Loss on ignition: a qualitative or quantitative method for organic matter and carbonate mineral content in sediments?

Since the publication of the paper of , loss on ignition (LOI) has been widely used as a method to estimate the amount of organic matter and carbonate mineral content (and indirectly of organic and inorganic carbon) in sediments. The relationships between LOI at 550 °C (LOI₅₅₀) and organic carbon (OC) content and between LOI at 950 °C (LOI₉₅₀) and inorganic carbon (IC) content are currently accepted as a standard. However, the comparison of 150 analyses of samples of diverse lithologies, collected from a single core, reveals that these relationships are affected by sediment composition (presence of clays, salts, and the variable content of organic carbon). This results in an incremental error on the estimation of carbon content from LOI values that invalidates the use of LOI values as a quantitative method for estimating carbon content. Conversely, the general trends of LOI₅₅₀ and LOI₉₅₀ show a good correlation with carbon content (both organic and inorganic) allowing use of LOI as a qualitative test for carbon content. Similarly, in our case, LOI at 105 °C (LOI₁₀₅) is a good qualitative proxy for the trends in gypsum content.     

Aspects of the loss-on-ignition (LOI) technique in the context of clay-rich, glaciolacustrine sediments

The loss‐on‐ignition (LOI) technique for organic matter determination is evaluated with reference to clay‐rich, glaciolacustrine sediments. Examples of the use of LOI in glaciolacustrine literature are inconsistent in their methodology, and standardisation is called for. Problems with application of the technique to glaciolacustrine sediments stem mainly from the effects of additional weight loss due to release of structurally bound water and exposure time to ignition temperatures. Exposure time should be increased from 1 hour to 2.5 hours in the light of significant additional weight loss occurring between 2 and 2.5 hours in clay‐rich samples. The reason for this sudden increase in LOI after 2 hours (up to 86% of total LOI in some cases) appears to be the build‐up of a distinct surface crust during heating that insulates the core of the sample from ignition temperatures. Some time between 2 and 2.5 hours, the crust breaks down and exposes the sample core to ignition temperatures, increasing weight loss significantly. Overestimation of LOI due to loss of structural water is thought to be insignificant. Replicates of LOI at 550 and 1000°C in non‐calcareous, clay‐rich (>40%) sediments, show differences of <0.25%, which, for the purpose of inferring broad changes in glacier extent in lake catchments, is an acceptable error.     

Controls on loss-on-ignition variation in cores from two shallow lakes in the northeastern United States

Loss-on-ignition analysis of Quaternary lake sediments provides an inexpensive and easy way to investigate past environmental changes. The mass loss on ignition at 550 °C (LOI) from lake sediment cores may vary because of temporal changes in: (1) sediment composition controlled by factors such as productivity, inorganic inputs, and decomposition; and (2) the patterns of sediment accumulation controlled by factors such as basin morphology and water level. Climatic changes can alter both. Here, modern surface samples and transects of sediment cores, collected across small (<10 ha), shallow (<4 m) lakes in the northeastern United States, show that LOI varies little (2–5%) across the deep portions of these small lakes at a given time. Large changes in LOI occur only at the transition into the littoral (shallow) zone. LOI variations in sediment cores that exceed 2–5%, therefore, appear to represent meaningful environmental changes. However, because of the many possible controls, changes in the LOI of a single core are often hard to interpret. Multiple cores increase the interpretability. At lakes studied here, similar LOI trends among several cores confirm that some LOI changes resulted from basin-wide shifts in sediment composition. Differences among cores, however, developed during the early- and mid-Holocene and indicate that the edge of the littoral zone moved towards the centers of the lakes during two periods of low lake levels, at ca. 11 000–8000 and ca. 5400–3000 cal yr B.P. The basin-wide balance of sediment sources controlled the LOI from deep-water sediments, but sedimentation patterns, which changed as lake levels changed, were also important. LOI differences among cores may therefore help identify past lake-level changes in other lakes.     

Loss on ignition vs. thermogravimetric analysis: a comparative study to determine organic matter and carbonate content in sediments

Journal of Paleolimnology - Mass loss at specified temperatures has been used widely to determine amounts of organic matter and carbonate in sediment samples. The loss on ignition (LOI) method is...     

