Jacques Connan

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Annexe sur CD-ROM

Connan Jacques. Annexe sur CD-ROM. In: Le tell d'Akkaz au Koweït / Tell Akkaz in Kuwait Lyon ... more

La fluorescence spectrale et la géochimie organique moléculaire . Deux voies nouvelles pour évaluer la maturité de la matière organique de sédiments à Tasmanacées

Geochemical analysis of bituminous samples from the Pre-Pottery Neolithic B site of Nahal Efe (Northern Negev, Israel): Earliest evidence in the region and an example of alteration of the Dead Sea bitumen

by Jacob Vardi and Jacques Connan

Organic Geochemistry, 2024

Thirty-six bituminous samples from the Pre-Pottery Neolithic site of Nahal Efe (8000–7700 cal. BC... more Thirty-six bituminous samples from the Pre-Pottery Neolithic site of Nahal Efe (8000–7700 cal. BCE, Negev, Israel) were analysed to determine their origins. Most samples are mixtures of bitumen with minerals, predominantly quartz, calcite, dolomite and aragonite. The aragonite is from marine shells, which were crushed to be incorporated into the mixtures. Dead Sea bitumen was identified in all samples. The Nahal Efe geochemical data were compared to samplesfrom Tell Yarmuth (2800–1100 BCE), Tall Dhiban (700–800 cal. BCE), Tel Gezer (1250–700 cal. BCE) and to floating asphalt blocks from the Dead Sea. The stable carbon isotope values of resins and asphaltenes of the Nahal Efe bitumens differ from those of the Dead Sea floating blocks, Tell Yarmuth, Tel Gezer and Tall Dhiban, apparently a consequence of diagenesis. Thus, δ13C values of asphaltenes may not always be a reliable representative of the stable carbon isotope composition of the unaltered source bitumen. Surprisingly, the sterane and terpane patterns of the Nahal Efe samples are not severely biodegraded and clearly indicate a Dead Sea bitumen
source. No difference was recorded between mixtures and pure bitumen. Some changes have, however, been observed when using quantitative data on biomarkers. The shifts in δ13C values of resins and asphaltenes is not related to biodegradation but rather to oxidation of the Nahal Efe samples. This is the earliest and most complete evidence of Dead Sea bitumen exploitation and use, which included the preparation of different ‘recipes’, in the Negev and Sinai arid regions

format_quoteEarliest evidence of Dead Sea bitumen use at Nahal Efe includes multiple 'recipes' for mixtures, not due to biodegradation but oxidation.format_quote

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by Jacques Connan, Ferran Id, Steven Ortiz, and Alex Zumberge

Organic Geochemistry, 2024

Thirty-six bituminous samples from the Pre-Pottery Neolithic site of Nahal Efe (8000-7700 cal. BC... more Thirty-six bituminous samples from the Pre-Pottery Neolithic site of Nahal Efe (8000-7700 cal. BCE, Negev, Israel) were analysed by geochemical techniques. Dead Sea bitumen was identified in all samples. This is the earliest and most complete evidence of Dead Sea bitumen exploitation and use, which included the preparation of different ‘recipes’, in the Negev and Sinai arid regions.
The Nahal Efe geochemical data was compared to samples from Tell Yarmuth (2800-1100 BCE), Tall Dhiban (700-800 cal. BCE), Tel Gezer (1250-700 cal. BCE, unpublished) and to floating asphalt blocks from the Dead Sea.
The stable carbon isotope values of resins and asphaltenes of the Nahal Efe bitumens differ from those of the Dead Sea floating blocks, Tell Yarmuth, Tel Gezer and Tall Dhiban, apparently a consequence of diagenesis. Thus, 13C values of asphaltenes may not always be a reliable representative of the stable carbon isotope composition of the unaltered source bitumen.
Surprisingly, the sterane and terpane patterns of the Nahal Efe samples are not severely biodegraded and clearly indicate a Dead Sea bitumen source. No difference was recorded between mixtures and pure bitumen. Some changes have, however, been observed when using quantitative data on biomarkers. The shifts in 13C values of resins and asphaltenes is not related to biodegradation but rather to oxidation of the Nahal Efe samples.
Mixtures of bitumen with minerals constitute most of the samples set. Dominant minerals are quartz, calcite, dolomite and aragonite. Aragonite comes from marine shells, which were crushed to be incorporated into the mixtures.

