The Upper Jurassic–Lower Cretaceous of eastern Heilongjiang, northeast China: stratigraphy and regional basin history

In eastern Heilongjiang, the Upper Jurassic is marine and restricted to the Suibin and Dong’an areas, where it is characterized faunally by Callovian–Volgian (Tithonian) bivalves and florally by dinoflagellates. The Lower Cretaceous is widely distributed in eastern Heilongjiang, and characterized faunally by Berriasian–Valanginian bivalves, Barremian–Albian ammonites and Aucellina, and florally by dinoflagellates. To the west, the marine facies grade into non-marine beds. Thus, in the east, for example in the Dong’an and Dajiashan areas, near the northwestern Palaeo-Pacific, the Lower Cretaceous is marine; westward, in the Yunshan, Longzhaogou, Peide, and Zhushan areas, marine and non-marine deposits alternate, whereas further west still, e.g. in the Jixi Basin, non-marine facies are intercalated with marine beds. This regional distribution is indicative of a large, shallow embayment opening eastwards to the Palaeo-Pacific; during the Early Cretaceous successive transgressive-regressive events influenced the climate and biota of eastern Heilongjiang and northeastern China. Many of the Lower Cretaceous sections contain abundant coals, demonstrating that in this region the Early Cretaceous was an important coal-forming period. Some non-marine bivalve species are common to the Lower Cretaceous Jixi Group of eastern Heilongjiang, the Jehol Group of western Liaoning and the Transbaikalian Group of Siberia, suggesting that these groups are of comparable Early Cretaceous age.     

Chemical oceanographic influences on sediment accumulations of a carbonate ramp: Holocene Yucatan Shelf,Mexico

Global controls on the oceanographic influences on the nature of carbonate factories are broadly understood. The details of the influences of changes in temperature and nutrients across individual carbonate shelves are less well constrained, however. This study explores spatial and temporal variations in chemical oceanography along and across the Yucatan Shelf, a modern carbonate ramp, and how these factors relate to variable bottom character, sediment and sediment geochemistry. In‐situ sensors and remote‐sensing data indicate the sporadic presence of cool, upwelled water with low dissolved oxygen and elevated Chlorophyll‐a. This current‐driven, westward flow of upwelled water is most evident in a zone just offshore of the northern peninsular shoreline, but its influence wanes ca 75 km offshore and as the shore turns southward. The impacts of this water mass include a transitional photozoan–heterozoan assemblage with biosiliceous components, relict grains and common thin Holocene sediment accumulations nearshore; further offshore are coralgal reefs and expansive sand plains. Geochemical proxies of bulk sediment, including high δ¹⁸O and elevated HREE/LREE (heavy rare‐earth element/light rare‐earth element) ratios near, and downcurrent of, the upwelling source, are interpreted to represent the signal of nearshore, westward movement of the cool and nutrient‐rich, upwelled water. Collectively, these data emphasize how local processes such as upwelling and longshore transport can variably influence carbonate sediment accumulations and their geochemical signatures, both along and across individual shelves. These data and insights provide an analogue for the influences of spatial variability of water masses in the geological record, and for accurate interpretation of stratigraphic changes of sedimentary and geochemical proxy data in carbonate archives.     

Rare earth and other trace element mobility during mylonitization: a comparison of the Brevard and Hope Valley shear zones in the Appalachian Mountains, USA

