External-source contamination during extraction—distillation in isotope-ratio analysis of soil inorganic nitrogen

The sources of contamination introduced during the extraction, distillation and drying phases of isotope-ratio analysis of soil inorganic nitrogen (ammonium and nitrite + nitrate) were identified, and the individual amounts of contaminants were quantified by isotope dilution. The procedure involves addition of internal standard solutions of ¹⁵N-labelled ammonium and nitrite to reagent blanks which are carried through each stage of the analysis at the same time as the test samples. Potassium chloride extractants, filter-papers, distillation reagents and atmospheric ammonia all contributed to dilution of the sample ¹⁵N. Some materials tested contained sufficient contaminants to cause large errors in the determination of sample ¹⁵N abundance. Both the amount and isotopic composition of contaminants can be determined by the isotope-dilution procedure, which permits the measured sample ¹⁵N abundance to be corrected for contamination.     

Catalyst contamination in the process of coal extract hydrogenation

The coke and mineral-matter deposition on NiMo/Al₂O₃ and NiCoMo/Al₂O₃ catalysts used in the process of coal extract hydrogenation is described.

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NiMo/Al₂O₃ NiCoMo/Al₂O₃, .

     

Radiocesium contamination in soil due to the Chernobyl accident

Three different cereal cultivated fields (rice, maize/wheat, wheat/barley) were selected and soil samples were collected in order to study the behaviour of the radiocesium deposited over the crops after the Chernobyl accident fall-out (April 1986) together with its distribution at different ground depths. For each field, soil samples were removed during the sowing (Oct–Nov '86), in Spring (Apr '87) and during the harvest time (Jun–Sept '87). The⁴⁰K concentration and stable potassium content in soil was also evaluated by nuclear spectrometry and by atomic absorption spectrometry. Beside soil sample measurements, the cultivated cereals produced in the 1986 harvest (rice, maize, wheat) were analyzed to evaluate the deposited contamination, and in order to evaluate the contamination during the growth and naturation we also analyzed whole plants (roots, stalks, grains) of the cultivated cereals (rice, wheat, barley) in 1987. Results are presented and discussed.     

Assessment of occupational exposure and contamination

In order to assess the elemental concentration level in a galvanizing industry and alert for the need to assess the outcome of a long-term exposure, scalp hair and toenail samples were used as bioindicators and the industry environment was evaluated through airborne particulate matter. The elemental concentration results have pointed out a high exposure to pollutant at workplaces and a high elemental concentration in biomonitors suggesting endogenous contamination. The majority of the elements determined in airborne particulate matter were also determined in hair and toenail samples. The results evidence the efficiency of these matrixes as biomonitors and the importance to carry out the airborne particulate matter sampling in parallel to these biomonitors mainly in occupational epidemiological studies.     

Study of contamination sources in the process of cryogenic grinding

The study of contamination effect during cryogenic grinding of pure cellulose was carried out. The optimisation of important parameters of the grinding process (pre-cooling time, grinding time, cooling time and number of cycles) was performed and the different sources of a possible contamination of samples (earlier processed sample, metal parts of grinding tool) were evaluated. The results of ICP-oa-TOF MS analysis after microwave digestion of cellulose samples were used in this study. Significant contamination of cellulose samples by Fe at the level 130 microg kg(-1) caused by wearing of steel stoppers and an impact bar was detected. Cross-contamination by Fe, Cr, Mn and Cu at the level 400, 200, 200 and 2100 microg kg(-1), respectively was caused by previous grinding of electro-waste sample. This cross-contamination was possible to be avoided by changing of a polycarbonate part of a grinding vessel.     