$Fig. 1. Location of Nahal Efe and other southern Levantine prehistoric sites mentioned in the text. SE Os bia Evidence from late prehistoric sites (Bronze Age and Iron Age) is even more abundant and varied (Connan et al., 1992). The study of these assemblages, including most analyses on the isotopic and chemical changes that have affected the Dead Sea bitumen, are available for: Tell Yarmuth (3000-1100 cal. BCE, Connan et al., 2022), Tall Dhiban (ca. 750 cal. BCE, Connan et al., 2022), Tel Miqne-Ekron (ca. 600 cal. BCE, This paper presents the results of the study of the bituminous remains from Nahal Efe, which is the largest Middle PPNB site in the Negev and Sinai deserts (Fig. 1). The mere presence of bituminous remains at Nahal Efe is doubly interesting. Firstly, because no bitumen remains had pre- viously been reported in the Negev and Sinai region during the Pre- Pottery Neolithic. Secondly, the studied set comprises what a priori looked like both pure chunks and mixtures of bitumen with mineral matter, and thus might include samples that have a longer history and were more affected by alteration processes. The samples are, therefore, of particular interest to assess the possibility for isotopic and molecular changes of the chemical fractions of Dead Sea bitumen from this older occupation site. In addition to the samples from Nahal Efe, the present study includes five archaeological pure bitumen samples from the much later site of Tel Gezer (1250-700 cal. BCE) that, together with present day Dead Sea bitumen (1980 AD), have been used for comparative purposes as unaltered references.$

$Fig. 8. Mass fragmentograms of steranes (m/z 217) and terpanes (m/z 191) of two samples of Nahal Efe: pure bitumen (N°3502) and a mixture bitumen + minerals (N°3521). C29aBH = norhopane, C30apH = 17a,21B-hopane, C3lafHR = 17a,21$,22R-30-homohopane, C27oBPR + S = 5a,146,17B-20R + 20S-cholestane, C28aPpR + S = 5a,14B,17B-20R + 20S-24methylcholestane, C29aPBR + S = 5a,148,17B-20R + 20S-24ethylcholestane, C29aaa20S = 5a,140,170-20S-24ethyl- cholestane, Ts = 18a-22,29,30-trisnorneohopane, Tm = 17a-22,29,30-trisnorhopane, C34aBHS = C34-170,21fB-22S-extended hopane. Mass fragmentograms of steranes (m/z 217) and terpanes (m/z 191) of two samples of Nahal Efe, a chunk of pure bitumen (N° 3502) and a mixture (N°3521), are shown in Fig. 8. They were compared to two pure bitumens (Fig. 9): the floating blocks of Dead Sea bitumen (N°1937, Connan et al., 1992) and one sample of Tel Gezer (N° 3384). Unlike the differences in carbon isotope values of chromatographic fractions, steranes and terpanes of Nahal Efe samples were all comparable to the pure Dead Sea bitumen and not severely biodegraded. Mass fragmen- tograms of terpanes (m/z 191, Fig. 8) and steranes (m/z 217, Fig. 8) display the typical patterns of Dead Sea bitumen (Fig. 9): abundant quantities of tricyclic terpanes (C19/3 to C29/3), high Tm/Ts (17a- 22,29,30-trisnorhopane /18a-22,29,30-trisnorneohopane) ratio, high amount of gammacerane, C21Ste and C22Ste, low C27diasteranes, C27 > Cog > Cog steranes. At first glance, steranes and terpanes seem to be rather well preserved but some changes are observable. For instance, the amount of tricyclic terpanes and of C21-C2 steranes is reduced in Nahal Efe samples. By referring to quantitative data (Supplementary Table 5) and the plots of some parameters, for instance Ts/Tm vs. 5/3Casp (%0/VPDB, Fig. 10) and Diasteranes/Regular Steranes vs. Steranes/Ter- panes (Supplementary Fig. 3), biodegradation is detected to a limited extent. Ts/Tm and Diasteranes/Regular steranes increase in Nahal Efe either in pure bitumens or mixtures due to the selective biodegradation of Tm over Ts and to regular steranes over diasteranes (Bost et al., 2001; Connan et al., 2024). Samples of Tel Gezer are less affected and match the Dead Sea floating blocks and the pure bitumen of Tell Yarmuth. Biodegradation effects are also detected when considering the aBp-steranes composition in a ternary diagram %C27aPpPR&S steranes vs. A plot of SDasp and 5DNSO vs. 8'8Casp and 5!3Cresin in Supple- mentary Fig. 2 shows enrichments in 7H in Yarmuth and Nahal Efe$

