An assessment of chlorophyll preservation in lake sediments using multiple analytical techniques applied to the annually laminated lake sediments of Nylandssjön

Abstract Chlorophyll is frequently used as a proxy for autochthonous production in lakes. This use of chlorophyll concentrations in sediments to infer historical changes in lake primary production relies heavily on the assumption that preservation is sufficient to reflect the productivity in a meaningful way. In this study, we use a series of freeze cores from a lake with annually laminated sediments to assess how reliable down-core trends in chlorophyll are, and to what extent chlorophyll is degraded in the sediment. A striking consistency in the down-core chlorophyll trends in four sediment cores collected in different years (1983, 1992, 2002 and 2010) shows that the sediment preserves a consistent chlorophyll signal over longer timescales. However, there are also clear signs that diagenetic processes within the sediment affect the chlorophyll concentration in sediment layers younger than 10–15 years. This implies that care is needed when interpreting chlorophyll trends in recent sediments. Further, our data show that high-performance liquid chromatography (HPLC) and visible reflectance spectroscopy (VRS) detect similar chlorophyll concentrations for recently dried samples. A third analytical technique, pyrolysis–gas chromatography/mass spectrometry, which provides semi-quantitative values for chlorophyll, also produce a temporal trend that is highly correlated with data from the two quantitative techniques. For samples that have been stored dried at room temperature for several years there is, however, a large discrepancy between the two quantitative techniques. The VRS method is more robust with regards to degradation during storage, while HPLC results demonstrate clear storage effects.

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Application of a fractionation technique for better understanding of the removal of natural organic matter by alum coagulation

Water Science & Technology Water Supply ◽

10.2166/ws.2002.0200 ◽

2002 ◽

Vol 2 (5-6) ◽

pp. 427-433 ◽

Cited By ~ 4

Author(s):

J. van Leeuwen ◽

C. Chow ◽

R. Fabris ◽

N. Withers ◽

D. Page ◽

...

Keyword(s):

Organic Matter ◽

Natural Organic Matter ◽

High Performance ◽

Relative Proportion ◽

Water Source ◽

Size Exclusion ◽

Gas Chromatography Mass Spectrometry ◽

Pyrolysis Gas ◽

Alum Treatment ◽

Hydrophobic Acids

To gain an improved understanding of the types of organic compounds that are recalcitrant to water treatment, natural organic matter (NOM) isolates from two drinking water sources (Mt. Zero and Moorabool reservoirs, Victoria, Australia) were separated into fractions of distinct chemical behaviour using resins. Four fractions were obtained from each water source and were organics absorbed to: (1) XAD-8 (very hydrophobic acids, VHA); (2) DAX-4 (slightly hydrophobic acids, SHA); (3) bound to an anion exchange resin (charged organics, CHAR); and (4) not absorbed or bound to resins (neutrals, NEUT). These fractions were then tested to determine the capacity of alum to remove them from water and to correlate this with the character of each isolate. The fractions were characterised by the application of high performance size exclusion chromatography (HPSEC), bacterial regrowth potential (BRP), trihalomethane formation potential (THMFP), pyrolysis gas-chromatography mass spectrometry (Py-GC-MS) and thermochemolysis. The highest removals of dissolved organic carbon (DOC) by alum treatment were in waters spiked with the CHAR fractions while the NEUT fractions were the most recalcitrant. The number average molecular weights (Mn) of DOC of the CHAR fractions before treatment were the highest, whilst those of the NEUT fractions were the lowest. After alum treatment, the Mn of the NEUT fractions were only slightly reduced. Results from Py-GC-MS and thermochemolysis indicate that the NEUT fractions had the highest relative proportion of saccharide derived organic material. Nonetheless, the BRP of waters spiked with the NEUT fractions differed markedly, indicating that organics recalcitrant to alum treatment can vary substantially in their chemical composition and capacity to support microbial growth.