Evolution of products during the degradation of polyethylene in a batch reactor

The thermal degradation of two polyethylene samples (LDPE and HDPE) has been carried out in a batch reactor under dynamic conditions. The evolution of products generated after regular intervals of 5 min (temperature increments of approximately 25 °C) has been analyzed. The behaviour of LDPE and HDPE has been compared, and no differences in the quantity and weight fraction of the gaseous products obtained have been found. For both polymers, n-paraffins are the major products at the very beginning of the process, while as the decomposition proceeds 1-olefins are more abundant. The condensed fraction is much larger than the gaseous fraction and its analysis reveals some differences between the behaviour of LDPE and HDPE at the beginning of the degradation process. These differences disappear at higher temperatures where more similar trends are observed. 1-Olefins, n-paraffins, dienes and olefins with wide carbon number distributions are the most important condensed compounds obtained in the thermal degradation of both polyethylenes. The formation of 1-olefins and n-paraffins begins at slightly lower temperatures than for dienes and olefins. On the other hand, as the temperature increases, the amount of low and high molecular weight compounds increases at the expense of intermediate molecular weight products and the former become the most important by the end of the degradation process. This behaviour could be related to the thermal cracking of waxes through secondary reactions.     

Assessment of flavor volatiles of modified Iranian rice cultivars during the gelatinization process

A combined GC-MS with the headspace solid-phase microextraction (SPME) method has been employed for the analysis of the flavor volatiles of two modified Iranian rice cultivars during gelatinization. In order to optimize the different experimental parameters, the effect of fiber composition, water content of the rice samples, and equilibrium time were investigated. As a result, while gelatinization progresses, the amount of volatile compounds would increase as well. Therefore, a broad range of the flavor volatiles of rice could be extracted, concentrated, and identified. Altogether, 54 and 66 components were identified for HD5 and HD6 rice samples, respectively, of which 33 unique compounds were not detected previously. The identified volatile components in the modified cultivars belong to the chemical classes of aldehydes, ketones, alcohols, and heterocyclic compounds, phenolic compounds, and hydrocarbons.     

Energy characteristics of the process of air scrubbing from hydrocarbon contaminants in a barrier-discharge reactor

The electrical and chemical characteristics of air scrubbing, using a barrier discharge, from impurities of xylene, a typical organic contaminant, have been investigated. Based on the interrelation between the electrical and chemical characteristics, an approach to the optimization of the cleaning process has been proposed that allows a severalfold reduction of the energy input.     

Measurement of the neutron flux distribution in a research reactor by neutron activation analysis

Journal of Radioanalytical and Nuclear Chemistry - The neutron flux distribution in the core region of the JRTR was measured through the neutron activation analysis method. Sample mount and a tool...     

Development of a differential volume reactor system for soil biodegradation studies

Applied Biochemistry and Biotechnology - A bench scale experimental system was developed for the analysis of polycyclic aromatic hydrocarbon (PAH) degradation by mixed microbial cultures in PAH...     

Long-term monitoring of atrazine contamination in soil by ELISA

An enzyme-linked immunoassay (ELISA) was used for screening atrazine residues in soil. Samples were annually collected in Southern Germany between 1993 and 1998. An average of 419.5 samples was analyzed per year amounting to 2517 samples. The fraction of positive samples defined by atrazine concentrations >100 microg/kg soil decreased successively from 8% (corresponding to 33 samples) in 1993 to 0.6% (corresponding to 2 samples) in 1998. All positive samples and a selection of negative samples were subsequently validated by HPLC. Comparison of ELISA and HPLC data yielded correlation coefficient values of r = 0.958-0.981 (n = 18-47), except for 1995 when only a correlation of r = 0.864 (n = 18) was obtained. Four samples were overestimated and another 4 were underestimated with respect to the atrazine threshold value of 100 microg/kg soil as revealed by HPLC validation. Thus, 99.68% of 2,517 analyzed samples were correctly evaluated. The precision and reproducibility of the ELISA were adequate for a prescreening tool. The low cost per sample and the high sample throughput are not yet achievable by conventional analytical methods. The described combination of ELISA and HPLC has the potential to take advantage of both methods and to restrict determination errors to a minimum.     

