Effect of ultrasonic agitation on the release of copper, iron, manganese and zinc from soil and sediment using the BCR three-stage sequential extraction

An ultrasonic bath and an ultrasonic probe have been used to develop rapid versions of the three-stage Community Bureau of Reference (BCR, now the Standards, Measurement and Testing Programme) sequential extraction procedure. The effect of the ultrasonic treatments on the extraction of copper, iron, manganese and zinc from a sewage sludge-amended soil has been assessed. Recoveries similar to those of conventional shaking (i.e., conventional value, +/- 30%) could generally be obtained for copper, manganese and zinc, but not for the important matrix element iron. With the use of compromise sonication conditions, steps 1, 2 and 3 of the sequential extraction (excluding the hydrogen peroxide digestion in step 3, which was not performed with sonication) could be completed in 3, 5 and 1 min, respectively, using the ultrasonic probe, and in 3, 1 and 1 h, respectively, using the bath. The extraction procedures developed using the soil performed well when applied to lake sediment BCR CRM 601. Analyte partitioning was generally similar to that obtained with mechanical shaking, and overall metal recoveries were 84-98% of those obtained with the conventional BCR protocol, except for copper extracted with the probe (74%). Poorer performance (analyte recoveries, 58-104%) was obtained when the methods were applied to an intertidal sediment. This highlights the difficulty of developing a version of the BCR extraction, with ultrasonic assistance, which gives a performance equivalent to conventional shaking when applied to different substrates.     

Antimony speciation in terrestrial plants. Comparative studies on extraction methods

A suitable method for the extraction of antimony species from plant materials prior to IC-HG-AFS analysis is presented. The extraction efficiency with different extraction systems using various aqueous and aqueous/solvent mixtures was initially evaluated by analysing the Virginia Tobacco Leaves Certified Reference Material. The concentration of antimony extracted was compared with the total antimony content in the plant material measured by HG-AFS after focused microwave-acidic digestion using HNO3 and H2O2. The proposed extraction procedures were applied to antimony speciation in several plants from a natural terrestrial environment impacted by mining activities. End-over-end agitation (4 h) followed by sonication (1 h) extraction using 0.1 mol l(-1) citric acid was found to provide the best extraction efficiency while also giving reliable speciation information. Both inorganic and methylantimony species were found in the extractable portion of some terrestrial plants.     

Airborne exposure to wheat allergens: optimised elution for airborne dust samples

Well-validated methods for measuring airborne occupational allergens are essential for effective control and reduction of allergen exposures. For wheat flour allergens, specific immunoassays are available, but there is a need for optimisation and standardization of sample processing procedures. Wheat flour allergen elution and storage were studied using airborne dust samples collected in bakeries with a new parallel sampler. Forty-eight series of 9 parallel filters were subjected to extraction procedures varying in elution medium, shaking method, extraction vial, and centrifugation speed. Wheat allergens were measured with enzyme immunoassays, and the effect of various procedures evaluated by mixed regression analyses. The stability of the eluted allergens was assessed after storage for 20 days and 4 months at -20 degrees C, in the presence or absence of casein in the medium. Only the type of elution medium had significant effects on allergen recovery: addition of Tween-20 resulted in 3- to 100-fold increased levels, an effect that was most pronounced at low concentrations. Allergen levels in extracts were stable for at least 4 months at -20 degrees C, irrespective of the presence of casein in the medium. Addition of Tween-20 to the elution medium is essential for optimal extraction of wheat allergen. The recommended procedure further includes the use of conventional polystyrene tubes, simple shaking methods, and centrifugation after extraction. Wheat dust extracts in PBS-Tween can be stored frozen for at least 4 months, and addition of a stabilising protein is not required.     

