Samples for all analyses presented in this paper were collected along LOG-05, at the positions indicated on Supplementary Figure S1, aimed at obtaining a complete profile through the local K-Pg boundary section, with palynomorphs, foraminifera, macro charcoal, fossil wood, materials for dating, and iridium content, to ascertain their correct relative stratigraphic position, and to correlate with other K-Pg sections globally. All figures and tables related to the methods applied are available as Supplementary Information.
4.1 Palynology
Seventeen samples were collected through LOG-05 (Supplementary Fig. S1) and were prepared at the Marleni Marques Toigo Laboratory of Palynology at UFRGS, Porto Alegre, Brazil, using the methodology in Supplementary Table S1. Counts of two hundred palynomorphs per slide were made where possible. Biostratigraphic determinations were made utilizing first occurrence, last occurrence, and acme zones previously defined onshore and offshore Mexico [30, 49], and the USA [50–54] to help determine the relative age. In addition, the color of abundant spore Stereisporites spp. was recorded using the standard spore color index methodology [55].
The lowermost samples, collected from a blue-gray mudstone (Unit A) demonstrate a diverse assemblage of Maastrichtian palynomorphs including pollen (e.g. Classopollis spp., Tricolporopollenites spp.), spores (e.g. Biretisporites spp. and Todisporites spp.), and dinoflagellate cysts, including the Cretaceous markers Dinogymnium spp. and Yolkinigymnium spp., with representatives of fifty-four genera of both marine and terrestrial forms (Supplementary Fig. S2).
Above the bioclastic debrite the abundance and diversity are severely reduced, with only seven genera, and the sample dominated by fungal spores (Fig. S2). 18 m of section above the lapilli tuff is barren of palynomorphs, but rich in degraded humic debris. At the top of the study interval a spike in fern spores is observed (e.g. Baculatisporites comaumensis and Laevigatosporites spp.), along with diminutive Danian dinocysts (e.g. Damassadinium californicum) and a distinct absence of any Cretaceous palynomorphs. The count data are presented in Supplementary Table S2, where general groups of palynomorphs are also presented to demonstrate the wider variation in floral abundance.
4.2 Foraminifers and macro charcoal quantification
Separation of foraminifera tests and macro charcoal fragments was carried out concomitantly. Fifteen samples were collected through LOG-05 (collocated with samples for palynology, as shown in Fig. S1). Preparation and identification were conducted following standard procedures, e.g. [56], but the friable nature of the material simplified and shortened the process: 200 g fractions (and in some cases 400 g, for samples where recovery was poor) of each sample were immersed in a container with distilled water. After a few minutes, the samples were gently disaggregated manually and filtered in a 63 µm sieve to remove the clay minerals. The remaining material was then dried in an oven at a controlled temperature of 40o Celsius.
Selection of specimens was conducted using a Leica S6D stereoscopic microscope, and identification of the foraminifers was conducted using the ACEMAC Nano Scale Electron Microscopy and Analysis Facility at the University of Aberdeen, with the Carl Zeiss Gemini SEM 300 – high resolution Field Emission Scanning Electron Microscope (FESEM). 200 foraminifera specimens were counted and identified for each sample when possible, and the data are presented on Table S3. Macro charcoal particles were counted, and their total volumetric estimates were established based on original volume of each sample.
4.3 Fossil wood
The material consists of three trunks collected from LOG-05 site (Supplementary Fig. S1, location map in Fig. 2), that represent monopodial trees preserved as silica permineralization. Due to the size of these trunks, the sampling method implemented consisted in removing a fragment of its outermost wood and collecting dispersed wood fragments. Subsequently, the samples were transferred to the Paleobotany Laboratory of the Institute of Geology, UNAM, where they were cut to obtain sections in the three cutting planes (transverse, radial and tangential) used for wood anatomical studies. Conventional thin section techniques were applied. The photomicrographs were obtained with a Canon PowerShot A640 camera and a Carl Zeiss AxioCam ICc 5. Subsequently, they were assembled into photographic plates aided with Illustrator CS4 program.