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Organic Matter Composition of Manure and Its Potential Impact on Plant Growth

Sustainability ◽

10.3390/su11082346 ◽

2019 ◽

Vol 11 (8) ◽

pp. 2346 ◽

Cited By ~ 4

Author(s):

Jongkwan Park ◽

Kyung Hwa Cho ◽

Mayzonee Ligaray ◽

Mi-Jin Choi

Keyword(s):

Plant Growth ◽

Chlorophyll Concentration ◽

Three Dimensional ◽

Poultry Manure ◽

Molecular Composition ◽

Growth Potential ◽

Gas Chromatography Mass Spectrometry ◽

Pyrolysis Gas ◽

Nutrient Contents ◽

Positive Effects

Since the advent of flush toilet systems, the aquatic environment has received a massive contaminant flow. Furthermore, the perception of human feces has changed from a useful nutrient source for agriculture to a harmful contaminant. In this study, we compared the nutritional quality of five samples: (1) human manure (HM), (2) human manure from a family mainly eating organic food (HMO), (3) cow manure (CM), (4) poultry manure (PM), and (5) commercial nursery media (CNM). Samples were analyzed in terms of organic and inorganic nutrient contents, molecular composition, seed germination, and chlorophyll concentration. Pyrolysis gas chromatography/mass spectrometry (GC/MS) was used to describe the differences in molecular composition. Three-dimensional excitation and emission matrix fluorescence spectroscopy characterized the organic composition of water extracts. From the results, CNM, PM, and HMO showed humic- and fluvic-like substance peaks, the highest values of potassium and sulfate ions, and of C/N ratios, indicating greater plant growth potential. This was confirmed by their higher chlorophyll concentrations and germination index values. These results contribute knowledge about the positive effects of manure, changing the negative perception of human excreta from waste to resource. This work provides a reference for reducing the wastewater loading rate in society.

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Recognition of natural silk fibers, dyes and metal threads of historical Romanian textile fragments using the multi-analytical techniques approach

Textile Research Journal ◽

10.1177/0040517519898827 ◽

2020 ◽

Vol 90 (15-16) ◽

pp. 1671-1688

Author(s):

Nidal Al-Sharairi ◽

Irina Crina Anca Sandu ◽

Viorica Vasilache ◽

Ion Sandu

Keyword(s):

High Performance ◽

Fiber Type ◽

Analytical Techniques ◽

Attenuated Total Reflectance ◽

Fiber Structure ◽

Silk Fibers ◽

X Ray ◽

Analytical Technique ◽

Combined Use ◽

Initial Idea

A multi-analytical technique approach involving the combined use of micro-invasive and nondestructive techniques was used to identify the type of fiber, mordant and natural dye constituents for eight historical textiles fragments from the 17th–18th centuries, found in monasteries in Northern Romania. The analysis was performed using optical microscopy (OM), scanning electron microscopy with an energy-dispersive X-ray detector (SEM-EDX), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) and high-performance liquid chromatography (HPLC). HPLC could determine two flavonol-based structure yellow dyes (possibly weld and Persian berries), one naphthoquinone-based structure brown dye (juglone-walnut) and five samples composed of anthraquinone-based structure red dyes (two fragments contain kermes, one cochineal, one lac and one madder). Elemental analysis using EDX was utilized to identify the possible using of alum as a mordant and the use of metallic threads (pure silver and gilt threads). OM and SEM techniques identified the fiber type and the existence of metal threads, while ATR-FTIR analysis could provide an initial idea about the functional groups of the textile components for the fiber structure substrates.

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Critical Assessment of Analytical Methods for the Harmonized and Cost-Efficient Analysis of Microplastics

Applied Spectroscopy ◽

10.1177/0003702820921465 ◽

2020 ◽

Vol 74 (9) ◽

pp. 1012-1047 ◽

Cited By ~ 15

Author(s):

Sebastian Primpke ◽

Silke H. Christiansen ◽

Win Cowger ◽

Hannah De Frond ◽

Ashok Deshpande ◽

...