东南极拉斯曼丘陵中晚全新世湖泊生物量的变化记录

对东南极拉斯曼丘陵莫愁湖ZH沉积柱进行了生态地质学的研究,通过AMS-14C定年构建年龄框架,采用550℃烧失量、粒度和元素地球化学指标等,恢复了中晚全新世该地区较高分辨率的湖泊生物量记录。结果显示,距今6600-6100年、5400-4800年、4650-3750年和3500年-2850年为莫愁湖生物量高值期,气候相对温暖适宜,湖泊生产力旺盛;距今6100-5400年、4800-4650年和3750-3500年为湖泊生物量低值期,气候相对寒冷,湖泊生产力相对较弱。而且在整体较暖的气候环境下,出现了其它无冰区沉积物中鲜有记录的距今4800-4650年、4400年前后和3750-3500年的气候快速变冷事件。根据莫愁湖湖泊生物量恢复的东南极拉斯曼地区高分辨的气候变化特征,与太阳活动强度和东南极大陆冰芯记录相吻合,为东南极中晚全新世多样的气候格局研究提供了新的依据。     

The effects of organic removal treatment on the integrity of δ<Superscript>18</Superscript>O measurements from biogenic silica

Prior to oxygen isotope analysis of biogenic silica by fluorination techniques, sediments must be cleaned of all organic compounds. Despite the expanding volume of research utilising oxygen isotope ratios in biogenic silica in palaeoclimatology, very little is known about the effects of different standard preparation methods for the removal of organic matter on the isotope values. Here we compare a number of methods for the removal of organic matter in order to assess their effectiveness and influence on subsequent isotope measurements. Not all the methods described here effectively removed organic matter, the best treatments were H₂O₂ and ignition in air at 550°C. Ignition in air at 950°C, and heating in vacuum at 250 and 450°C results in marked alteration of isotope values, whereas use of hydrogen peroxide (H₂O₂), nitric acid (HNO₃) and plasma ashing have little or no effect, within the bounds of analytical error. Ignition in air at 550°C was the most effective technique, and induced no alteration of δ¹⁸O_silica, but practical constraints may limit the application of this method routinely. Our findings indicate that considerable caution is required when preparing sediment for isotope analysis of biogenic silica.     

Geochemical evidence for the variation of historical seabird population on Dongdao Island of the South China Sea

From a rare freshwater lake characteristic of alkalescence, named “Cattle Pond”, on the Dongdao Island of South China Sea (16°39′–16°41′ N, 112°43′–112°45′ E), we collected two undisturbed sediment cores that contain seabird droppings. In this paper, we determined the concentration-versus-depth profiles of the geochemical elements in the ornithogenic sediment layers of the two cores, analyzed these profiles by various statistical methods, and studied their geochemical characteristics. The concentration profiles of As, Cd, Cu, Se, Zn, P and S are significantly correlated with each other and with loss on ignition (LOI) at 550°C, the measure for the abundance of organic matter. Similar geochemical characteristics, however, were not observed in the upper sediment layer of the Cattle Pond notably affected by cattle excrements, as well as in the bottom sediment layer compositionally dominated by coral sand and gravel. This shows that these “bio-elements” are mainly derived from seabird feces and their geochemical composition is an important geochemical characteristic of the lacustrine ornithogenic sediments. By Q-mode factor analysis (QFA) on the concentration profiles of these bio-elements, we reconstructed the historical seabird population on Dongdao Island between 1350 and 350 year B.P., and observed significant fluctuations in the calculated population. The fluctuations seem to be related to the change of sea surface temperature (SST) in the Southern China Sea. This study provides new paleoenvironmental information of past seabird population changes in low latitude areas using an indirect geochemical method.     

