts

Lipid extracts of two samples (J19 and J21) were subjected to trimethylsilylation prior to GCMS and the summary table is shown in Table 5. These extracts are characterised by awider range of short-chain alkanoic acids than was detected in the methylated extracts.
A plant sterol (sitosterol) was detected in J19 but not in J21. Levoglucosan and otherunidentiﬁed sugars were detected in the trimethylsilylated extracts. Levoglucusan isa monosaccharide pyrolysis product of cellulose and hemicellulose (Simoneit et al.
1999), although it is also produced by combustion of lignite or brown coal (Fabbri et al.
2009). This lends further support to the plant origin of the charred remains. In addition,
butanedioic acid was identiﬁed along with several substituted benzoic acid derivatives in
low abundance.

Sannai Maruyama pottery sherds—methylated extracts

The lipid composition of the methylated extracts is shown in Table 6. The absence of awider range of compound classes in these extracts, such as sterols, n-alkanols and so on,
is explained by the fact that since many of them have free –OH groups they will not bemethylated and thus are unlikely to pass through the GC column. No ω-(o-alkylphenyl)alkanoic acids were identiﬁed. Most samples comprise low levels of a relatively narrow
range of n-alkanoic acids. However, several extracts comprise a well-preserved lipid
fraction with a range of n-alkenoic acids present. The isoprenoid, phytanic acid, was also
detected in these samples.

Sannai Maruyama pottery sherds—trimethylsilylated extracts

Three of the well-preserved lipid residues (J10, J11 and J13) were re-extracted and© Japanese Archaeological Association

43

Carl HERON et al.

Table 5. Lipid composition of residues extracted from the charred remains and trimethylsilylated
prior to analysis
Samplen-alkanoic acids

n-alkenoic acids

Sitosterol

SugarsJ19
J21

C6 : 0–C26 : 0
C6 : 0–C26 : 0

C18 : 1
C18 : 1

Yes
nd

Yes
Yes

nd—not detected

Table 6. Lipid composition of methylated residues extracted from Sannai Maruyama pottery sherds
Samplen-alkanoic acids

n-alkenoic acids

Phytanic acid

J1
J2
J3
J4I
J4E
J5
J6
J7
J8
J9
J10
J11
J12
J13
J14
J15
J16
J17I
J17E
J18

nd
C14 : 0–C30 : 0
C14 : 0–C18 : 0
C16 : 0–C18 : 0
C16 : 0
C16 : 0–C18 : 0
C16 : 0–C18 : 0
C16 : 0–C28 : 0
C16 : 0C14 : 0–C18 : 0
C14 : 0–C30 : 0
C14 : 0–C26 : 0
C16 : 0C14 : 0–C30 : 0
C16 : 0–C18 : 0
C16 : 0–C18 : 0
C16 : 0–C18 : 0
C16 : 0–C18 : 0
nd
nd

nd
C18 : 1–C24 : 1
C18 : 1
C18 : 1nd
nd
C18 : 1
C18 : 1nd
nd
C18 : 1–C22 : 1
C18 : 1–C22 : 1nd
C18 : 1–C22 : 1nd
nd
C18 : 1
C18 : 1
nd
nd

No
Yes
nd
nd
nd
nd
nd
nd
nd
nd
Yes
Yes
nd
Yes
nd
nd
nd
nd
nd
nd

nd—not detected

trimethylsilylated prior to GC-MS. The results are presented in Table 7. The lipid
composition of these residues is remarkably similar. Figure 7 shows the lipid extract of
sherd J10. The main constituents are C16 : 0 and C18 : 0. A wider range of n-alkanoic acids
was detected in lower abundance from C6 : 0 to C30 : 0. As expected, even-carbon number
acids dominate over odd although traces of C11 : 0 to C17 : 0 are clearly seen. Unsaturated(alkenoic) acids are detected in very low abundance. In addition to the detection of
octadecenoic (C18 : 1) acid, eicosenoic (C20 : 1), docosenoic (C22 : 1) and tetracosenoic (C24 : 1)
were identiﬁed. Traces of hexadecenoic (C16 : 1) and hexacosenoic (C26 : 1) acids were also
© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