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Geochemical study of the luting and coating of medieval watercraft from the ship timbers discovered in the citadel of al-Balīd, Oman: Composition and origin

Journal of Archaeological Science: Reports

Ship timbers were discovered during the excavation of the Islamic site of al-Balīd recycled in th... more Ship timbers were discovered during the excavation of the Islamic site of al-Balīd recycled in the buildings of its citadel and the Great Mosque. These fragments stripped from the hulls of Indian Ocean medieval sewn vessels form the largest collection of archaeological evidence for the ships sailing during the Middle Islamic Period (10th–15th century CE). More than one third of the timbers bears traces of a bitumen mixture used as luting and coating to seal the ships planking to waterproof and protect their hulls, a practice generally associated with sewn-plank construction. This paper presents the result of the GC-MS, carbon and hydrogen isotope on chromatographic fractions, and X-Ray diffraction analyses on twenty-two samples of the luting extracted from fifteen timbers from al-Balīd. The nature of the constituents of the amalgam is determined showing that the luting consists of bitumen mixed with mineral matter, fat or oil and two triterpenic resins, dammar (Dipterocarpacea) and frankincense. The chemical signature of the bitumen indicates that it was likely sourced from two seeps in southwest Iranian: Mamatain and Ain Gir-Chersch Mehrgir-Dehluran. The origin of the bitumen might suggest that the luting was applied during the construction or repairing of Indian Ocean vessels in boatyards along the coasts of the Arabian/Persian Gulf or Southern and Eastern Arabia.

L'atelier de potiers de la période romaine des "Quatre Bornes" aux Rues-des-Vignes (Nord)

HAL (Le Centre pour la Communication Scientifique Directe), 2022

Molecular data: clues to trace the origin of archaeological organic materials

Annales d'Université "Valahia" Târgovişte. Section d'Archéologie et d'Histoire, 2011

Molecular studies of archaeological remains using a fractionation scheme of organic extracts and ... more Molecular studies of archaeological remains using a fractionation scheme of organic extracts and mass spectrometric techniques (GC-MS) allow identification of specific biomarkers. Such components are likely to provide information about the type of organic substances present and, more extensively on their history. In this paper, special emphasis has been put on the necessity for precise structural identification to distinguish beeswax and cuticular waxes. The results of the analysis of two unknown residues are also reported : the content of a pilgrim flask (Egypt, XXVI th dynasty, 664-525 BC) and the wall coating of Middle Age undergrounds (Corrèze, France).

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L’analyse du bitume des éléments de faucilles en silex d’Ougarit (Bâtiment B du chantier “Grand-rue”)

Un ensemble exceptionnel d’outils provenant d’un atelier de travail du silex a ete decouvert sur ... more Un ensemble exceptionnel d’outils provenant d’un atelier de travail du silex a ete decouvert sur le site de Ras Shamra (Syrie). Les silex mis a jour ont ete plus particulierement utilises pour la fabrication ou la reparation de faucilles. Une etude a ete realisee afin de determiner la nature et l’origine du materiau organique retrouve a la surface de certains silex et vraisemblablement employe comme adhesif pour fixer les silex sur des manches de faucilles. L’analyse par chromatographie en phase gazeuse couplee a la spectrometrie de masse des hydrocarbures satures de ces echantillons montre qu’ils sont principalement constitues de bitume severement altere. L’analogie de la composition isotopique du carbone ainsi que des profils moleculaires de ces bitumes avec ceux d’asphaltes naturels provenant du gisement de Kfarie, situe a proximite du site de Ras Shamra, a permis d’etablir que ce gisement etait a l’origine des echantillons de bitumes etudies. Ces profils moleculaires sont caract...