In progressing from a granitoid mylonite to an ultramylonite in the Brevard shear zone in North Carolina, Ca and LOI (H₂O) increase, Si, Mg, K, Na, Ba, Sr, Ta, Cs and Th decrease, while changes in Al, Ti, Fe, P, Sc, Rb, REE, Hf, Cr and U are relatively small. A volume loss of 44% is calculated for the Brevard ultramylonite relative to an Al–Ti–Fe isocon. The increase in Ca and LOI is related to a large increase in retrograde epidote and muscovite in the ultramylonite, the decreases in K, Na, Si, Ba and Sr reflect the destruction of feldspars, and the decrease in Mg is related to the destruction of biotite during mylonitization. In an amphibolite facies fault zone separating grey and pink granitic gneisses in the Hope Valley shear zone in New England, compositional similarity suggests the ultramylonite is composed chiefly of the pink gneisses. Utilizing an Al–Ti–Fe isocon for the pink gneisses, Sc, Cr, Hf, Ta, U, Th and M-HREE are relatively unchanged, Si, LOI, K, Mg, Rb, Cs and Ba are enriched, and Ca, Na, P, Sr and LREE are lost during deformation. In contrast to the Brevard mylonite, the Hope Valley mylonite appears to have increased in volume by about 70%, chiefly in response to an introduction of quartz. Chondrite-normalized REE patterns of granitoids from both shear zones are LREE-enriched and have prominent negative Eu anomalies. Although REE increase in abundance in the Brevard ultramylonites (reflecting the volume loss), the shape of the REE pattern remains unchanged. In contrast, REE and especially LREE decrease in abundance with increasing deformation of the Hope Valley gneisses. Mass balance calculations indicate that ≥95% of the REE in the Brevard rocks reside in titanite. In contrast, in the Hope Valley rocks only 15–40% of the REE can be accounted for collectively by titanite, apatite and zircon. Possible sites for the remaining REE are allanite, fluorite or grain boundaries. Loss of LREE from the pink gneisses during deformation may have resulted from decreases in allanite and perhaps apatite or by leaching ofy REE from grain boundaries by fluids moving through the shear zone. Among the element ratios most resistant to change during mylonitization in the Brevard shear zone are La/Yb, Eu/Eu*, Sm/Nd, La/Sc, Th/Sc, Th/Yb, Cr/Th, Th/U and Hf/Ta, whereas the most stable ratios in the Hope Valley shear zone are K/Rb, Rb/Cs, Th/U, Eu/Eu*, Th/Sc, Th/Yb, Sm/Nd, Th/Ta, Hf/Ta and Hf/Yb. However, until more trace element data are available from other shear zones, these ratios should not be used alone to identify protoliths of deformed rocks.     

Multiproxy approach to understanding the origin of Cretaceous pelagic limestone–marl alternations (DSDP site 391, Blake-Bahama Basin)

Limestone–marl alternations are usually directly interpreted to reflect cyclic palaeoenvironmental signals. However, uncertainty in such interpretations stems from the differential diagenesis that most limestone–marl alternations have undergone. Differential diagenesis results in markedly different alterations between limestones and marls and in the loss of comparability of many measurable parameters. For an unequivocal interpretation of the origin of rhythmic alternations, diagenetically robust parameters or parameters that clearly indicate the degree of diagenetic bias are required. The present study uses a multiproxy approach (independent biotic, sedimentary and geochemical parameters) in order to unravel the palaeoenvironmental signal recorded in Valanginian (Early Cretaceous) limestone–marl alternations from the Blake‐Bahama Basin (DSDP site 391). Using this approach, terrestrial and marine influences can be distinguished, changes in nutrient levels estimated and prediagenetic differences in the non‐carbonate fraction constrained. Surprisingly, no systematic variations in any of these parameters were observed between limestone and marl layers, implying that none of these was directly responsible for the formation of the rhythmic alternation. Hence, none of the current models of sedimentary formation of limestone–marl rhythmites is applicable here. Calcareous nannofossils are equally well preserved in limestone and marl layers, ruling out their dissolution in marl layers as a source of the calcite cement in the limestone beds. Sr values of 700–900 p.p.m. indicate that aragonite may have been present in the original, pelagic sediment. The assumption of fine‐grained sedimentary aragonite imported from nearby carbonate platforms as the source of the cement would explain a number of otherwise enigmatic features in these rhythmites, including the source of the calcite cement observed in the limestones, the equally good preservation of calcareous nannofossils in limestones and marls and the higher concentration of calcareous nannofossils in marl layers. The study demonstrates that examination of diagenetically inert parameters or parameters in which diagenetic effects can be filtered can yield unexpected results. Clearly, careful analysis of such parameters needs to be undertaken in order to make reliable palaeoenvironmental interpretations from rhythmite successions.     