烧失量分析在湖泊沉积与环境变化研究中的应用

烧失量分析是一种便捷的测定湖泊沉积物有机碳与碳酸盐含量的方法。由于沉积物烧失量主要受区域气温、有效降水等气候环境条件的控制,因此烧失量反映湖泊气候环境特征,成为指示区域气候环境变化的重要指标,该项指标在环境变化研究中具有重要作用。     

Holocene sediments of Sägistalsee, a small lake at the present-day tree-line in the Swiss Alps

Sägistalsee is a small lake located at the modern tree-line in the Swiss Alps. A 13.5 m long core taken in the central part of the 9.5 m deep basin consists of clayey silts and sands and dates back to about 9000 cal. BP. These sediments have a low organic content that steadily increases from 4–8% loss-on-ignition at 550 °C towards the top of the core, whereas the carbonate content decreases from 20 to about 10% loss-on-ignition at 950 %C. We outline the aims of an interdisciplinary research project centred on the Holocene sediments of Sägistalsee. We also present information about the lake, its sediments, and its catchment that forms the basis for different biotic and abiotic multi-proxy studies carried out on the sediments of Sägistalsee.     

A sediment record of trophic state change in an Arkansas (USA) reservoir

Reservoir sediments are used cautiously in paleolimnological studies because of dating uncertainties, possible sediment disturbances and even concerns that indicators of trophic status may behave differently in reservoirs as opposed to natural lakes. We measured loss on ignition (LOI), carbon to nitrogen ratio (C:N), diatom abundance, total nitrogen (TN), total phosphorus (TP), TN:TP ratio, and carbon and nitrogen isotopes (δ¹³C and δ¹⁵N) in an 83-cm sediment core to track recent trophic status changes in Beaver Reservoir, Northwest Arkansas, USA. Measurements showed that LOI, TN, TP and diatom abundance increased significantly from the bottom to the top of the core (p < 0.001). The C:N ratio and δ¹³C indicated a predominantly algal source for organic matter in the sediments. Increases in TN and TP were positively correlated with human population growth (p < 0.01) and the TN:TP ratio recorded a shift from phosphorus to nitrogen limitation around 1990. This shift may have encouraged cyanobacterial growth that caused episodes of taste and odor problems in the reservoir. This study suggests that despite concerns about sediment dating and disturbance, reservoir sediments can provide valuable information on past water quality changes.     

Chironomids as indicators of climate change: a 100‐lake training set from a subarctic region of northern Sweden (Lapland)

Multivariate numerical analyses (DCA, CCA) were used to study the distribution of chironomids from surface sediments of 100 lakes spanning broad ecoclimatic conditions in northern Swedish Lapland. The study sites range from boreal forest to alpine tundra and are located in a region of relatively low human impact. Of the 19 environmental variables measured, ordination by CCA identified mean July air temperature as one of the most significant variables explaining the distribution and the abundance of chironomids. Lossonignition (LOI), maximum lake depth and mean January air temperature also accounted for significant variation in chironomid assemblages. A quantitative transfer function was created to estimate mean July air temperature from sedimentary chironomid assemblages using weightedaveraging partial least squares regression (WAPLS). The coefficient of determination was relatively high (r² = 0.65) with root mean squared error of prediction (RMSEP, based on jack-knifing) of 1.13 °C and maximum bias of 2.1 °C, indicating that chironomids can provide useful quantitative estimates of past changes in mean July air temperature. The paper focuses mainly on the relationship between chironomid composition and July air temperature, but the relationship to LOI and depth are also discussed.     

Tracking Holocene environmental changes in an alpine lake sediment core: application of regional diatom calibration, geochemistry, and pollen

Diatom abundances in the surface sediment samples of 41 mountain lakes in the central Austrian Alps (Niedere Tauern) were related to environmental variables using multi-variate techniques. Canonical correspondence analysis (CCA) revealed that the pH, date of autumn mixing (A _mix), mean August water temperature (T _Aug), dissolved organic carbon (DOC), and relative water depth (Z _rel) made significant contributions to explain the diatom assemblage variation in the lakes of the training set. A weighted averaging partial least square regression and calibration model was used to establish Di-pH (R ² _boot= 0.72, RMSEP_boot= 0.131), and a thermistor measurements-based PLS model for A _mix (R ² _boot= 0.71, RMSEP_boot= 0.006 log₁₀ Julian days). The latter showed a better prediction than T _Aug, and was used in terms of climate change. These transfer functions, together with analyses of loss on ignition (LOI), the total carbon/nitrogen (C/N)-ratios, and selected pollen, were applied to an early to mid-Holocene (11.5–4 cal. ky BP) sediment core section from an Austrian Alpine treeline lake on crystalline bedrock. Additionally, passive sample scores in the CCA of the diatom training set were used to show trends in the variables DOC and Z _rel. During the early Holocene, diatoms indicative of increased pH, extended warm summers, and low water levels dominated. Between 10.2 and 7.6 cal. ky BP it was followed by diatom assemblages that indicated an increase in lake water depth and an earlier A _mix. The multi-proxy data suggest that the A _mix decline is the result of a series of snow-rich summer cool and wet climate fluctuations, which were divided by climate warming at ∼9 cal. ky BP. Increased A _mix, LOI and DOC, and the correspondent decline in the C/N-ratios, show subsequent climate warming between 7.3 and 6 cal. ky BP. The long-term trend in Di-pH indicates the impact of catchment-related processes during the early-Holocene, that were superimposed by climate.     