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Characterization of organic matter of several Recent sediments

Preservation, Degradation, and Destruction of Trapped Oil

Petroleum is a fragile fluid, a part of which is likely to be destroyed or lost to the atmosphere... more Petroleum is a fragile fluid, a part of which is likely to be destroyed or lost to the atmosphere. The moment crude oil separates from bitumen in the source rock, it begins to undergo compositional changes that continue throughout migration and accumulation. The processes and factors influencing oil composition in an accumulation take effect before, during, and after entrapment. The primary factors influencing oil composition before entrapment are source rock characteristics, primary migration, and secondary migration. The main factors influencing oil composition during entrapment are pressure and temperature, as they establish the conditions under which secondary alteration processes take place. After entrapment, secondary alteration processes influencing oil composition are the effect of thermal maturation, physical and biological degradation, gravity segregation, dysmigration (separation-migration), and deasphalting. These alteration processes can increase the API gravity and gas-oil ratio of the oil, but generally decrease the API gravity. Knowledge of the conditions and mechanisms of degradation are needed to understand the nature and distribution of oil shows and to carry out oil-oil and oil-source rock correlations. Considerable progress has been made in understanding secondary alteration processes, but more is expected as the more poorly understood macromolecular and polar fractions are investigated. Presently, molecular chemistry is a useful tool that can recognize incipient biodegradation, detect oil gravity segregation, and discriminate a pyrobitumen from a precipitated asphaltene, whereas bulk analyses are currently inaccurate.

Geochemistry of Crude Oils and Crude-Oil-Source-Rock Correlations in Four Carbonate Basins

Petroleum Geochemistry and Source Rock Potential of Carbonate Rocks, 1984

Crude oils and rock samples from carbonate basins in France (Aquitaine), Guatemala, Iraq, and Tun... more Crude oils and rock samples from carbonate basins in France (Aquitaine), Guatemala, Iraq, and Tunisia/Libya were analyzed by the usual methods of organic geochemistry. The studies were based mainly on computerized gas chromatography-mass spectrometry, with special emphasis on mass fragmentography. Several classes of biological markers were used for the purpose of characterizing the environments of deposition and for correlating crude oils with source rocks. The following specific features commonly were observed in the oil and rock samples from these carbonate formations: (1) the predominance of normal alkanes with even carbon numbers, usually more pronounced in the rocks than in the oils; (2) a ratio of pristane to phytane mostly below 1; (3) the presence in significant concentrations of the higher homologs of the hopane triterpanes, up to C 35 (more important in rocks than in oils); (4) usually small amounts of steranes (C^-C^ and C 27-C 29 ranges), with predominance of non-rearranged structures; and (5) commonly an unusually high concentration of individual isoalkanes (Qj) and cyclohexylalkanes (C 21). These molecular criteria partly reflect an important microbial contribution, which is usually more pronounced in highly anoxic environments. Furthermore, they have been used successfully in correlations among crude oils and between crude oils and their source rocks. The results agree with other geochemical and geological data.