Table 7. Lipid composition of residues extracted from Sannai Maruyama pottery sherds(trimethylsilylated extracts)
Samplen-alkanoic
acids

n-alkenoic
acids

J10
J11
J13

C6 : 0–C30 : 0
C6 : 0–C30 : 0
C6 : 0–C30 : 0

C16 : 1–C26 : 1
C16 : 1–C26 : 1
C16 : 1–C26 : 1

Phytanic
Cholesterol
acid
Yes
Yes
Yes

Yes
Yes
Yes

Sitosteroln-alkanols

Dihydroxyalkanoic
acids

Yes
Yes
Yes

C22–C32
C22–C32
C22–C32

C16 : 0–C22 : 0
C16 : 0–C22 : 0
C16 : 0–C22 : 0

Figure 7. Extracted ion current (m/z 129) chromatogram of the lipid extract of sample J10. The
peaks labelled 8 to 30 are saturated n-alkanoic acids with n carbon atoms. C16 : 0 and C18 : 0 are plotted
off the scale to highlight the wide distribution of acids in low abundance. Peaks labelled n:1 are nalkenoic acids with n carbon atoms and one double bond. Peaks labelled * are dihydroxyalkanoic
acids with 18, 20 and 22 carbon atoms respectively in order of elution. C—cholesterol, S—sitosterol,
T—unassigned triterpenoid (base peak, m/z 189)

identiﬁed in very low abundance. Longer chain n-alkenoic acids are not commonly
reported in lipid residues of archaeological date. These molecules can be found in planttissues, although their occurrence is restricted, and in the tissues of aquatic organisms.
One isoprenoid acid (phytanic) is present. Both cholesterol and sitosterol are present
and suggest both animal and plant products associated with the vessels. Acyl lipid ishighly depleted in all samples. In J10 a trace of monopalmitin survives suggesting thathydrolysis has impacted signiﬁcantly on the lipid residue. A series of n-alkanols (C22–
C32) was also detected by scanning for the characteristic m/z 103 ion. This also supports© Japanese Archaeological Association

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Carl HERON et al.

a plant contribution.
Although ω-(o-alkylphenyl)alkanoic and dioic acids are absent, a suite ofdihydroxyalkanoic (C16 : 0 –C22 : 0) is present in all three extracts. Although molecularions are absent, M-15 ions are seen at m/z 489, 517, 545 and 573 respectively in mass
spectra of the C16 : 0, C18 : 0, C20 : 0 and C22 : 0 acids. Dihydroxyalkanoic acids are degradation
products of monounsaturated alkenoic acids formed via secondary reactions withhydroperoxides (Hansel & Evershed 2009). This study demonstrated that the positions of
the hydroxyl groups correspond to the position of the double bond in the precursor fatty
acid. This biomarker can help to distinguish aquatic from terrestrial resources (Hansel &Evershed 2009; Heron et al. 2010) and can be helpful where vessel contents may not havebeen subject to protracted heating leading to the formation of ω-(o-alkylphenyl)alkanoic
acids (Hansel et al. 2011).
The presence of dihydroxyalkanoic acids in the residues adds signiﬁcantly to theinterpretative potential of the lipid biomarker evidence since the positions of thehydroxyl groups identify the position of the double bond in the precursor alkenoic
acid. Whereas 9,10-dihydroxyoctadecanoic acid is indicative of 9-octadecenoic acid—aubiquitous constituent of most fats and oils, 11,12-dihydroxydocosanoic acid derives
from 11-docosenoic acid (C22 : 1; cetoleic acid)—the most abundant C22 : 1 n-alkenoic
acid in marine organisms (Morris & Culkin 1989, 149; Heron et al. 2010). In contrast
13,14-dihydroxydocosanoic acid is formed from 13-docosenoic acid (erucic acid)and is the most common C22 : 1 n-alkenoic acid found in terrestrial plants. Indeed
13,14-dihydroxydocosanoic acid has been reported in residues of probable plant(Brassicaceae) oils in pottery vessels of archaeological date (Colombini et al. 2005;
Copley et al. 2005). The predominance of the 11,12-dihydroxydocosanoic acid isomer insample J10 suggests the presence of lipid derived from aquatic organisms—either marineor freshwater. The survival of long chain n-alkenoic acids (C20 : 1, C22 : 1, C24 : 1, and C26 : 1)
provides strong corroborative evidence of this conclusion.
Further data in support of an aquatic contribution to these residues is the presence ofphytanic (3,7,11,15-tetramethylhexadecanoic) acid. Plant tissues do not contain phytanicacid. Nevertheless it is a constituent of ruminant animals (both in the adipose tissues andmilk) as well as marine and freshwater organisms and is produced when phytol, liberated
from chlorophyll in the gut, is converted to phytanic acid and incorporated into the tissuesof the organism. This molecule was detected in both the methylated and trimethylsilylated
extracts of J10, J11 and J13. Aquatic tissues comprise relatively high concentrations ofisoprenoid acids, particularly phytanic acid, pristanic (2,6,10,14-tetramethylpentadecanoic)
acid and 4,8,12-TMTD (4,8,12-trimethyltridecanoic acid). These molecules have also been
identiﬁed in pottery vessels associated with the processing of marine and freshwater
resources (Hansel et al. 2004; Craig et al. 2007; Craig et al. 2011; Craig et al. 2013).
© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