Regional assessment of ozone sensitive tree species using bioindicator plants

Tropospheric ozone occurs at phytotoxic levels in the northeastern and mid-Atlantic regions of the United States. Quantifying possible regional-scale impacts of ambient ozone onforest tree species is difficult and is confounded by other factors, such as moisture and light, which influence the uptake of ozone by plants. Biomonitoring provides an approach to document direct foliar injury irrespective of direct measure ofozone uptake. We used bioindicator and field plot data from theUSDA Forest Service to identify tree species likely to exhibit regional-scale ozone impacts. Approximately 24% of sampled sweetgum (Liquidambar styraciflua), 15% of sampled loblollypine (Pinus taeda), and 12% of sampled black cherry (Prunus serotina) trees were in the highest risk category. Sweetgum and loblolly pine trees were at risk on the coastal plain of Maryland, Virginia and Delaware. Black cherry trees were at riskon the Allegheny Plateau (Pennsylvania), in the Allegheny Mountains (Pennsylvania, West Virginia, and Maryland) as well ascoastal plain areas of Maryland and Virginia. Our findings indicate a need for more in-depth study of actual impacts on growth and reproduction of these three species.     

Concentrations of Arsenic, Cadmium, Copper, Lead, Selenium, and Zinc in Fish from the Mississippi River Basin, 1995

Fish were collected in late 1995 from 34 National Contaminant Biomonitoring Program (NCBP) stations and 12 National Water Quality Assessment Program (NAWQA) stations in the Mississippi River basin (MRB), and in late 1996 from a reference site in West Virginia. The NCBP sites represented key points (dams, tributaries, etc.) in the largest rivers of the MRB. The NAWQA sites were typically on smaller rivers and were selected to represent dominant land uses in their watersheds. The West Virginia site, which is in an Eastern U.S. watershed adjacent to the MRB, was selected to document elemental concentrations in fish used for other aspects of a larger study and to provide additional contemporaneous data on background elemental concentrations. At each site four samples, each comprising (nominally) 10 adult common carp (Cyprinus carpio, 'carp') or black bass (Micropterus spp., 'bass') of the same sex, were collected. The whole fish were composited by station, species, and gender for analysis of arsenic (As), lead (Pb), and selenium (Se) by atomic absorption spectroscopy and for cadmium (Cd), copper (Cu), and zinc (Zn) by inductively-coupled plasma emission spectroscopy. Concentrations of most of the elements examined were lower in both carp and bass from the reference site, a small impoundment located in a rural area, than from the NCBP and NAWQA sites on rivers and larger impoundments. In contrast, there were few overall differences between NCBP sites NAWQA sites. The 1995 results generally confirmed the continued weathering and re-distribution of these elemental contaminants in the MRB; concentrations declined or were unchanged from 1984-1986 to 1995 at most NCBP sites, thus continuing two-decade trends. Exceptions were Se at Station 77 (Arkansas R. at John Martin Reservoir, CO), where concentrations have been elevated historically and increased slightly (to 3.8-4.7 microg g-(1) in bass and carp); and Pb, Cd, and Zn at Station 67 (Allegheny R. at Natrona, PA), where levels of these metals were high in the past and increased from 1986 to 1995.     

大气颗粒物中多环芳烃的索氏提取研究

通过对大气颗粒物中多环芳烃的索氏提取过程中的不同阶段的提取液中多环芳烃的分析 ,绘制了索氏提取曲线 ,发现提取效率主要取决于提取循环次数 ,而与提取浸泡时间关系不大。通过比较 1 1种提取液对加标参考物和实验参考物的索氏提取效率 ,发现常用的环己烷、苯等提取液提取效率很低。提取能力的序列为喹啉 乙醇 >吡啶 乙醇 >丙酮>乙醇 >二氯甲烷 >苯 >环己烷 >石油醚 >丙酮 乙醇 环己烷 >氯仿 >四氢呋喃。     

The extraction of aged polycyclic aromatic hydrocarbon (PAH) residues from a clay soil using sonication and a Soxhlet procedure: a comparative study