Is laser particle size determination possible for carbonate-rich lake sediments?

This paper examines the potential of a relatively new technique – laser diffraction particle size analysis – for use with carbonate-rich lake sediments, material traditionally difficult to analyse. Three experiments are considered. The first two use a carbonate standard to determine optimal instrument conditions – the choice of optical model, and a suitable transport fluid. The third experiment uses sample material from lake cores and compares four different pre-treatment methods: none, removal of carbon by loss on ignition, removal of carbon by digestion with hydrogen peroxide, and finally removal of carbonates with hydrochloric acid and then removal of organic material by digestion with hydrogen peroxide. Only this final method produces repeatable results. As such, whilst the laser diffraction instrument offers improvements in the speed, required sample volume and repeatability of analysis, it does not overcome the problems inherent in the analysis of carbonates. Any catchment disturbance signal preserved in the carbonate fraction will remain undetected.     

The efficiency of kerosene flotation for extraction of chironomid head capsules from lake sediments samples

Kerosene, a grade mineral oil, is commonly used to extract beetles from sediment. Here, the use of kerosene to extract chironomid head capsules was tested on 10 samples from sediment of different lakes, with different organic matter content as measured by loss on ignition, and estimated ages. Our results revealed that this flotation tool is very effective in extracting either full or half chironomid head capsules. The mean extraction efficiency was 89.3 ± 8.0% with an estimated relative abundance error ranging from −1% to 1% for 46 of the 57 identified taxa. Larger chironomids (400–500 μm width), which are often full of sediment particles, have the highest relative abundance error, with a maximum of 4.3% for Corynocera oliveri-type. A canonical correspondence analysis showed that, despite this small bias, samples retrieved with the kerosene flotation do not differ from the whole sample assemblages. These results give us confidence in the use of this flotation technique for chironomid sample preparation.     

Comparison of radiocarbon and OSL dating methods for a Late Quaternary sediment core from Lake Ulaan,Mongolia

Both radiocarbon and optically stimulated luminescence (OSL) dating methods were applied to test their suitability for establishing a chronology of arid-zone lacustrine sediments using a 5.88-m-long core drilled from Lake Ulaan, southern Mongolia. Although the radiocarbon and OSL ages agree in some samples, the radiocarbon ages are older than the corresponding OSL ages at the 550-cm depth horizon (late Pleistocene) and in the 100–300-cm interval (early to late Holocene). In the early to late Holocene, radiocarbon ages are consistently older than OSL ages by 4,100–5,800 years, and in the late Pleistocene by 2,700–3,000 years. Grain-size analysis of early to late Holocene sediments and one late Pleistocene sediment sample (550-cm depth) indicates that eolian processes were the dominant sediment-transport mechanism. Also, two late Pleistocene sediments samples (from 400- to 500-cm depths) are interpreted to have been deposited by both eolian and glaciofluvial processes. Accordingly, the radiocarbon ages that were older than the corresponding OSL ages during the Holocene seem to have been a consequence of the influx of ¹⁴C-deficient carbon delivered from adjacent soils and Paleozoic carbonate rocks by the westerly winds, a process that is also active today. In addition to the input of old reworked carbon by eolian processes, the late Pleistocene sediments were also influenced by old carbon delivered by deglacial meltwater. The results of this study suggest that when eolian sediment transport is suspected, especially in lakes of arid environments, the OSL dating method is superior to the radiocarbon dating method, as it eliminates a common ‘old-carbon’ error problem.     