Petrographical and geochemical characterization of Comblanchien limestone (Bourgogne,France): A fingerprint of the building stone provenance

The Comblanchien limestone is a well-known building stone that deserves a quantitative characterization in order to be able to certify its origin. We compare petrographical and geochemical characteristics of limestones commercialized under the name of Comblanchien to those of one of their competitors (VATC, a Portuguese coated grain-bearing limestone). From macroscopic and microscopic observations, the distinction is somehow difficult but the coated grain-bearing Comblanchien samples have δ¹³C values (from +1.75 to +2.25‰) different from those of the VATC sample (negative δ¹³C value). As an example of application of these results, three samples from a building site near Paris are also studied in order to verify their provenance. We conclude that they do not come from quarries from the Comblanchien area, but likely from Portugal. The study shows that a detailed analysis of building limestones may provide a robust tool for discriminating between currently mined stones of different provenances, and thus open the possibility to attach to a given limestone a fingerprint, an identity card, and if required a commercial label.     

Oceanographic and eustatic control of carbonate platform evolution and sequence stratigraphy on the Cretaceous (Valanginian–Campanian) passive margin,northern Gulf of Mexico

An integrated sequence stratigraphic study based on outcrop, core and wireline log data documents the combined impact of Cretaceous eustacy and oceanic anoxic events on carbonate shelf morphology and facies distributions in the northern Gulf of Mexico. The diverse facies and abundant data of the Comanche platform serve as a nearly complete global reference section and provide a sensitive record of external processes affecting Cretaceous platform development. Regional cross‐sections across the shoreline to shelf‐margin profile provide a detailed record of mixed carbonate–siliciclastic strata for the Hauterivian to lower Campanian stages (ca 136 to 80 Ma). The study window on the slowly subsiding passive margin allows the stratigraphic response to external forcing mechanisms to be isolated from regional structural processes. Three second‐order supersequences comprised of eight composite sequences are recognized in the Valanginian–Barremian, the Aptian–Albian and the Cenomanian–Campanian. The Valanginian–Barremian supersequence transitioned from a siliciclastic ramp to carbonate rimmed shelf and is a product of glacial ice accumulation and melting, as well as variable rates of mid‐ocean ridge volcanism. The Aptian–Albian supersequence chronicles the drowning and recovery of the platform surrounding oceanic anoxic events 1a and 1b. The Cenomanian–Campanian supersequence similarly documents shelf drowning following oceanic anoxic event 1d, after which the platform evolved to a deep‐subtidal system consisting of anoxic/dysoxic shale and chalk in the time surrounding oceanic anoxic event 2. Each period of oceanic anoxia is associated with composite sequence maximum flooding, termination of carbonate shelf sedimentation and deposition of condensed shale units in distally steepened ramp profiles. Composite sequences unaffected by oceanic anoxic events consist of aggradational to progradational shelves with an abundance of grain‐dominated facies and shallow‐subtidal to intertidal environments. Because they are products of eustacy and global oceanographic processes, the three supersequences and most composite sequences defined in the south Texas passive margin are recognizable in other carbonate platforms and published eustatic sea‐level curves.     