A sonication method was compared with Soxhlet extraction for recovering polycyclic aromatic hydrocarbons (PAH) from a clay soil that had been contaminated with tar materials for several decades. Using sonication over an 8 h extraction period, maximum extraction of the 16 US EPA priority PAH was obtained with dichloromethane (DCM)-acetone (1 + 1). The same procedure using hexane-acetone (1 + 1) recovered 86% of that obtained using DCM-acetone (1 + 1). PAH recovery was dependent on time of extraction up to a period of 8 h. The sonication procedure showed that individual PAH are extracted at differing rates depending on the number of fused rings in the molecule. Soxhlet extraction [with DCM-acetone (1 + 1)] over an 8 h period recovered 95% of the PAH removed by the sonication procedure using DCM-acetone (1 + 1), indicating that rigorous sonication can achieve PAH recoveries similar to those obtained by Soxhlet extraction. The lower recovery with the Soxhlet extraction was explained by the observed losses of the volatile PAH components after 1-4 h of extraction. The type of solvent used, the length of time of extraction and extraction method influenced the quantification of PAH in the soil. Therefore, the study has implications for PAH analyses in soils and sediments, and particularly for contaminated site assessments where the data from commercial laboratories are being used. The study emphasizes the importance of establishing (and being consistent in the application of) a vigorous extraction, particularly for commercial laboratories that handle samples of soil in batches (at different times) from a single site investigation or remediation process. The strong binding of PAH to soil, forming aged residues, has significant implications for extraction efficiency. This paper illustrates the problem of the underestimation of PAH using the US EPA method 3550, specifically where a surrogate spike is routinely employed and the efficiency of the extraction procedure for aged residues is unknown. The implications of this study for environmental monitoring, particularly where numerous batches of samples from a single site assessment or remediation program are submitted to commercial laboratories, is that it would be advisable for these laboratories to check their existing method's extraction efficiencies by conducting a time course sonication extraction on their particular soil to determine the optimum extraction time.     

Characteristics of aerosol types during large-scale transport of air pollution over the Yellow Sea region and at Cheongwon,Korea, in 2008

Episodes of large-scale transport of airborne dust and anthropogenic pollutant particles from different sources in the East Asian continent in 2008 were identified by National Oceanic and Atmospheric Administration satellite RGB (red, green, and blue)-composite images and the mass concentrations of ground level particulate matter. These particles were divided into dust, sea salt, smoke plume, and sulfate by an aerosol classification algorithm. To analyze the aerosol size distribution during large-scale transport of atmospheric aerosols, aerosol optical depth (AOD) and fine aerosol weighting (FW) of moderate imaging spectroradiometer aerosol products were used over the East Asian region. Six episodes of massive airborne dust particles, originating from sandstorms in northern China, Mongolia, and the Loess Plateau of China, were observed at Cheongwon. Classified dust aerosol types were distributed on a large-scale over the Yellow Sea region. The average PM10 and PM2.5 ratio to the total mass concentration TSP were 70% and 15%, respectively. However, the mass concentration of PM2.5 among TSP increased to as high as 23% in an episode where dust traveled in by way of an industrial area in eastern China. In the other five episodes of anthropogenic pollutant particles that flowed into the Korean Peninsula from eastern China, the anthropogenic pollutant particles were largely detected in the form of smoke over the Yellow Sea region. The average PM10 and PM2.5 ratios to TSP were 82% and 65%, respectively. The ratio of PM2.5 mass concentrations among TSP varied significantly depending on the origin and pathway of the airborne dust particles. The average AOD for the large-scale transport of anthropogenic pollutant particles in the East Asian region was measured to be 0.42 ± 0.17, which is higher in terms of the rate against atmospheric aerosols as compared with the AOD (0.36 ± 0.13) for airborne dust particles with sandstorms. In particular, the region ranging from eastern China, the Yellow Sea, and the Korean Peninsula to the Korea East Sea was characterized by high AOD distributions. In the episode of anthropogenic polluted aerosols, FW averaged 0.63 ± 0.16, a value higher than that in the episode of airborne dust particles (0.52 ± 0.13) with sandstorms, showing that fine anthropogenic pollutant particles contribute greatly to atmospheric aerosols in East Asia.     