Compound speciﬁc carbon isotope analysis

Analysis of the carbon isotope composition of the C16 : 0 and C18 : 0 n-alkanoic acids fromboth pottery residues and the charred remains show distinctive proﬁles (Figure 8). Twoof the charred remains plot in the range identiﬁed for chestnuts from analysis of modern
Japanese reference materials, while the lipids extracted from the pottery are indicative of
terrestrial animals, salmonids and, in one instance, marine resources. It is also worthy ofnote, however, that some of the intermediate values for these two n-alkanoic acids could
be the result of two-member mixing between plant and marine resources as suggested by
the lipid biomarker data. The differences between the charred remains and the pottery
lipids suggest that the two types of samples found at the site represent distinct foodprocessing activities.

Microscopic analysis of ‘charred remains’

The analysis yielded very low counts of starch granules and phytoliths, identiﬁed inonly two samples. However all samples were found to have a variable amount of poorly
diagnostic plant tissues, mostly very small in size, suggesting plant processing (forstorage) was occurring. Among these are the remains of epidermis tissues consistent withthe pericarp and spermoderm of chestnuts, buckeyes and acorns. Although unambiguous
identiﬁcation cannot be achieved from these data alone, in part due to the fragmentary
nature of the remains, the presence of plant tissues in the charred remains supports the

Figure 8. δ13C values of C16 : 0 and C18 : 0 n-alkanoic acids extracted from pottery (grey circles)
and charred remains (black triangles). The data are compared with reference ranges for authentic
reference lipids from modern tissues and archaeological bone (66.7% conﬁdence)© Japanese Archaeological Association

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Carl HERON et al.

molecular and isotope data for the plant origin of the charred remains.

5. Conclusions
The lipid composition of the pottery extracts is remarkably similar although some of thesherds exhibited better preservation and a wider range of molecules were detected albeit
in lower abundance. There is a marked contrast with the composition of the lipid extractsof the charred remains. Table 8 summarises the ﬁndings. The lipid compositions of these
two sample sets suggest aquatic resources in the pottery but with a plant contribution. The
charred remains contain plant tissues most likely with a high starch composition such as nuts.
Lipids were recovered from the majority of the samples. Preservation varies althoughn-alkenoic acids and acyl lipids are considerably depleted compared with modern fats andoils. This is in accordance with published data on lipids extracted from pottery vessels
and charred remains from other parts of the world. Methylation provided evidence ofthe range of fatty acids present together with the presence of ω-(o-alkylphenyl)alkanoic
acids. Trimethylsilylation enabled a wider range of compound classes to be detected
especially those containing free –OH groups.
The presence of long-chain n-alkenoic acids, dihydroxyalkanoic acids (especially thedominance of the precursor molecule cetoleic acid over other C22 : 1 isomers) and phytanicacid suggests that at least some of the pottery vessels were used for the processing ofaquatic tissues. The absence of ω-(o-alkylphenyl)alkanoic acids tends to suggest thateither they are below the limits of detection (although C18 acids were found in the
methylated extracts of the charred remains) or the temperatures in the vessels were nothigh enough to allow for their formation. Based on a series of experiments, Evershed etal. (2008) conclude that ω-(o-alkylphenyl)alkanoic acids form when n-alkenoic acids are
Table 8. Differences in molecular composition between the absorbed pottery residues and ‘charredremains’
Pottery residues

