Ocena wpływu przygotowania próbek na uzyskiwane wyniki analiz pirolitycznych

Nafta-Gaz ◽  
2021 ◽  
Vol 77 (5) ◽  
pp. 299-312
Author(s):  
Marek Janiga ◽  
◽  
Małgorzata Kania ◽  
Agnieszka Wciślak ◽  
Karol Spunda ◽  
...  

The aim of the work, the results of which are presented in the article, was to evaluate the influence of the method of sample preparation on the results of pyrolytic analyses: RockEval, Py-GC-FID (gas chromatography with FID detector) and Py-GC-IRMS (isotope mass spectrometry with gas chromatography). Mortars and ball mills are most often used to grind the samples. Three rock samples with a higher organic carbon content (shales) and five with a lower organic carbon content (including two samples of dolomites and three of anhydrites) were prepared. The rocks were homogenized and divided into three parts. Each part was ground: by hand in a mortar, in a ball mill for 5 minutes, and in a ball mill for 15 minutes. A total of 24 RockEval analyses, 48 Py-GC-FID analyses (two pyrolysis temperatures corresponding to RockEval pyrolysis conditions) and 24 Py-GC-IRMS analyses were performed. The grinding of the samples for the RockEval analyses is insignificant. The differences in the results seem to indicate the influence of the analysis error and the nature of the sample. For the Py-GC-FID methodology, the influence of milling on the results of desorption carried out at the temperature of 300ºC for most of the tested samples can be considered insignificant and negligible. At the temperature of 500ºC, various types of samples show some correlations, but they are insufficient to reject one of the methods of sample preparation. Therefore, it is important to analyze the results comprehensively, taking into account both the group composition and the distribution of pyrolysis products. In the case of the isotopic composition analyses (Py-GC-IRMS), also no differences in δ13C values related to different types of grinding samples can be found. Summarizing, all the results show a negligible influence of the method of grinding the samples on the results of pyrolysis analyses. Nevertheless, it is important that only one method of sample preparation is used for a separate sample series.

2021 ◽  
Vol 54 (2A) ◽  
pp. 60-74
Author(s):  
Arwa M. S. Al-Dolaimy

A total of 56 cuttings samples of Sargelu and Kurrachine formations from different wells (Ain Zalah, Baiji, and Jabal Kand) in northern Iraq have been investigated in this study. Both the Sargelu and Kurrachine formations were examined using Rock-Eval pyrolysis to assess the richness of organic matter and thermal maturity level. The Sargelu Formation Have Total Organic Carbon wt.% ranged from 0.22–2.52 wt.%, average 1.26 wt.% in Ain Zalah Well, and between 0.57–8.90 wt.%, average 2.95 wt.% in Baiji Well, and between 0.81–11.80 wt.%, average 5.01wt.% in for Kand Well. It is considered a potential source rock based on total organic carbon content. total organic carbon wt. % in Ain Zalah and Kand in the Kurrachine Formation is considered poor source rock with a total organic carbon content of 0.17, 0.39 wt. %, respectively, while in Baiji Well is considered moderate source rock with total organic carbon content 0.53 wt. %. The Rock-Eval data are not always sufficient to define the kind of organic matter through the use of the van Krevelen diagram because HI and OI are affected by both matrix mineralogy and the kerogen mixture. For accurate assessments of the source rocks, gas chromatography has been relied on, which provides a direct indication of the kerogen type as well as the type of hydrocarbons that kerogen can generate during maturity. Gas chromatography analysis indicates that all selected samples contained type II kerogen. The highest value of the TAS/ (MAS+TAS) ratio was found in Ain Zalah samples (Sargelu Formation), and this result indicates the occurrence of an aromatization process with increasing thermal maturation.


2020 ◽  
Vol 22 (1) ◽  
pp. 113-122
Author(s):  
R. Alani ◽  
K. Olayinka ◽  
B. Alo

Contamination of Lagos soils with persistent, bioaccumulative and toxic micropollutants (PBTs) may not only affect the non-target species residing in the soil, but also raises the concern of the possibility of the chemicals finding their way into the Lagoon and other water courses via soil run-off and leaching. In this study, soil samples were collected from three busy areas of Lagos (Apapa, Okobaba and Iddo) and analyzed for Polychlorinated Biphenyls (PCBs), Organochlorine pesticides (OCS), and Polycyclic Aromatic Hydrocarbons (PAHs). Gas Chromatography with Mass Selective Detector (GC/MSD) was used for the analyses. Iddo had the highest percentage organic carbon content of 39.39% with highest total PAHs of 2,706.93 ng/g. The highest total PCBs of 23.63 ng/g was found at Apapa 3 which was one of the three sampling points in Apapa. PCB 74 was the onlyPCB found in all the soil samples and ranged between 3.55 ng/g and 23.64 ng/g at Apapa 1 and Apapa 2 respectively. High concentrations of the following organic compounds were also obtained at the following locations- naphthalene (1,625.10 ng/g) at Iddo; dichlorodiphenyldichloroethylene (p,p'DDE ), (117.98 ng/g) at Okobaba, and PCB 74 (23.63 ng/g) at Apapa 1. The results obtained showed that the higher the municipal activity, the higher the percentage organic carbon content. Key words: Bioaccumulative and toxic micropollutants, Gas chromatography/Mass selective detector, Persistent organic carbon, Soil organic pollutants


2021 ◽  
Vol 24 ◽  
pp. e00367
Author(s):  
Patrick Filippi ◽  
Stephen R. Cattle ◽  
Matthew J. Pringle ◽  
Thomas F.A. Bishop

Author(s):  
Emmanuelle Vaudour ◽  
Cécile Gomez ◽  
Philippe Lagacherie ◽  
Thomas Loiseau ◽  
Nicolas Baghdadi ◽  
...  

2021 ◽  
Author(s):  
Christoph Rosinger ◽  
Michael Bonkowski

AbstractFreeze–thaw (FT) events exert a great physiological stress on the soil microbial community and thus significantly impact soil biogeochemical processes. Studies often show ambiguous and contradicting results, because a multitude of environmental factors affect biogeochemical responses to FT. Thus, a better understanding of the factors driving and regulating microbial responses to FT events is required. Soil chronosequences allow more focused comparisons among soils with initially similar start conditions. We therefore exposed four soils with contrasting organic carbon contents and opposing soil age (i.e., years after restoration) from a postmining agricultural chronosequence to three consecutive FT events and evaluated soil biochgeoemical responses after thawing. The major microbial biomass carbon losses occurred after the first FT event, while microbial biomass N decreased more steadily with subsequent FT cycles. This led to an immediate and lasting decoupling of microbial biomass carbon:nitrogen stoichiometry. After the first FT event, basal respiration and the metabolic quotient (i.e., respiration per microbial biomass unit) were above pre-freezing values and thereafter decreased with subsequent FT cycles, demonstrating initially high dissimilatory carbon losses and less and less microbial metabolic activity with each iterative FT cycle. As a consequence, dissolved organic carbon and total dissolved nitrogen increased in soil solution after the first FT event, while a substantial part of the liberated nitrogen was likely lost through gaseous emissions. Overall, high-carbon soils were more vulnerable to microbial biomass losses than low-carbon soils. Surprisingly, soil age explained more variation in soil chemical and microbial responses than soil organic carbon content. Further studies are needed to dissect the factors associated with soil age and its influence on soil biochemical responses to FT events.


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