川西盆地下白垩统古流向逆变及沉积地球化学响应

通过对川西盆地下白垩统古流向的研究发现,川西盆地东缘早白垩世早期沉积的平均古流向为142°～145°,中、晚期沉积的平均古流向则为264°～288°,说明古流向发生了逆变。下白垩统泥质岩稀土、微量元素丰度的纵向变化表明,与此古流向逆变过程相对应沉积层段的元素丰度,也产生了明显的相对异常。这一地球化学异常既为该古流向逆变的存在提供了进一步的佐证,也揭示了该现象具有很好的、区域性的沉积地球化学响应。     

Rare earth element geochemistry of scleractinian coral skeleton during meteoric diagenesis: a sequence through neomorphism of aragonite to calcite

Rare earth element geochemistry in carbonate rocks is utilized increasingly for studying both modern oceans and palaeoceanography, with additional applications for investigating water–rock interactions in groundwater and carbonate diagenesis. However, the study of rare earth element geochemistry in ancient rocks requires the preservation of their distribution patterns through subsequent diagenesis. The subjects of this study, Pleistocene scleractinian coral skeletons from Windley Key, Florida, have undergone partial to complete neomorphism from aragonite to calcite in a meteoric setting; they allow direct comparison of rare earth element distributions in original coral skeleton and in neomorphic calcite. Neomorphism occurred in a vadose setting along a thin film, with degradation of organic matter playing an initial role in controlling the morphology of the diagenetic front. As expected, minor element concentrations vary significantly between skeletal aragonite and neomorphic calcite, with Sr, Ba and U decreasing in concentration and Mn increasing in concentration in the calcite, suggesting that neomorphism took place in an open system. However, rare earth elements were largely retained during neomorphism, with precipitating cements taking up excess rare earth elements released from dissolved carbonates from higher in the karst system. Preserved rare earth element patterns in the stabilized calcite closely reflect the original rare earth element patterns of the corals and associated reef carbonates. However, minor increases in light rare earth element depletion and negative Ce anomalies may reflect shallow oxidized groundwater processes, whereas decreasing light rare earth element depletion may reflect mixing of rare earth elements from associated microbialites or contamination from insoluble residues. Regardless of these minor disturbances, the results indicate that rare earth elements, unlike many minor elements, behave very conservatively during meteoric diagenesis. As the meteoric transformation of aragonite to calcite is a near worst case scenario for survival of original marine trace element distributions, this study suggests that original rare earth element patterns may commonly be preserved in ancient limestones, thus providing support for the use of ancient marine limestones as proxies for marine rare earth element geochemistry.     

Calpionellid zonation of the Jurassic–Cretaceous transition in North-Atlasic Tunisia. Updated Upper Jurassic stratigraphy of the ‘Tunisian trough’ and regional correlations

The analysis of calpionellid associations from jebels Amar and Jédidi sections in North-Atlasic Tunisia provides, for the first time, a precise biozonation of the Jurassic–Cretaceous transition succession. In the light of the new data obtained and considering recently published results, the age of Upper Jurassic formations is clarified, allowing correlations with the Tunisian ‘Dorsale’ and the North–South Axis successions. Within the Maghrebides' range, sections from the external zones correlated to the Tunisian successions are quite distinctive from their equivalent in the internal zones. Both have evolved in different palaeogeographic domains related to the early structuration of the northwestern and southwestern Tethys margins. To cite this article: M. Boughdiri et al., C. R. Geoscience 338 (2006).     

Stratigraphic evolution of a fluvial–eolian succession: The example of the Upper Jurassic—Lower Cretaceous Guará and Botucatu formations, Paraná Basin, Southernmost Brazil