Methodology for identifying particle sources in indoor environments

Growing concern about airborne particles in indoor environments requires fast source identification in order to apply remedial actions. A methodology for identifying sources emitting particles larger than 0.5 microm was designed and applied. It includes: (1) visual inspection of interior surfaces in order to identify deposited particles and inspection of potential sources (equipment, materials, activities etc.) of airborne particles. (2) Technical measurements of airborne particles at different positions in a building with simultaneous logging of activities. (3) Isolating potential activities/particle sources in a test chamber, initially free from particles, for controlled characterizations of the particles generated. The methodology was applied in a study of three houses in southern Sweden. The results show that source identification is facilitated by knowledge of concentration variations between different rooms, real-time measurements together with activity reports and information on particle characteristics that are comparable with results from laboratory simulations. In the houses to which the methodology was applied, major particle emissions from textile handling were identified, which were likely due to detergent zeolite residues.     

Characterisation of airborne particles collected within and proximal to an opencast coalmine: South Wales,U.K

Airborne particulate matter has been collected from within,and proximal to, an opencast coal mine in south Wales. Thiswork forms the first part of a three year project to collectand characterise, then determine the possible toxicology ofairborne particles in the south Wales region. High-resolutionField Emission SEM has shown that the coal mine dusts consistlargely of an assemblage of mineral grains and vehicle exhaustparticles. SEM-EDX has shown that the mineralogical make-up ofthe PM10 is complex, heterogeneous, and constantly changing.These findings are supported by analytical TEM-EPXMA.However, patterns can be determined relating the mineralogicalcomposition of the airborne particles to collection locationsand mining activities within the opencast. At our studyopencast, Park Slip West, quartz, which has known healtheffects, never exceeded 30% of the total collection mass, andaverage levels were much less. Vehicle exhaust emissions wasthe largest source in terms of particle numbers. The mass ofairborne particulate matter within the pit averagedapproximately twice that of outside the pit: importantlyhowever, this higher mass was due to relatively large, andnon-respirable, mineral grains. This study demonstrates that the physicochemical andmineralogical characterisation of airborne particles frommining and quarrying is essential to quantify the respirablefraction, and to identify potentially hazardous componentswithin the PM10.     

微囊藻中叶绿素a提取方法的优化

用组织研磨、浸泡提取、热浴超声3种提取方法和丙酮、甲醇、乙醇3种提取溶剂，从实验室纯培养微囊藻中提取叶绿素a，并以高效液相色谱法测定其质量浓度。结果表明，经组织研磨破碎藻细胞后用甲醇提取的效果好于丙酮和乙醇，经浸泡和超声破碎藻细胞后用乙醇的提取效果好于丙酮和甲醇；使用乙醇-热浴超声法在所有的试验组合中获得最佳提取效果，条件为：乙醇温度为50℃-55℃，超声6min-8min后再静置提取5h-6h。     

Particle emission from heavy-duty engine fuelled with blended diesel and biodiesel

In this study, particulate matter (PM) were characterized from a place impacted by heavy-duty vehicles (Bus Station) fuelled with diesel/biodiesel fuel blend (B3) in the city of Londrina, Brazil. Sixteen priority polycyclic aromatic hydrocarbons (PAH) concentrations were analyzed in the samples by their association with atmospheric PM, mass size distributions and major ions (fluorite, chloride, bromide, nitrate, phosphate, sulfate, nitrite, oxalate; fumarate, formate, succinate and acetate; lithium, sodium, potassium, magnesium, calcium and ammonium). Results indicate that major ions represented 21.2% particulate matter mass. Nitrate, sulfate, and ammonium, respectively, presented the highest concentration levels, indicating that biodiesel may also be a significant source for these ions, especially nitrate. Dibenzo[a,h]anthracene and indeno[1,2,3,-cd]pyrene were the main PAH found, and a higher fraction of PAH particles was found in diameters lower than 0.25 μm in Londrina bus station. The fine and ultrafine particles were dominant among the PM evaluated, suggesting that biodiesel decreases the total PAH emission. However, it does also increase the fraction of fine and ultrafine particles when compared to diesel.     