Assessment of elemental contamination in road dust using EDXRF

Road dust samples were collected in different locations of heavy traffic, medium traffic, express way and industrial areas of Mumbai. The concentrations of various elements (Mg, Al, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn and Pb) in road dust samples were analyzed using EDXRF. The average elemental profile of road dust in Mumbai was comparable with studies carried out in other countries with slight variations. The estimated geo accumulation indices and enrichment factors indicated moderate elemental contamination and enrichment of anthropogenic elements in road dust samples. Factor analysis of elemental data resolved four sources namely crustal, tyre wear, vehicular/industrial emissions and break wear.     

Determination of actinide nuclides in water samples from the primary circuit of a research reactor

Primary coolant samples from a research have been analyzed for^239,240Pu,²³⁸Pu,²³⁸U,²³⁷Np and²³⁹Np. The determination of²³⁷Np and²³⁸U was carried out with the help of isotope dilution neutron activation analysis with²³⁹Np or²³⁸Np as tracer. For determination of^239,240Pu and²³⁸Pu alpha spectroscopic isotope dilution analysis with²³⁸Pu as tracer was used.²³⁹Np was determined with the help of isotope dilution analysis using²³⁸Np as tracer. Nuclides were isolated by chemical separation on anionite resin. Before measurement, Pu isotopes were electrolytically deposited on stainless steel plates. Activity ratios referred to²³⁸U were reported. They are helpful for identification of the sources of actinide activity in reactor effluents.     

Parameters of heterogenic liquid phase process and temperature profile in a displacement-type reactor

The results are presented of mathematical modeling the processes of heat and mass transfer in a displacement-type reactor.     

Continuous alcoholic fermentation process in a tower reactor with recycling of flocculating yeast

The influence of different substrate concentrations on the performance of a continuous system of alcohol prduction by fermentation using a tower reactor with recycling of flocculating yeasts was investigated. All experiments were carried out using a flocculating yeast strain IR-2, isolated from fermented food, and identified asSaccharomyces cerevisiae. Cane sugar juice was used as a substrate with sugar concentrations of 160, 170, 180, 190, and 200 g/L. Constant values of dilution rate, 0.20 h^?1, temperature, 30°C, and pH 3.3, were used. The performance of the reactor was observed to be efficient with high substrate concentrations. Maximum productivities of 18 g/L/h, 99% substrate conversion and ethanol concentrations of 90 g/L were obtained using 200 g/L of sugar in the feedstock. For substrate concentrations of 160 g/L, a maximum yield of 0.45 g of ethanol/g of sugar was observed or 90% of the theoretical value.

     

Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography-mass spectrometry

In order to reduce the amount of sample to be collected and the time consumed in the analytical process, a broad range of analytes should be preferably considered in the same analytical procedure. A suitable methodology for pesticide residue analysis in soil samples was developed based on ultrasonic extraction (USE) and gas chromatography–mass spectrometry (GC–MS). For this study, different classes of pesticides were selected, both recent and old persistent molecules: parent compounds and degradation products, namely organochlorine, organophosphorous and pyrethroid insecticides, triazine and acetanilide herbicides and other miscellaneous pesticides. Pesticide residues could be detected in the low- to sub-ppb range (0.05–7.0 μg kg⁻¹) with good precision (7.5–20.5%, average 13.7% R.S.D.) and extraction efficiency (69–118%, average 88%) for the great majority of analytes. This methodology has been applied in a monitoring program of soil samples from an intensive horticulture area in Póvoa de Varzim, North of Portugal. The pesticides detected in four sampling programs (2001/2002) were the following: lindane, dieldrin, endosulfan, endosulfan sulfate, 4,4′-DDE, 4,4′-DDD, atrazine, desethylatrazine, alachlor, dimethoate, chlorpyrifos, pendimethalin, procymidone and chlorfenvinphos. Pesticide contamination was investigated at three depths and in different soil and crop types to assess the influence of soil characteristics and trends over time.     