The Guará and Botucatu formations comprise an 80 to 120 m thick continental succession that crops out on the western portion of the Rio Grande do Sul State (Southernmost Brazil). The Guará Formation (Upper Jurassic) displays a well-defined facies shift along its outcrop belt. On its northern portion it is characterised by coarse-grained to conglomeratic sandstones with trough and planar cross-bedding, as well as low-angle lamination, which are interpreted to represent braided river deposits. Southwards these fluvial facies thin out and interfinger with fine- to medium-grained sandstones with large-scale cross-stratification and horizontal lamination, interpreted as eolian dune and eolian sand sheets deposits, respectively. The Botucatu Formation is characterised by large-scale cross-strata formed by successive climbing of eolian dunes, without interdune and/or fluvial accumulation (dry eolian system). The contact between the Guará and the Botucatu formations is delineated by a basin-wide deflation surface (supersurface). The abrupt change in the depositional conditions that took place across this supersurface suggests a major climate change, from semi-arid (Upper Jurassic) to hyper-arid (Lower Cretaceous) conditions. A rearrangement of the Paraná Basin depocenters is contemporaneous to this climate change, which seems to have changed from a more restrict accumulation area in the Guará Formation to a wider sedimentary context in the Botucatu Formation.     

Prograde metamorphic sequence of REE minerals in pelitic rocks of the Central Alps: implications for allanite–monazite–xenotime phase relations from 250 to 610 °C

The distribution of REE minerals in metasedimentary rocks was investigated to gain insight into the stability of allanite, monazite and xenotime in metapelites. Samples were collected in the central Swiss Alps, along a well‐established metamorphic field gradient that record conditions from very low grade metamorphism (250 °C) to the lower amphibolite facies (～600 °C). In the Alpine metapelites investigated, mass balance calculations show that LREE are mainly transferred between monazite and allanite during the course of prograde metamorphism. At very low grade metamorphism, detrital monazite grains (mostly Variscan in age) have two distinct populations in terms of LREE and MREE compositions. Newly formed monazite crystallized during low‐grade metamorphism (<440 °C); these are enriched in La, but depleted in Th and Y, compared with inherited grains. Upon the appearance of chloritoid (～440–450 °C, thermometry based on chlorite–choritoid and carbonaceous material), monazite is consumed, and MREE and LREE are taken up preferentially in two distinct zones of allanite distinguishable by EMPA and X‐ray mapping. Prior to garnet growth, allanite acquires two growth zones of clinozoisite: a first one rich in HREE + Y and a second one containing low REE contents. Following garnet growth, close to the chloritoid–out zone boundary (～556–580 °C, based on phase equilibrium calculations), allanite and its rims are partially to totally replaced by monazite and xenotime, both associated with plagioclase (± biotite ± staurolite ± kyanite ± quartz). In these samples, epidote relics are located in the matrix or as inclusions in garnet, and these preserve their characteristic chemical and textural growth zoning, indicating that they did not experience re‐equilibration following their prograde formation. Hence, the partial breakdown of allanite to monazite offers the attractive possibility to obtain in situ ages, representing two distinct crystallization stages. In addition, the complex REE + Y and Th zoning pattern of allanite and monazite are essential monitors of crystallization conditions at relatively low metamorphic grade.     

Discussion of ‘Oceanographic and eustatic control of carbonate platform evolution and sequence stratigraphy on the Cretaceous (Valanginian–Campanian) passive margin,northern Gulf of Mexico’ by Phelps et al. (2014), Sedimentology, 61, 461–496

Errors in Phelps et al. ( 2014 ) arise from: (i) inclusion of the East Texas Basin and basin‐flank formations in a regional stratigraphic transect purported to represent the San Marcos Arch (axis of the Comanche Platform, central and south Texas); and (ii) revision of Edwards Group strata (Person Formation) that ignores well‐documented studies in the subsurface and adjacent outcrops in the Balcones fault zone and Edwards Plateau. Consequently, the Upper Albian Composite Sequence 104–101 of Phelps et al. ( 2014 ) should be revised from one cycle to three and the upper boundary of the Albian Supersequence should be elevated to 99·6 Ma.     