Coal-Mine Hollow Fill and Settling Pond Influences on Headwater Streams in Southern West Virginia, USA

The influences of coal-mine hollow fills and associated settling ponds in three headwater streams were assessed in southern West Virginia, USA. Fill drainage waters had elevated conductivities and metal concentrations, compared to a regional reference. Benthic macroinvertebrate richness was not affected consistently by the hollow fill drainages, relative to a regional reference, although a more tolerant community, lacking in Ephemeroptera taxa at most locations, was evident. Collector-filterer populations were elevated at monitoring stations directly below the settling ponds, indicating that the ponds’ presence influenced macroinvertebrate community structure by means of organic enrichment. Corbicula fluminea growth was enhanced in monitoring locations directly below the settling ponds, also an apparent result of organic enrichment. Results of acute water column toxicity testing with Ceriodaphnia dubia, sediment chronic toxicity testing with Daphnia magna, and in-situ ecotoxicological assessments with C. fluminea demonstrated no mortality or toxic influence at most of the sites tested below the ponds. The settling ponds appear to serve as sinks in collecting some, but not all, trace metals.     

Evaluation of performance of time-saving extraction devices in the BCR three-step sequential extraction procedure

Two alternative extraction methods--a routine ultrasonic bath and a microwave oven--were developed and optimized for their eventual exploitation in the three-stage sequential extraction procedure proposed by the European Standards, Measurements and Testing (S, M & T) Programme, formerly Bureau Communitaire de Reference (BCR), for the operationally defined speciation of Cd, Cr, Cu, Ni and Zn. The conventional BCR three-stage sequential extraction procedure was modified at each stage, applying ultrasonic or microwave devices in order to shorten the required 16 h of shaking in all three steps. The experimental tests and the optimization of the operating parameters were carried out on a highly homogenized estuarine sediment reference material (RM S7) prepared by the Joint Research Centre (JRC) of ISPRA. Extractable metal contents were measured by inductively coupled plasma-mass spectrometry (ICP-MS) and the results obtained in each fraction by all three methods were statistically compared for all the studied elements. The conventional and newly developed alternative extraction methods were finally compared by the analysis of BCR 601, which is certified for the three-step BCR sequential extraction procedure. According to the statistical evaluation of the results, the proposed accelerated sequential extraction methods are valid alternatives to conventional shaking, with much shorter extraction times.     

Weekly variation of atmospheric particle micromorphology and chemistry in Brussels urban environment

The purpose of this study was to measure the impact of urban activities on airborne particle dynamics during weekend periods in Brussels urban area. Differences in the granulometry and micromorphology between particles sampled on working days and weekends were studied. We quantified the area, size, number, and the chemistry parameters of the airborne particles and compared between Saturday, Sunday, and Monday. We report and analyze data on airborne particles up to PM10, measured in the Brussels region from October 2002 to September 2003. Our investigation reveals detailed information regarding chemical composition of the airborne particles over the weekend period in the Brussels urban area. Furthermore, the majority of the airborne particles in the Brussels region may belong to sources geographically outside the (in situ) Brussels area.     

江苏泰州城市霾天和沙尘天气溶胶中细菌群落结构特征研究

近年来,空气污染已成为长三角地区最关键的环境问题之一,气溶胶颗粒物(PM)是最主要的污染物之一.生物气溶胶作为颗粒物的重要组成部分,可能对空气质量和人体健康产生不利影响.利用高通量测序方法研究了江苏省泰州2019年11月至2020年1月期间发生沙尘和霾污染时生物气溶胶中细菌群落结构组成特征.结果表明:冬季沙尘天和霾天气...     