Charred remains

Low C16 : 0/C18 : 0 ratios
C16 : 1–C26 : 1
Isoprenoid acid (phytanic acid)
Dihydroxyalkanoic acidsnd
Cholesterol dominates over trace of plant sterol

High C16 : 0/C18 : 0 ratios
C18 : 1nd
nd
C18 ω-(o-alkylphenyl)alkanoic acids
Plant sterol (sitosterol) in all samples;cholesterol absent
Levoglucosan and other sugarsndnd—not detected© Japanese Archaeological Association

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RESIDUE ANALYSIS OF JOMON POTTERY AND CHARRED REMAINS

subjected to prolonged heating above 270°C with a ceramic matrix. The charred remains
not directly associated with pottery may derive from basketry which no longer survives.
This serves as a reminder that food processing takes place in many ways and in manydifferent contexts than may be represented by surviving pottery vessels alone.
In conclusion, molecular and isotope investigations can be a powerful tool foradvancing our understanding of the foodways of prehistoric people. The results of ouranalyses indicate that organic residues do survive in association with pottery vessels andcharred remains excavated from Jomon sites. Lipids were recovered from the majorityof the samples, although the preservation varied: given that our samples were obtained
primarily from waterlogged middens, where the preservation is generally better thanin dry sites, preservation condition will be an important factor to be considered when
conducting this type of research in the future. The separation between the lipid extractsof pottery with marine or aquatic signature, and those of the charred remains withindications of plant origins is particularly worth noting. The evidence may point tospecialised culinary practices involving distinct cooking technologies. It is particularlyinteresting that pottery seems to be largely dedicated for processing aquatic foods, as
observed in other Jomon contexts (Craig et al., 2013; Lucquin et al. 2016; Horiuchi etal. 2015), whilst other aceramic technologies were presumably used to cook plant foods.
Since our sample size is still too small to infer temporal and spatial variability, further
analysis is needed to understand changes through time in Jomon foodways as well as
variability between sites or locations.

Acknowledgements
This study is part of the ‘Long-term Sustainability through Place-Based, Small-Scale
Economies: Approaches from Historical Ecology’ Project (R-09) at the Research Institutefor Humanity and Nature in Kyoto, Japan. Support is also obtained from the Arts andHumanities Research Council (AH/L00691X/1) ‘The innovation and development of pottery
in East Asia.’ Samples were provided by the Preservation Ofﬁce of the Sannai Maruyama
Site (Sannai Maruyama Iseki Hozon Katsuyo Suishinshitsu) and the Archaeological Centerof Aomori Prefecture to the Berkeley Sannai Maruyama and Goshizawa Matsumori
Project, which was funded by the Henry Luce Foundation and the Center for JapaneseStudies of the University of California, Berkeley. The presence of charred crusts was ﬁrst
noted by Mikako Koshika and Mayumi Wakayama, who worked at the Preservation Ofﬁceof the Sannai Maruyama Site. Fumio Shiratori helped us retrieve potsherd samples from
Sannai Maruyama No. 9. Drawings of ‘charred remains’ in Figure 4 were produced by
Tomokazu Onishi. To these institutions and individuals, we express our gratitude. Carl
Heron wishes to thank the Alexander von Humboldt Stiftung for a Research Award during© Japanese Archaeological Association

49

Carl HERON et al.

2014–15 and the Wellcome Trust for an Engaging Science award to the British Museumin 2016. We also wish to thank Peter Chamberlain, Andy Gledhill and Val Steele for help
with the analysis.

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