Aeschnidiid nymphs from the Jehol biota (latest Jurassic–Early Cretaceous), China, with a discussion of the family Aeschnidiidae (Insecta, Odonata)

Undoubted fossil nymphs of the family Aeschnidiidae within the Aeschnidioidea of the Anisoptera, Odonata are identified and described and their phylogenetic relationship and bioecological characteristics are deduced. The nymphs discovered previously in China, Mongolia and Russia and considered to be aeschnidiids are, in fact, unrelated to this group. All nine Chinese species in six genera can be merged into one alone, Aeschnidium heishankowense. It is the first animal from the ‘Jehol biota’ of East Asia to be linked with the species known from the Lower Tithonian of Germany. The geological age of the oldest strata bearing the fossil nymphs is debatable; it could be latest Jurassic rather than Early Cretaceous.     

REE地球化学在砂岩型铀成矿研究中的应用--以川北砂岩型铀矿床为例

本文在系统的取样分析基础上,总结了川北砂岩型铀矿床的稀土元素地球化学特征,分析研究了围岩、矿石、方解石脉和铀矿物的稀土元素组成、关系,讨论了岩、矿石沉积和成岩过程的稀土元素变化规律,与国内外典型的火山岩型和变质岩型热液成因铀矿床进行了对比,认为川北砂岩型铀矿具有热液（水）改造成矿作用的稀土元素地球化学特征,铀矿化经历了沉积成岩和热液改造富集两个阶段,为砂岩型铀矿成矿研究提供了新的思路。     

藏南洛扎地区侏罗纪—早白垩世层序地层与地层格架——兼论基本层序变化规律调查在区调工作中的运用

根据米级旋回垂向上的变化规律，新特提斯洋北缘北喜马拉雅被动大陆边缘的沉积层序自侏罗纪—早白垩世共可划分二级层序3个，三级层序18个。早、中侏罗世低位体系域不发育，由海进体系域与高位体系域两部分组成。晚侏罗世出现大型深切河谷。海平面下降幅度最大。早白垩世发育陆架边缘体系域。在此基础上建立了测区侏罗纪—早白垩世地层格架。讨论了当前1∶〖KG-*2〗25万、1∶〖KG-*2〗5万区调填图过程中岩石地层单位内基本层序调查应从静态的代表性基本层序描述转变为动态的基本层序变化规律的调查，阐明了基本层序变化规律与层序地层的关系。     

Oil seepage and carbonate formation: A case study from the southern Gulf of Mexico

Oil seeps from the southern Gulf of Mexico can be regarded as natural laboratories where the effect of crude oil seepage on chemosynthesis‐based communities and carbonate precipitation can be studied. During R/V Meteor cruise 114 the seep sites UNAM (Universidad Nacional Autónoma de México) Ridge, Mictlan Knoll and Tsanyao Yang Knoll (Bay of Campeche, southern Gulf of Mexico) were investigated and sampled for authigenic carbonate deposits containing large amounts of liquid oil and solid asphalt. The δ¹³C values of individual carbonate phases including: (i) microcrystalline matrix aragonite and calcite; (ii) grey, cryptocrystalline to microcrystalline aragonite; and (iii) clear, fibrous aragonite cement, are between ?30‰ and ?20‰, agreeing with oil as the primary carbon source. Raman spectra reveal that residual heavy oils from all sites are immature and most likely originate from the same reservoir. Geochemical batch modelling using the software code PHREEQC demonstrates how sulphate‐driven oxidation of oil‐derived low‐molecular to high‐molecular weight hydrocarbons affects carbonate saturation state, and shows that the oxidation state of carbon in hydrocarbon compounds and oxidation rates of hydrocarbons control carbonate saturation and precipitation at oil seeps. Phase‐specific trace and rare earth element contents of microcrystalline aragonite and calcite, grey cryptocrystalline aragonite and clear aragonite were determined, revealing enrichment in light rare earth elements for grey aragonite. By comparing trace element patterns of carbonates with those of associated oils, it becomes apparent that liquid hydrocarbons constitute an additional source of trace metals to sedimentary pore waters. This work not only demonstrates that the microbial degradation of oil at seeps may result in the precipitation of carbonate minerals, it also elucidates that trace metal inventories of seep carbonates archive diagnostic elemental patterns, which can be assigned to the presence of heavy hydrocarbons in interstitial pore waters.     