A method for the replacement of 137Cs with 40K as a non-hazardous radioactive tracer for open-source decommissioning research applications

The potential of ⁴⁰K as a radioactive tracer analogue of ¹³⁷Cs in ion exchange experiments is reported. Solutions of varying concentrations of potassium chloride (KCl) have been monitored radiometrically in a sodium iodide well-counter to determine the activity-concentration relationship. Ion exchange reactions using an exemplar ion exchange resin, KCl and non-radioactive caesium chloride (CsCl) solutions have been studied radiometrically. The adsorbed amounts of potassium and caesium are observed, inferred from displaced K⁺ ions, to be consistent with the total exchange capacity of the resin. Adsorption isotherm models have been applied to the experimental data, with the Freundlich isotherm observed to fit the data with the highest degree of consistency. The reported results indicate that decontamination techniques involving hazardous isotopes of anthropogenic origin such as ¹³⁷Cs can be developed, evaluated and optimised by substituting a chemically and physically similar non-hazardous radioactive isotope, in this case ⁴⁰K. This represents a means by which innovative decontamination techniques and regimes might be identified without the need to use ¹³⁷Cs and thus avoids additional generation of radioactive wastes.     

Comparative evaluation of organic contamination sources from roller and pencil type PVA brushes during the Post-CMP cleaning process

In post-CMP (chemical mechanical polishing) processing, the use of poly vinyl acetal (PVA) brushes to clean the wafer surface is one of the most effective and prominent techniques applied for the removal of CMP contaminants. Recently, organic contaminants induced in different types of PVA brushes during brush manufacturing have been drawing substantial research interest in CMP communities. In this study, investigated the root cause of these residual organic impurities in two different types of PVA brushes was investigated: roller and pencil type brushes. PVA roller brushes have a skin layer due to the brush molding process, but pencil-type PVA brushes do not have the skin layer. Extraction of organic impurities from both types of brushes was accomplished using an ultrasound-assisted technique at a sonication frequency of 40 kHz, and input power of 600 W. Further evaluation of these organic impurities using Field Emission Scanning Electron Microscopy (FE-SEM) revealed a large number of organic impurities in roller brushes and negligible impurities in pencil brushes. Time of flight secondary ion mass spectrometry (TOF-SIMS) analysis confirmed polydimethylsiloxane (PDMS) as the organic impurities extracted from PVA roller brushes, which were generated during the brush manufacturing process. The PDMS content in PVA roller brushes was further analyzed using FE-SEM micrographs via dissolving the organic impurities in tetramethylammonium hydroxide solution (TMAH). During brush fabrication, the high content of PDMS organic impurities in roller PVA brushes is essentially attributed to the presence of the additional skin layer formed by the mold releasing agent at the mold-cavity interface.     

Nuclear science and engineering education at a university research reactor

The role of an on-site irradiation facility in nuclear science and engineering education is examined. Using the example of a university research reactor, the use of such devices in laboratory instruction, public outreach programs, special instructional programs, research, etc. is discussed. Examples from the Oregon State University curriculum in nuclear chemistry, nuclear engineering and radiation health are given.     

Voltammetric determination of nitroaromatic and nitramine explosives contamination in soil

The contamination of soil by nitroaromatic and nitramine explosives is widespread during the manufacture, testing and disposal of explosives and ammunitions. The analysis for the presence of trace explosive contaminants in soil becomes important in the light of their effect on the growth of different varieties of plants and crops. 2,4,6-Trinitrotoluene (TNT), cyclotrimethylene trinitramine (Research Department explosive, RDX) and cyclotetramethylene tetranitramine (high melting point explosive, HMX), other related explosive compounds and their by-products must be monitored in soil and surrounding waterways since these are mutagenic, toxic and persistent pollutants that can leach from the contaminated soil to accumulate in the food chain. In this study, a voltammetric method has been developed for the determination of explosive such as RDX, HMX and TNT. The electrochemical redox behavior of RDX, HMX and TNT was studied through cyclic voltammetry and quantitative determination was carried out by using square wave voltammetry technique. Calibration curves were drawn and were linear in the range of 63-129 ppm for RDX with a detection limit of 10 ppm, 49-182 ppm for HMX with a detection limit of 1 ppm and 38-139 ppm for TNT with a detection limit of 1 ppm. This method was applied to determine the contaminations in several soil samples that yielded a relative error of 1% in the concentrations.