A review of analytical methods for assessing preservation in waterlogged archaeological wood and their application in practice

Waterlogged archaeological wood can present management challenges due to its vulnerability to chemical and biological decay, both during burial and post-excavation. Decay processes also often leave it severely weakened and therefore susceptible to mechanical damage. Quantifying preservation and understanding active decay mechanisms is therefore critical in informing the management of this unique cultural resource. It is critical that assessments of preservation are robust, and sensitive enough to allow changes over time to be detected. A wide range of analytical methods can be applied to assess the state of preservation of waterlogged archaeological wood, and determining which of these is most appropriate to the circumstances can be challenging. This review summarises some of the most commonly reported methods suitable for the analysis of waterlogged archaeological wood, ranging from widely used ‘low-tech’ methods, to assessment using advanced analytical instrumentation. Methods are evaluated in terms of the information gained weighed up against their cost, logistical considerations, and time investments, with the aim of supporting the development of an analytical strategy. We conclude that although an analytical strategy must be informed by the aims of assessment as well as any external restrictions, the best available analytical techniques should be employed in order to supply an accurate baseline against which future change can be measured. Critically, a multi-analytical approach is vital in obtaining a clear picture of the present state of decay, as no single technique gives the best assessment

Correction to : A review of analytical methods for assessing preservation in waterlogged archaeological wood and their application in practice (Heritage Science, (2020), 8, 1, (83), 10.1186/s40494-020-00422-y)

Following publication of the original article [1], it was reported that the caption for Fig. 4a erroneously stated that it showed soft rot decay. In fact, the image shows decay by erosion bacteria. The caption for Fig. 4a has been amended and the original article has been updated

Molecular fossils as a tool for tracking Holocene sea-level change in the Loch of Stenness, Orkney

Sediments deposited in the Loch of Stenness (Orkney Islands, Scotland) during the Holocene transgression, previously dated to between ~5939–5612 bp, were analysed for molecular fossils – lipids and chlorophyll pigments from primary producers – that complement conventional microfossil and lithological approaches for studying past sea-level change. While microfossil and lithological studies identified a transgression between 102 and 81 cm core depth, key molecular fossils fluctuate in occurrence and concentration between 118 and 85 cm, suggesting an earlier start to the transgression. Terrestrial lipid concentrations decreased and algal-derived, short-chain, n-alkanoic acid concentrations increased at 118 cm, indicating a disruption of the freshwater lake conditions associated with the early stages of the marine transgression. The lipid and pigment analyses provided information that complements and extends that from microfossil analysis, presenting a more complete record of Holocene sea-level changes and local vegetation changes in the Loch of Stenness. The isostatic stability of Stenness during the Holocene points towards other factors to explain the transgression, such as regional factors and/or melting of the Antarctic ice sheet (which occurred up to 3 ka)

An aminostratigraphy for the British Quaternary based on Bithynia opercula

Aminostratigraphies of Quaternary non-marine deposits in Europe have been previously based on the racemization of a single amino acid in aragonitic shells from land and freshwater molluscs. The value of analysing multiple amino acids from the opercula of the freshwater gastropod Bithynia, which are composed of calcite, has been demonstrated. The protocol used for the isolation of intra-crystalline proteins from shells has been applied to these calcitic opercula, which have been shown to more closely approximate a closed system for indigenous protein residues. Original amino acids are even preserved in bithyniid opercula from the Eocene, showing persistence of indigenous organics for over 30 million years. Geochronological data from opercula are superior to those from shells in two respects: first, in showing less natural variability, and second, in the far better preservation of the intra-crystalline proteins, possibly resulting from the greater stability of calcite. These features allow greater temporal resolution and an extension of the dating range beyond the early Middle Pleistocene. Here we provide full details of the analyses for 480 samples from 100 horizons (75 sites), ranging from Late Pliocene to modern. These show that the dating technique is applicable to the entire Quaternary. Data are provided from all the stratotypes from British stages to have yielded opercula, which are shown to be clearly separable using this revised method. Further checks on the data are provided by reference to other type-sites for different stages (including some not formally defined). Additional tests are provided by sites with independent geochronology, or which can be associated with a terrace stratigraphy or biostratigraphy. This new aminostratigraphy for the non-marine Quaternary deposits of southern Britain provides a framework for understanding the regional geological and archaeological record. Comparison with reference to sites yielding independent geochronology, in combination with other lines of evidence, allows tentative correlation with the marine oxygen isotope record

Early Ipswichian (last interglacial) sea level rise in the channel region : Stone Point Site of Special Scientific Interest, Hampshire, England