Tetrapods from the Upper Cretaceous (Turonian–Maastrichtian) Bauru Group of Brazil: a reappraisal

An updated, annotated list of all tetrapods from the Adamantina, Uberaba and Marília formations (Bauru Group), which constitute some of the best studied Upper Cretaceous units in Brazil, is presented. Tetrapod diversity in the Bauru Group is remarkable, including an admixture of typically austral Gondwanan taxa (e.g., abelisaurids, notosuchians) and boreal Gondwanan forms (e.g., carcharodontosaurids). Of note is the absence of Laurasian taxa in the upper portion of the Bauru Group. With the exception of some turtles, an anuran, mesoeucrocodylians and one titanosaur, most taxa from the Bauru Group are based on fragmentary and isolated bones, and as such many specimens can be identified only to a higher taxonomic level. Fishes, turtles, anurans, mesoeucrocodylians, dinosaurs, birds and mammals from the Adamantina and Marília formations resemble the latest Late Cretaceous vertebrate faunas from southern South America, except for the absence of ornithischian dinosaurs.     

Mudstones of the Tanqua Basin, South Africa: an analysis of lateral and stratigraphic variations within mudstones, and a comparison of mudstones within and between turbidite fans

Permian deep‐water mudstones in the Tanqua Basin, South Africa, have been studied using geochemical and spectral gamma ray techniques. The mudstones occur as thick sequences between sand‐rich submarine fans, but also occur as thinner mud‐rich units within each fan. The interfan mudstones are interpreted to have accumulated during transgression and the consequent period of relatively high sea‐level, while the submarine fans and their intrafan mudstones were deposited during regression and relatively low sea‐level. Geochemical analyses revealed systematic differences between interfan and intrafan mudstones because the two types of mudstones have slightly different source lithologies. Differences between the two types of mudstone suggest that changes in relative sea‐level played a role in controlling exposure of sediment source areas. There are geochemical signals that display systematic stratigraphic trends within both interfan and intrafan mudstones. These are best explained by gradual denudation, exposure and weathering of different lithologies within a single sediment source area. Both interfan and intrafan mudstones have uniform geochemical signals along the flow direction except for the relative amount of uranium. It is most likely that the basinward increase in uranium in the mudstones is the result of reduced clastic dilution of uranium‐bearing pelagic fallout.     

Happy Jack Uraninite: A New Reference Material for High Spatial Resolution Analysis of U‐Rich Matrices

There is currently a lack of well‐characterised matrix‐matched reference materials (RMs) for forensic analysis of U‐rich materials at high spatial resolution. This study reports a detailed characterisation of uraninite (nominally UO_2+x) from the Happy Jack Mine (UT, USA). The Happy Jack uraninite can be used as a RM for the determination of rare earth element (REE) mass fractions in nuclear materials, which provide critical information for source attribution purposes. This investigation includes powder X‐ray diffraction (pXRD) data, as well as major, minor and trace element abundances determined using a variety of micro‐analytical techniques. The chemical signature of the uraninite was investigated at the macro (cm)‐scale with micro‐X‐ray fluorescence (µXRF) mapping and at high spatial resolution (tens of micrometre scale) using electron probe microanalysis (EPMA) and laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) analyses. Based on EPMA results, the uraninite is characterised by homogeneous UO₂ and CaO contents of 91.57 ± 1.49% m/m (2s uncertainty) and 2.70 ± 0.38% m/m (2s), respectively. Therefore, CaO abundances were used as the internal standard when conducting LA‐ICP‐MS analyses. Overall, the major element and REE compositions are homogeneous at both the centimetre and micrometre scales, allowing this material to be used as a RM for high spatial resolution analysis of U‐rich samples.