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Analytical Techniques ◽

Field Work ◽

Gas Chromatography Mass Spectrometry ◽

Pyrolysis Gas ◽

Combined Application ◽

Chromatography Mass Spectrometry ◽

Recent Developments ◽

Cost Efficient

Microplastics are of major concerns for society and is currently in the focus of legislators and administrations. A small number of measures to reduce or remove primary sources of microplastics to the environment are currently coming into effect. At the moment, they have not yet tackled important topics such as food safety. However, recent developments such as the 2018 bill in California are requesting the analysis of microplastics in drinking water by standardized operational protocols. Administrations and analytical labs are facing an emerging field of methods for sampling, extraction, and analysis of microplastics, which complicate the establishment of standardized operational protocols. In this review, the state of the currently applied identification and quantification tools for microplastics are evaluated providing a harmonized guideline for future standardized operational protocols to cover these types of bills. The main focus is on the naked eye detection, general optical microscopy, the application of dye staining, flow cytometry, Fourier transform infrared spectroscopy (FT-Ir) and microscopy, Raman spectroscopy and microscopy, thermal degradation by pyrolysis–gas chromatography–mass spectrometry (py-GC-MS) as well as thermo-extraction and desorption gas chromatography–mass spectrometry (TED-GC-MS). Additional techniques are highlighted as well as the combined application of the analytical techniques suggested. An outlook is given on the emerging aspect of nanoplastic analysis. In all cases, the methods were screened for limitations, field work abilities and, if possible, estimated costs and summarized into a recommendation for a workflow covering the demands of society, legislation, and administration in cost efficient but still detailed manner.

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Multi-analytical techniques in characterization and identification of Chinese historical rubbings

10.21203/rs.3.rs-314543/v1 ◽

2021 ◽

Author(s):

Na Yao ◽

Xiangsheng Zhan ◽

Qinglin Ma ◽

Shuya Wei

Keyword(s):

Aromatic Hydrocarbons ◽

Staining Method ◽

Analytical Techniques ◽

Gas Chromatography Mass Spectrometry ◽

Pyrolysis Gas ◽

Scientific Support ◽

Biochemical Compounds ◽

Polycyclic Aromatic ◽

Marker Compounds ◽

Conifer Wood

Abstract For authenticity and conservation purposes, the precious historical rubbings preserved in Wuyuan Museum were studied by multi-analytical techniques including Pyrolysis gas chromatography-mass spectrometry (Py-GC/MS), SEM-EDS and Herzberg staining method. Through Py-GC/MS analyses, five types of constituents could be detected: (1) polycyclic aromatic hydrocarbons from soot; (2) retene and methyl dehydroabietate from tar of conifer wood; (3) marker compounds of egg; (4) additives of menthol and curcumene compounds; (5) biochemical compounds of bark paper. Based on this analytical results, the ink type, binding media and additives in the ink, as well as the fiber origin source of the rubbing paper could be concluded. The materials information of the rubbings obtained through this study could not only provide evidence for its authenticity, but also supply scientific support for its conservation and restoration.

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Pyrolysis gas chromatography - mass spectrometry of humic substances extracted from Canadian lake sediments

Canadian Journal of Chemistry ◽

10.1139/v99-228 ◽

2000 ◽

Vol 78 (1) ◽

pp. 51-63 ◽

Cited By ~ 4

Author(s):

Helen A Joly ◽

Hongbo Li ◽

Nelson Belzile

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Humic Acid ◽

Lake Sediments ◽

Humic Substances ◽

Gas Chromatography Mass Spectrometry ◽

Pyrolysis Gas ◽

Pyrolysis Products ◽

Pyrolysis Gas Chromatography ◽

Chromatography Mass Spectrometry

Humic substances (HS) were extracted with the aid of 0.1 M Na4P2O7 and 0.5 M NaOH solutions from the sediments of four lakes located in the Sudbury area in Ontario, Canada, namely, Tilton, Clearwater, Silver and Ramsey Lake. The humic acid (HA) and fulvic acid (FA) extracts, purified and characterized using classical methods i.e., elemental analysis, FTIR spectroscopy, and CPMAS 13C NMR (see N. Belzile, H.A. Joly, and H. Li. (1997)), were submitted to pyrolysis - gas chromatography - mass spectrometry (Py-GC-MS). The pyrolysates of the HA and FA extracts were found to be complex mixtures of at least 200 compounds. Results based on statistical analysis of the abundances of pyrolysis products (of known origin) revealed trends similar to those obtained from the classical bulk characterization techniques. The Py-GC-MS technique supported the observation, obtained from classical methods, that the chemical composition of HA extracts varied less significantly among the four lake sediments than for the FA extracts. The abundances of lignin and carbohydrate pyrolysates showed the highest variation among the FA extracts. Pyrolysis products originating from lignin, carbohydrates, proteins, and fatty acids were identified. Key words: humic substances, humic acid, fulvic acid, pyrolysis, pyrolysis gas chromatography mass spectrometry, lake sediments.