Constraining the speed of sea level rise at the start of an interglacial is important to understanding the size of the ‘window of opportunity’ available for hominin migration. This is particularly important during the last interglacial when there is no evidence for significant hominin occupation anywhere in Britain. There are very few finer grained fossiliferous sequences in the Channel region that can be used to constrain sea level rise and they are preserved only to the north of the Channel, in England. Of these, the sequence at Stone Point SSSI is by far the most complete. Data from this sequence has been previously reported, and discussed at a Quaternary Research Association Field Meeting, where a number of further questions were raised that necessitated further data generation. In this paper, we report new data from this sequence – thin section analysis, isotopic determinations on ostracod shells, new Optical Stimulated Luminescence ages and Amino Acid Recem analyses. These show early sea level rise in this sequence, starting during the pre-temperate vegetation zone IpI, but no early warming. The implications of this almost certainly last interglacial sequence for the human colonisation of Britain and our understanding of the stratigraphic relationship of interglacial estuarine deposits with their related fluvial terrace sequences is explored

Early Ipswichian (last interglacial) sea level rise in the channel region : Stone Point Site of Special Scientific Interest, Hampshire, England

Constraining the speed of sea level rise at the start of an interglacial is important to understanding the size of the ‘window of opportunity’ available for hominin migration. This is particularly important during the last interglacial when there is no evidence for significant hominin occupation anywhere in Britain. There are very few finer grained fossiliferous sequences in the Channel region that can be used to constrain sea level rise and they are preserved only to the north of the Channel, in England. Of these, the sequence at Stone Point SSSI is by far the most complete. Data from this sequence has been previously reported, and discussed at a Quaternary Research Association Field Meeting, where a number of further questions were raised that necessitated further data generation. In this paper, we report new data from this sequence – thin section analysis, isotopic determinations on ostracod shells, new Optical Stimulated Luminescence ages and Amino Acid Recem analyses. These show early sea level rise in this sequence, starting during the pre-temperate vegetation zone IpI, but no early warming. The implications of this almost certainly last interglacial sequence for the human colonisation of Britain and our understanding of the stratigraphic relationship of interglacial estuarine deposits with their related fluvial terrace sequences is explored

A new method for enamel amino acid racemization dating : A closed system approach

Analysis: of the predictable breakdown of proteins and amino acids in ancient biominerals enables age estimation over the Quaternary. We postulate that enamel is a suitable biomineral for the long-term survival of endogenous amino acids. Analysis of multiple amino acids for geochronological studies is typically achieved using a RP-HPLC method. However, the low concentrations of amino acids coupled with high concentrations of inorganic species make accurate determination of amino concentrations challenging. We have developed a method for the routine preparation of multiple enamel samples using biphasic separation. Furthermore, we have shown that amino acids that exhibit effectively closed system behaviour can be isolated from enamel through an exposure time of 72 h to bleach. Elevated temperature experiments investigating the processes of intra-crystalline protein degradation (IcPD) do not appear to match the patterns from fossil samples, reinforcing the need for a comprehensive understanding of the underlying mechanisms of protein degradation. This novel preparative method isolates intra-crystalline amino acids suitable for the development of mammalian geochronologies based on enamel protein degradation. The lower rates of racemization in enamel (cf. Bithynia opercula) suggest that the enamel AAR may be able to be used as a relative dating technique over time scales >2.8 Ma. Enamel AAR has the potential to directly date mammalian remains past the limit of all other current direct dating methods, providing an invaluable tool for geochronological studies

Assessing the intra-crystalline approach to amino acid geochronology of Neogloboquadrina pachyderma (sinistral)

While amino acid (AA) geochronology has been widely applied to foraminiferal biomineral proteins, there has been limited assessment of the potential of isolating an ‘intra-crystalline’ fraction of proteins to improve the reliability of AA geochronology for foraminifera. In this study, bleaching experiments were carried out on the foraminifer Neogloboquadrina pachyderma (sinistral) from an independently dated core from the south eastern Norwegian Sea spanning the last 120 ka. Results show that this species contains a bleach-resistant fraction of biomineral proteins, and that this intra-crystalline fraction may behave as a closed system. Racemisation in both the intra-crystalline and whole-protein fractions was found to systematically increase with time. Isoleucine epimerisation showed reliable trends with depth when analysed by ion exchange chromatography (IEC); analysis by reverse-phase liquid chromatography (RP-HPLC) resulted in reliable age-D/L relationships for aspartic acid, glutamic acid and alanine. Isolating the intra-crystalline fraction with a 48 h bleach treatment reduced the influence of contamination in younger material. Therefore, this paper recommends that the intra-crystalline approach is used when analysing Neogloboquadrina pachyderma (sinistral) for AA geochronology, especially for younger samples. Material-specific regression equations developed in this study successfully convert IEC A/I to RP-HPLC D/L values for aspartic acid, glutamic acid and alanine, enabling integration of geochronologies developed using different methods for this class of biomineral