Acid soil indicators in forest soils of the Cherry River Watershed, West Virginia

Declining forest health has been observed during the past several decades in several areas of the eastern USA, and some of this decline is attributed to acid deposition. Decreases in soil pH and increases in soil acidity are indicators of potential impacts on tree growth due to acid inputs and Al toxicity. The Cherry River watershed, which lies within the Monongahela National Forest in West Virginia, has some of the highest rates of acid deposition in Appalachia. East and West areas within the watershed, which showed differences in precipitation, stream chemistry, and vegetation composition, were compared to evaluate soil acidity conditions and to assess their degree of risk on tree growth. Thirty-one soil pits in the West area and 36 pits in the East area were dug and described, and soil samples from each horizon were analyzed for chemical parameters. In A horizons, East area soils averaged 3.7 pH with 9.4 cmol_c kg^???1 of acidity compared to pH 4.0 and 6.2 cmol_c kg^???1 of acidity in West area soils. Extractable cations (Ca, Mg, and Al) were significantly higher in the A, transition, and upper B horizons of East versus West soils. However, even with differences in cation concentrations, Ca/Al molar ratios were similar for East and West soils. For both sites using the Ca/Al ratio, a 50% risk of impaired tree growth was found for A horizons, while a 75% risk was found for deeper horizons. Low concentrations of base cations and high extractable Al in these soils translate into a high degree of risk for forest regeneration and tree growth after conventional tree harvesting.     

An experimental design for the optimization of the extraction methods of metallic mobile fractions from environmental solid samples

The evaluation of the cadmium and lead mobile forms from environmental solid samples provides information about their mobility and bioavailability. In the present study, the Cd and Pb mobile fractions were obtained by two modified extraction methods applied to industrial and acidic pH soils or to polluted sediments. In order to highlight that the extraction procedure does not significantly influence the quantitative atomic absorption spectrometric determination of cadmium and lead, the robustness of the extraction methods was evaluated and proven applying a Youden and Steiner factorial design. Within this experimental design, the shaking rate, the shaking time, and the solid/liquid extraction ratio were modified. The measurement uncertainty of the whole analytical procedure was assessed, the contribution of the factors involved in the extraction process being insignificant compared to the other uncertainty sources. The importance of the study is related to the fact that it proves the applicability in the routine laboratory practice of the modified extraction methods by increasing the extraction ratio following thorough optimization and robustness studies.     

Correlation between soil characteristics and lead and cadmium content in the aboveground biomass of Virginia tobacco

The study was conducted on alluvial-meadow, maroon-forest soils and vertisols with Virginia tobacco. The total content of lead and cadmium is measured through decomposition by HF, HClO₄, and HNO₃ acids. A solution of 0.005 M diethylentriaminepentaacetic acid + 0.1 M triethanolamine, pH 7.3 was used for extraction of the elements’ mobile forms from soils. The preparation of plant samples was made by means of dry ashing and dissolution in 3 M HCl. An atomic absorption spectrometer “Spektra AA 220” of the Australian company Varian was used for determination of Pb and Cd content in the soil and plant samples. Certified reference materials (three soils and tobacco leaves) were also analyzed for the verification of the accuracy of Pb and Cd determination. A correlation/regression analysis was conducted between pH, humus content, total and mobile forms of lead and cadmium in the soil, and the concentration of these elements in the aboveground biomass of Virginia tobacco. It was established that there are no statistically significant dependencies determined between soil pH and lead concentration in the plant organs of Virginia tobacco. Regressional dependencies of great significance were determined between the humus content, total and mobile lead and cadmium in the soil, and the element concentration in the leaves of the three harvesting zones.     

Quantification of pendimethalin in soil and garlic samples by microwave-assisted solvent extraction and HPLC method

A method for the residual pendimethalin in soil and vegetable samples was developed. The method is based on extraction of pendimethalin from samples using microwave-assisted solvent extraction (MASE) with acetone, ethanol, and water as extraction solvent. Extracted pendimethalin samples were analyzed by high-performance liquid chromatography with ultraviolet detector at 240 nm. The MASE parameters, temperature, heating time, and solvent types were optimized with the feasibility of MASE application in the determination of pendimethalin extraction efficiency of pendimethalin from soil and vegetable samples. The maximum temperature that can be used during the heating for MASE is 60°C, where the recovery percentages reached 97%. Linearity for pendimethalin was found in the range of 2?C20 ??g mL^???1 with limits of detection and limits of quantification of 0.059 and 0.17 ??g mL^???1, respectively.