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Organic geochemistry of hydrocarbon seeps associated with sulfurous spring water, western Iraq: Biodegradation, source rock and sedimentary environment

Journal of Petroleum Science and Engineering, 2022

Abstract Oil seep samples from Abu-Jir Fault Zone (AJFZ) were geochemically characterized to dete... more Abstract Oil seep samples from Abu-Jir Fault Zone (AJFZ) were geochemically characterized to determine the level of biodegradation and the depositional environment of correlative source rocks. For this purpose, saturated and aromatic biomarkers and stable carbon isotopes of thirteen samples were analyzed and measured. Saturated hydrocarbons of the AJFZ are low; whereas polar fractions are relatively high. Normal alkanes and isoprenoids of these oil seeps are totally removed; steranes are still intact in some samples, and slightly to heavily degraded in other samples; whereas hopanes are intact These criteria indicate that these samples are moderately to heavily biodegraded. low C24/C23, high C22/C21 tricyclic terpanes and C29/C30 hopane ratios suggest that these oil seeps were generated from carbonate source rocks. In addition, the high C35/C34 hopanes and homohopane index values suggest deposition under marine anoxic conditions. Low values of diasteranes/regular steranes, Ts/Tm, and moretane/hopane for most samples suggest early-mature source rocks. Sterane distributions and carbon isotopic composition of the AJFZ oil seep samples suggest they are not genetically related with the oils of the southern oilfields (Majnoon, Nasiriyah, West Qurna, North Rumaila, Luhais, Abu Gharab, Faka, Buzergan), nor consistent with the main source rocks (Sargelu and Naokelekan), but they are closely related to the East Baghdad oilfield and Chia Gara extracts. This study suggests the oil seeps were generated from Chia Gara Formation (upper Jurassic-lower Cretaceous).

Étude géochimique d'enduits de surface, de tissus de calfatage, de blocs de poix et de bitume des épaves gallo-romaines du Parc Saint-Georges de Lyon

Archaeonautica, 2010

CONNAN Jacques, Charrie-Duhaut Armelle. Étude géochimique d'enduits de surface, de tissus de ... more CONNAN Jacques, Charrie-Duhaut Armelle. Étude géochimique d'enduits de surface, de tissus de calfatage, de blocs de poix et de bitume des épaves gallo-romaines du Parc Saint-Georges de Lyon. In: Archaeonautica, 16, 2010. Les épaves de Saint-Georges – Lyon – Ier-XVIIIe siècles, sous la direction de Éric Rieth. pp. 147-172

The bitumen of Tell Brak from the Middle Uruk (c.3500 BC) to Late Bronze Age (c.1280 BC): origin and trade routes

Journal of Historical Archaeology & Anthropological Sciences, 2018

13 archaeological samples, dated from the Middle Uruk period (c.3500 BC) to the Late Bronze age (... more 13 archaeological samples, dated from the Middle Uruk period (c.3500 BC) to the Late Bronze age (c.1280 BC), were analyzed by geochemical techniques in order to identify bitumen and to attempt to find its origin. Extracts do show that the samples are characteristic archaeological bitumens. Bitumens of Tell Brak were compared to some other archaeological asphalts, to crude oils and natural asphalts. Utilization of carbon isotopes on asphaltenes and biomarkers namely steranes and terpanes allowed us to identify two main areas of bitumen supply, Hit on one side along the Euphrate river, northern Iraq on the other side.

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Chemical analyses of Egyptian mummification balms and organic residues from storage jars dated from the Old Kingdom to the Copto-Byzantine period

Journal of Archaeological Science, 2017

Twenty three samples of Egyptian organic materials, spanning from the Old Kingdom to the Copto-By... more Twenty three samples of Egyptian organic materials, spanning from the Old Kingdom to the Copto-Byzantine Period, were investigated by gas chromatography-mass spectrometry. The sample set was comprised of ten balm samples from human mummies, three balms from shrews, and ten samples of residues scraped from jars and amphora from storehouses. This research program was undertaken with two main goals: Firstly to provide complementary data on the mummification balms from both humans and animals with an emphasis on the occurrence of bitumen in mummification mixtures. Secondly to explore whether the jar residues were mixtures that were used for mummification purposes or whether they were pure ingredients stored for various uses including ritual practices. The analysis highlighted that the most abundant constituents of the mummification balms were: fats or oils, waxes, conifer resin, pitch, mastic resin, castor oil, and bitumen. Balms from animal mummies were not found to be significantly different from the balms from human mummies. Residues from potsherds appeared to belong to two categories: pure products (fats and castor oil) and mixtures containing fats, Pinaceae resin and pitch, mastic resin, and castor oil, i.e. the constituents also identified in mummification balms. The mixtures were thus residues of preparations for ritual practices and embalming. This study demonstrates that bitumen is underestimated by the chemical approach currently applied in most archaeometric studies of Egyptian organic residues, which are better suited for the identification of lipids and resinous materials. We thus applied a specific analytical design, targeted at bitumen. Bitumen from the Dead Sea was conclusively identified using as reference materials for comparison, i.e. the present day bitumen from the Dead Sea floating blocks, as well as several bitumens from mummification balms and bitumen lumps unearthed from the archaeological site of Tell Yarmouth near Jerusalem in Israel.