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Anthropogenic Influence on the 14C Activity and Other Constituents of Recent Lake Sediments: A Case Study1

Radiocarbon ◽

10.1017/s0033822200063864 ◽

1992 ◽

Vol 34 (3) ◽

pp. 585-592 ◽

Cited By ~ 16

Author(s):

Dušan Srdoč ◽

Nada Horvatinčić ◽

Marijan Ahel ◽

Walter Giger ◽

Christian Schaffner ◽

...

Keyword(s):

Lake Sediments ◽

Anthropogenic Activities ◽

Sediment Cores ◽

Gas Chromatography Mass Spectrometry ◽

Computer Assisted ◽

Sudden Increase ◽

Recent Sediment ◽

Activity Measurements ◽

Oligotrophic Water ◽

Excessive Nutrients

Anthropogenic activities that introduce an excess of nutrients and other pollutants into rivers and lakes are causing significant changes in their aquatic environment. Excessive nutrients greatly accelerate eutrophication, and lake marl formed during eutrophication differs from that formed in oligotrophic water.We analyzed recent sediment cores from Prošće and Kozjak lakes located in Plitvice National Park, central Croatia. Analyses consisted of 14C activity of calcareous lake marl, the ratio of stable isotopes (δ13C, δ18O), organic compounds in the sediment and the distribution of diatoms. Previous 14C activity measurements helped to determine the sedimentation rate and thus the time period of increased input of nutrients into lakes. We determined the increased 14C activity in lake sediments caused by nuclear bomb effect in recent depth profiles. We attributed the sudden increase in diatom species, Cyclotella operculata unipuctata and Achnanthes clevei rostrata, in the uppermost 5-cm layer, to eutrophication of the lake water.We performed a molecular characterization of hydrocarbons isolated from the sediments, and applied computer-assisted high-resolution gas chromatography/mass spectrometry to estimate contributions of biogenic, fossil and pyrolytic hydrocarbons.

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Analysis of Intact Glycosidic Aroma Precursors in Grapes by High-Performance Liquid Chromatography with a Diode Array Detector

Foods ◽

10.3390/foods10010191 ◽

2021 ◽

Vol 10 (1) ◽

pp. 191

Author(s):

Cristina Cebrián-Tarancón ◽

José Oliva ◽

Miguel Ángel Cámara ◽

Gonzalo L. Alonso ◽

M. Rosario Salinas

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Solid Phase ◽

Analytical Techniques ◽

Array Detector ◽

Diode Array ◽

Diode Array Detector ◽

Analytical Technique ◽

Aroma Precursors

Nowadays, the techniques for the analysis of glycosidic precursors in grapes involve changes in the glycoside structure or it is necessary the use of very expensive analytical techniques. In this study, we describe for the first time an approach to analyse intact glycosidic aroma precursors in grapes by high-performance liquid chromatography with a diode array detector (HPLC-DAD), a simple and cheap analytical technique that could be used in wineries. Briefly, the skin of Muscat of Alexandria grapes was extracted using a microwave and purified using solid-phase extraction combining Oasis MCX and LiChrolut EN cartridges. In total, 20 compounds were selected by HPLC-DAD at 195 nm and taking as a reference the spectrum of phenyl β-D-glucopyranoside, whose DAD spectrum showed a first shoulder from 190 to 230 nm and a second around 200–360 nm. After that, these glycosidic compounds were identified by High-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (HPLC-qTOF-MS). Disaccharides hexose pentose were the most abundant group observed with respect to the sugars and monoterpendiols the main aglycones found.