西辽河流域中晚全新世气候环境演变及其对农牧业演替的影响

气候变化是人类文明演化的重要驱动力之一,中国东北西辽河流域地处季风气候敏感带,早中全新世以来古文化演替频繁,具有研究气候变化与早期农业文明响应的重要价值。本文基于西辽河流域兴隆洼（XLW）剖面高精度年代学框架开展多种气候代用指标分析,重建了中晚全新世以来西辽河流域的气候环境演变历史。结果显示,距今5.0 ka以来研究区经历了冷干—暖湿—冷干的气候演变过程。5.0—3.7 cal. ka BP期间,磁化率、烧失量等指标的低值反映了气候由全新世大暖期向冷干环境的转变,可能与东亚夏季风的衰退有关。该时期红山文化衰退,逐渐被以渔猎和农业并重的小河沿文化所取代,东北地区遗址数量有所减少并出现明显南偏。3.7 cal. ka BP后,磁化率、烧失量等指标的高值指示了夏季风的增强,水热条件的改善促进了旱作农业的发展,为夏家店下层文化的发展提供了有利条件。这一阶段东北地区出现人口大爆发,遗址数量达到峰值。2.8 cal. ka BP后,磁化率与烧失量波动降低,表明夏季风波动频繁,气候逐渐转冷干,水热条件的衰退可能导致了夏家店上层文化时期旱作农业的退化与游牧业的发展,且遗址分布出现南偏。     

Diatoms as indicators of climatic and limnological change in Swedish Lapland: a 100-lake calibration set and its validation for paleoecological reconstructions

This study investigated the distribution of subfossil diatom assemblages in surficial sediments of 100 lakes along steep ecological and climatic gradients in northernmost Sweden (Abisko region, 67.07° N to 68.48° N latitude, 17.67° E to 23.52° E longitude) to develop and cross-validate transfer functions for paleoenvironmental reconstruction. Of 19 environmental variables determined for each site, 15 were included in the statistical analysis. Lake-water pH (8.0%), sedimentary loss-on-ignition (LOI, 5.9% and estimated mean July air temperature (July T, 4.8%) explained the greatest amounts of variation in the distribution of diatom taxa among the 100 lakes. Temperature and pH optima and tolerances were calculated for abundant taxa. Transfer functions, based on WA-PLS (weighted averaging partial least squares), were developed for pH (r² = 0.77, root-mean-square-error of prediction (RMSEP) = 0.19 pH units, maximum bias = 0.31, as assessed by leave-one-out cross-validation) based on 99 lakes and for July T (r² = 0.75, RMSEP = 0.96 °C, max. bias = 1.37 °C) based on the full 100 lake set. We subsequently assessed the ability of the diatom transfer functions to estimate lake-water pH and July T using a form of independent cross-validation. To do this, the 100-lake set was divided in two subsets. An 85-lake training-set (based on single limnological measurements) was used to develop transfer functions with similar performance as those based on the full 100 lakes, and a 15-lake test-set (with 2 years of monthly limnological measurements throughout the ice-free seasons) was used to test the transfer functions developed from the 85-lake training-set. Results from the intra-set cross-validation exercise demonstrated that lake-specific prediction errors (RMSEP) for the 15-lake test-set corresponded closely with the median measured values (pH) and the estimations based on spatial interpolations of data from weather stations (July T). The prediction errors associated with diatom inferences were usually within the range of seasonal and interannual variability. Overall, our results confirm that diatoms can provide reliable and robust estimates of lake-water pH and July T, that WA-PLS is a robust calibration method and that long-term environmental data are needed for further improvement of paleolimnological transfer functions.     