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Identification of alkyl guaiacyl dehydroabietates as novel markers of wood tar from Pinaceae in archaeological samples

Organic Geochemistry, 2016

Resinous materials from conifers from the Pinaceae family are frequently found in an archaeologic... more Resinous materials from conifers from the Pinaceae family are frequently found in an archaeological context. These materials were used, notably, as waterproofing agent, as adhesive, or for the caulking of boats. Two main types of materials can be distinguished: resin, the exsudate of conifer tree, and wood tar obtained by dry distillation of wood. Molecular investigations of such materials aim, notably, at developing new molecular tools for the determination of their biological and geographical origin or of the manufacturing techniques, and for the discrimination between resin and wood tar. In this context, we report here the identification by synthesis of alkyl guaiacyl dehydroabietates, which occur in a series of recent and archaeological conifer wood tar samples from shipwrecks and Gallo-Roman tar preparation sites. They most likely result from the reaction of dehydroabietic acid and alkyl guaiacols, the latter being typical wood pyrolysis products formed during the preparation of wood tar. Alkyl guaiacyl dehydroabietates are therefore proposed to be specific molecular markers for conifer wood tar, allowing a clear molecular distinction between this material and resin to be made. They are also more resistant to the alteration undergone by archaeological samples than other compounds previously proposed as markers of conifer wood tar such as anhydrosugars or alkyl guaiacols.

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In vitro biodegradation of steranes

ABSTRACT

Laboratory Simulation and Natural Diagenesis. 1. Thermal Evolution of Asphalts from the Aquitaine Basin (SW France)

Kerogen maturity and gas/oil properties in shale/sand stone sequences

Abstract The present study deals mainly with shale sandstone series in which the disseminated ker... more Abstract The present study deals mainly with shale sandstone series in which the disseminated kerogen is mostly composed of land-derived debris. The organic matter characterization was performed by means of microscopic and chemical techniques. The kerogen maturity was assessed by microscopic studies, mainly using vitrinite reflectance measurements. Chemical properties of shale kerogens, as well as of oil – and gas – shows, were examined in several sedimentary basins in different parts of the world. Oil and gas properties were tentatively interpreted in terms of maturity. For this purpose, oils properties were compared to the kerogen characteristics of shales interbedded with the impregnated sandstone reservoirs. This synthesis is documented in several case histories form New Zealand, Colombia, Australia, Indonesia, In low maturation stages (immature zone), dry gas with minor condensate is observed, whereas in higher maturity levels (oil window), wet gas with high paraffinic crudes are generally recorded. Pristane to n-C17 ratios permit differentiation between immature (> 1.0) and mature (> 1.0) condensates i.e. intensively cracked crude oils. i-C4 to n-C4 ratios enable an adequate discrimination between gases produced with immature condensate (i-C4/n-C4 > 0.80) and those produced with high wax crudes or mature condensates (i-C4/n C4 > 0.80). Shallow depth condensates and their related gases have also been identified as immature fluids. Properties of some mature condensates are given as references. This study should provide a maturity framework as a guide for oil – and gas – show prediction in shale-sandstone sequences containing landderived kerogen.

Technical report on the comparative , compositional and isotopic analysis of the H3bitumen

Chemical analysis of reed- boat remains form the Ubaid period

Jacques Connan

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