The recognition of the anatomical characters was based on [57–61]. For quantification, 20 measurements were obtained per attribute, and for ray height 35 measurements were made. Subsequently, for each characteristic, its average minimum and maximum values were obtained, expressed as follows: average (minimum-maximum) unit. Regarding the measurement and quantification of the tracheid radial pitting, the contiguity index (Cp) and seriation index (Si) of [62] were followed.
For the taxonomic identification of fossil woods at genus level we followed [60–61, 63–65]. For species level identification, comparisons were made with conifer wood of extant species based mainly on [58, 66–67]; while comparisons with fossil wood articles describing wood of the same or similar taxa were also used, e.g. [68–72].
4.4 Raman spectrometry
Raman spectra were obtained through random sampling of individual charcoal fragments (n = 50), with no additional treatment. Charcoal sampling surfaces were selected for high reflectivity where possible to ensure adequate spectral response. A laser power of < 0.3mW was applied over 3 accumulations, totalling 15s exposure per sample. No combustion damage was observed on laser-irradiated surfaces post-exposure. All spectra were deconvolved within Renishaw WiRE 3.4 software, applying smoothing and a cubic spline interpolative baseline, and bands D and G fit solely. For geothermometric purposes, parameter FWHMRa (D- and G-band width ratio) was utilised within the following equation
$$Formation Temperature \left(℃\right)= \frac{\left[FWHMRa\right]-3.1765}{-0.0016}$$
From Theurer et al. (unpubl.). See also Supplementary Information, Table S4, Fig. S3. Statistical analyses were conducted in IBM SPSS v. 25, via histogram and boxplot presentation (Supplementary Figures S4 and S5, Table S5).
4.5 SHRIMP U-Pb zircon dating
For SHRIMP U-Pb zircon analyses, 1.5 kg of a rock sample of the tuff (SF-30, indicated in Fig. S1) were crushed, powdered, and sieved. Heavy mineral concentrates were obtained by panning, and purified using heavy liquid procedures. Grains were set in epoxy resin mount (together with the Temora zircon standard) and polished. Backscattered electron and cathodoluminescence images were obtained for better spot targeting using a FEI-QUANTA 250 scanning electron microscope equipped with secondary-electron and cathodoluminescence (CL) detectors. The analyses were performed in a SHRIMP IIe/MC at Center of Geochronological Research of the University of Sao Paulo (CPGeo-USP) following the procedures described by [73]. 206Pb/238U ratio was calibrated using the standard Temora [74]. Measured 204Pb was applied for the common lead correction.
Data reduction, plots and calculated ages were carried out using Excel spreadsheets with the support of Squid 2.0 [75] and Isoplot 3.0 [76]. A more detailed description can be found in [77]. Twenty-eight grains were analyzed, and the data are presented in Supplementary Table S6. Supplementary Figure S6-A shows all results in the concordia diagram. Three analyses were interpreted as from detrital or inherited older grains (in green, Supplementary Table S4), and one analysis was considered an outlier (in blue). The 24 remaining analyses yielded a 66.12 ± 0.32 Ma concordia age (1 sigma error) (Supplementary Fig. S3-B) and 66.12 ± 0.65 Ma 206Pb/238U weighted mean age (2 sigma error) (Supplementary Fig. S3-C).
4.6 Iridium analysis
Three samples were collected for iridium content analysis by NiS Fire Assay-Instrumental Neutron Activation Analysis (INAA) (indicated in Supplementary Fig. S1): two (LOG-05-07 and LOG-05-21) from the pebbly mudstones of the K-Pg deposits and one (MWD-18) of the hemipelagic mudstone immediately above. They were pulverized to a nominal 2 mm, mechanically split to obtain a representative sample and then pulverized to at least 95% passing − 105 µm or smaller. Samples were subsequently transferred to the ACTLAB facilities in Ontario, Canada, and analyzed following the procedures described in [78–79].
25 g of each sample, along with 2 blanks, 3 certified standards and 3 duplicates, were fire assayed using nickel sulfide (NiS) fire assay procedure. The nickel sulfide button was then dissolved in concentrated HCl, and the residues of this reaction, containing all the iridium (and other PGE) were then collected on a filter paper. This residue was then submitted to two irradiations and three separate counts to measure all the elements.
Iridium concentrations for the three samples analyzed and used in this paper are presented in Table S7, along detection limits of the method used.