Discriminating Bio-Induced and Detrital Sedimentary Processes from Particle Size Distribution of Carbonates and Non-Carbonates in Hard Water Lake Sediments

Particle size distribution (PSD) and carbonate content are two of the most frequently used parameters for describing lake sediments. This paper presents a method for rapidly measuring both these parameters using a laser particle-sizer, as well as an original way in which to separately interpret the PSD of the carbonate and non-carbonate fractions. Differential particle size analyses are produced by measuring the PSD of each sample twice. The first PSD is measured using the bulk sample. The second PSD is measured after the carbonate fraction has been completely dissolved by adding hydrochloric acid to the sample. As well as particle size analyses, laser particle-sizers automatically give obscuration values for the samples being analysed. By comparing the obscuration value for the bulk sample with the value for the de-carbonated fraction, the carbonate content of the sediment can be determined. In order to test the accuracy of the method, the results were compared with chemical analyses of carbonate content. This comparison showed that when applied to diatom-rich samples the method underestimates the carbonate content. This is due to the fact that the differential particle size method measures the volume concentrations of the carbonate and non-carbonate fractions, whereas chemical analysis measures the weight concentrations. As diatoms are hollow and have relatively low-densities, differential particle size analyses of diatom-rich samples overestimate the non-carbonate fraction. Despite this limitation, and bearing in mind that laser particle-sizer distributions are expressed in terms of volume percent for each size class and not weight percent, PSDs can provide useful data for interpreting sedimentary processes. One of the main advantages of this method is that it can be used to separate the PSDs of the carbonate (autochthonous) fraction and the non-carbonate (allochthonous) fraction from the PSD of the bulk sample. The value of such an approach was demonstrated by the analysis and interpretation of a 9 m-long core from Lake Bourget in France. An analysis of the bulk sample PSDs plotted as a function of depth showed the consistency of sedimentary processes over the last 7200 years. Amongst these processes, it was possible to identify two modes of clastic material deposition: river-borne fine sedimentation during major floods and gravity reworking of sandy sediment from the lakeshore.     

Seed germination of Southern Chihuahuan Desert plants in response to elevated temperatures

High temperature is one of the main factors that prevent germination, through premature aging of the embryo. The high temperatures reached in the soil of arid environments can affect seed survival and plant establishment. In this study we tested whether seed exposure to high temperature (40 °C and 70 °C) affected germination of eight species common to the Southern Chihuahuan Desert, and used for fodder, firewood and timber, fiber, edible flowers, fruits and stems. The responses to heat varied between species. Two of the tested species were not affected by heat exposure; for two other species germination was higher, and for the remaining four, germination was lower. There was also a delay of germination after heat exposure. Seeds of three species germinated >1 d slower after exposure to high temperatures. These results could help establish management programs for these Chihuahuan desert species under a climate change scenario.     

Sieve mesh size and quantitative chironomid paleoclimatology

The minimum sieve mesh size for fossil chironomid analysis is usually set at 100 μm, to ensure adequate recovery of small species. Yet taking into account the labor intensity of sorting and identifying fossil chironomid remains, the large numbers of samples requiring processing in paleoclimate studies with high temporal resolution, and the increasing need to engage non-specialist analysts in this work, it seems appealing to sieve samples through a larger mesh size that would mainly retain easier-to-see, easier-to-extract and easier-to-identify fossil specimens. In this study we evaluated the influence of sieve mesh size on chironomid-based quantitative paleoenvironmental reconstructions in African lakes. We developed two chironomid-salinity calibration data sets based on either the >100 μm or >150 μm size fractions of surface-sediment fossil assemblages, and compared the performance of salinity-inference models derived from them. We find that, despite ∼35% additional fossil loss, restriction to >150 μm data did not appreciably affect individual taxon optima or tolerances, and resulted in only a modest reduction of mean taxon richness per lake. Parameters of statistical model performance were as good, or better than those of models based on the >100 μm data, albeit only after excluding two atypically dilute (<100 μS/cm) lakes from the calibration. Application of inference models based on >150 μm or >100 μm data to a 200-year fossil record from Lake Abiyata, Ethiopia, produced very similar trends, amplitudes and uncertainty ranges of inferred past salinity change. Restriction to >150 μm data reduced the mean fossil yield of core samples by ∼20% on average, i.e. fossil loss was markedly lower than in surface-sediment samples. Using the larger mesh size reduced sample processing time by up to 50%, partly by removing a significant proportion of visually obstructive organic debris, and partly by allowing a greater fraction of chironomid fossils to be identified directly in the sorting tray. The fraction of 1st instar group taxa in surface-sediment samples was reduced from 13% to 3%, increasing the mean taxonomic resolution of fossil assemblages, and thus their ecological specificity.