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Unmasking a wild man: scientific analysis of Bertoldo di Giovanni’s Shield Bearer in The Frick Collection

Heritage Science ◽

10.1186/s40494-020-00453-5 ◽

2020 ◽

Vol 8 (1) ◽

Author(s):

Elena Basso ◽

Federica Pozzi ◽

Julia Day ◽

Linda Borsch

Keyword(s):

New York ◽

Current Knowledge ◽

Analytical Techniques ◽

Gas Chromatography Mass Spectrometry ◽

Italian Renaissance ◽

Pyrolysis Gas ◽

X Ray ◽

Select Group ◽

Scientific Analysis ◽

Wild Man

Abstract Bertoldo di Giovanni (ca. 1440–1491) was the primary sculptor and medal worker for Lorenzo the Magnificent (1449–1492). Despite being one of the most prominent Italian Renaissance artists working in Florence, little is known about his workshop and practice. The Frick Collection, New York, owns a Shield Bearer, one of a small number of bronze statuettes attributed to Bertoldo predominantly based on stylistic grounds. This article presents the results obtained from the scientific analysis of The Frick statuette, including a detailed technical characterization of the casting alloy, gilding, solder, organic coatings, and other later alterations. An array of analytical techniques was employed, including X-radiography, micro- and portable X-ray fluorescence (μXRF and pXRF) spectroscopies, scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM/EDS), Raman and Fourier-transform infrared (FTIR) spectroscopies, and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). This work supported a larger technical study of Bertoldo’s statuettes and reliefs related to an exhibition organized by The Frick, which brought together a select group of medals, as well as eleven bronzes ascribed to the artist, including the museum’s statuette. Close collaboration between conservators, curators, and scientists was critical throughout the study of the Shield Bearer, which also included extensive visual examination of the object in order to understand details of manufacture, identify sampling sites, and interpret the collected data. This study confirmed that The Frick figure was cast from the same brass alloy as a second very similar Shield Bearer in the Liechtenstein Collection, Vienna, suggesting that the two are a pendant pair that was likely cast simultaneously. In addition, analysis supported the assertion that the copper base on The Frick sculpture is original and assisted in identifying later alterations in both works. This focused research has expanded the current knowledge of the sculptor’s materials and methods, enabling scholars to better contextualize his artistic production within the framework of Italian Renaissance sculpture.

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The Cinderella story of metabolic profiling: does metabolomics get to go to the functional genomics ball?

Philosophical Transactions of the Royal Society B Biological Sciences ◽

10.1098/rstb.2005.1734 ◽

2005 ◽

Vol 361 (1465) ◽

pp. 147-161 ◽

Cited By ~ 104

Author(s):

Julian L Griffin

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Functional Genomics ◽

High Performance ◽

Analytical Techniques ◽

Disease Diagnosis ◽

Gas Chromatography Mass Spectrometry ◽

Human Populations ◽

Chromatography Mass Spectrometry ◽

The Impact

To date most global approaches to functional genomics have centred on genomics, transcriptomics and proteomics. However, since a number of high-profile publications, interest in metabolomics, the global profiling of metabolites in a cell, tissue or organism, has been rapidly increasing. A range of analytical techniques, including 1 H NMR spectroscopy, gas chromatography–mass spectrometry (GC–MS), liquid chromatography–mass spectrometry (LC–MS), Fourier Transform mass spectrometry (FT–MS), high performance liquid chromatography (HPLC) and electrochemical array (EC-array), are required in order to maximize the number of metabolites that can be identified in a matrix. Applications have included phenotyping of yeast, mice and plants, understanding drug toxicity in pharmaceutical drug safety assessment, monitoring tumour treatment regimes and disease diagnosis in human populations. These successes are likely to be built on as other analytical and bioinformatic approaches are developed to fully exploit the information obtained in metabolic profiles. To assist in this process, databases of metabolomic data will be necessary to allow the passage of information between laboratories. In this prospective review, the capabilities of metabolomics in the field of medicine will be assessed in an attempt to predict the impact this ‘Cinderella approach’ will have at the ‘functional genomic ball’.

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