微波消解-石墨炉原子吸收分光光度法测定海洋沉积物中镉和铬

以硝酸作为消解液,采用微波消解仪对海洋沉积物进行消解,用石墨炉原子吸收分光光度法测定消解液中的Cd和Cr。该方法在0μg/L~10.0μg/L范围内线性良好,Cd和Cr的方法检出限分别为0.04 mg/kg和2.0 mg/kg,实际样品的加标回收率在96.0%~100%之间,RSD为0.3%~5.2%。用该方法与国标法同时测定北部湾海域海洋沉积物实际样品,结果无明显差异,而该方法处理样品更为省时省力。     

原子吸收光谱法测定多维元素药片中矿物质含量

采用原子吸收光谱法测定了多维元素药片中矿物质含量。样品用硝酸消解,用火焰原子吸收法测定钙、镁、钾、铜、铁、锰,用石墨炉原子吸收法测铬和镍。方法灵敏可靠,测量相对标准偏差<2.4%,回收率在90%～100%之间,能满足药品检测要求。     

微波消解-原子吸收光度法测定土壤中铜锌铅镉镍铬

用微波消解－原子吸收光度法测定土壤中铜，锌，铅，镉，镍和铬。通过硝酸－氢氟酸－过氧化氢体系消解液对土壤样品消解，选择出微波最佳消解条件。对硝酸－盐酸－过氧化氢体系消解液和硝酸－氢氟酸－过氧化氢体系消解液进行消解对比试验，发现前者不能将土壤样品完全消解，后者能将样品消解完全，但需将消解液中剩余的酸赶尽，否则测定结果将明显偏低。微波消解土壤与传统电热消解相比，操作简便快速，可提高工作效率。     

微波高压络合消解石墨炉原子吸收分光光度法测定环境空气中锑

用有机滤膜采集空气中颗粒物样品,用微波高压络合消解后制成样品溶液。用石墨炉原子吸收分光光度法可确定样品溶液中锑的浓度。该方法具有对有机滤膜和样品消解完全,省时,无损失,灵敏度高,准确度、精密度好等特点。     

火焰原子吸收法间接测定环境水中的硫化物

利用空气-乙炔火焰原子吸收法间接测定水中硫化物,方法适用于环境水中硫化物的测定.用改进后的装置进行预处理,样品中加入10ml磷酸,用氮气作载气将生成的硫化氢吹出,载气流量50ml/min,吹气40min.用pH4.5的乙酸-乙酸钠缓冲介质中的Cu(Ⅱ)作吸收液,并加入95％的乙醇作气泡分散剂.测定吸收液水相中剩余的Cu(Ⅱ),以达到间接测定硫化物的目的.方法相对标准偏差为1.6％～3.4％,检测下限0.02mg/L.     

石墨炉原子吸收法用Pd基体改进剂测地表水中的Pb

石墨炉原子吸收法用Ｐｄ基体改进剂测地表水中的Ｐｂ李惠兰，牛星梅（南京市环境监测中心站２１００１３）１前言石墨炉原子吸收光谱法是测定环境样品中的痕量元素最有效的方法之一，它比火焰原子吸收的绝对灵敏度高三个数量级，方法简便，通常情况下液体样品可不用予处理...     

火焰原子吸收法测定河流沉积物中微量铜,铅,锌,镉,镍

河流沉积物中微量金属元素的原子吸收测定法已有报道,通常采用的分解方法是用高氯酸—氢氟酸—硝酸混合酸体系消解.但此法的分解效果不是很好,分解液中往往有油脂状物质残留,分解后期会出现溅暴现象,影响测定结果的重现性和准确性.本文研究了用氯酸—氢氟酸—硝酸混合酸体系分解河流沉积物样品.与上述方法比较,此方法分解效果好,分解液澄清,没有油脂状物质残留;操作方便,避免了溅暴现象.     

高压微波络合消解石墨炉原子吸收分光光度法测定环境空气中锡

用有机滤膜采集空气中颗粒物样品，用HNO3-HCl-HClO4-EDTA微波络合消解后制成样品溶液。用石墨炉原子吸收分光光度法可确定样品溶液中锡的浓度。该方法具有消解完全，无损失，灵敏度高，准确度、精密度好等特点。     

流动注射—原子吸收光谱分析

本文研究流动注射在原子吸收光谱仪中应用.主要优点是,省去了以往常规分析方法的标准系列配制工作,提高了分析速度.一、实验原理 实验装置如图1所示.贮液瓶A浓度为C_0的溶液以速率u_0流入样品池B,被搅拌均匀后以速率U流出吸入原子吸收雾化器.在t时刻,样品池溶液浓度C的变化率:     

微波消解—石墨炉原子吸收法测定农产品中痕量铅空白值的降低方法探讨

对于铅含量痕量级的水果、蔬菜等农产品,微波消解-石墨炉原子吸收法分析时称样量受到限制,其样品消解液中待测元素的总量很小,常出现空白值大于样品值的情况.本文就造成空白值高的原因及处理方法逐一进行了分析研究.     

南昌市周边农田土壤中多环芳烃的污染特征及来源分析

采集南昌市周边三个县的18个农田表层土壤样品,采用液固萃取-层析净化-高效液相色谱分析技术,研究了土壤中16种优控多环芳烃类物质的含量和组分特征,运用主成分因子荷载方法分析了其污染来源,并初步评价了其风险水平。结果表明,该区域内农田土壤33.3%轻度污染,最高污染样点PAHs含量为422.8ng/g,最低污染样点PAHs含量为75.2ng/g,平均含量为197.9ng/g,且远离城市的农田土壤残留水平明显低于靠近城市的农田土壤;PAHs的组分特征为以毒性水平较低的低环化合物为主;其污染来源主要是煤、天然气和汽油燃烧组成的混合源。     

Stormwater toxicity in Chollas Creek and San Diego Bay,California

Stormwater discharges from Chollas Creek, a tributary of San Diego Bay, have been shown to be toxic to aquatic life. The primary objective of this study was to provide the linkage between in-channel measurements and potential impairments in the receiving waters of San Diego Bay. This study addressed this objective within the context of four questions: (1) How much area in San Diego Bay is affected by the discharge plume from Chollas Creek during wet-weather conditions?; (2) How much of the wet-weather discharge plume is toxic to marine aquatic life?; (3) How toxic is this area within the wet-weather discharge plume?; and (4) What are the constituent(s) responsible for the observed toxicity in the wet-weather plume? The stormwater plume emanating from Chollas Creek was dynamic, covering areas up to 2.25 km2. Approximately half of the plume was estimated to be toxic to marine life, based upon the results of purple sea urchin (Strongylocentroutus purpuratus) fertilization tests. The area nearest the creek mouth was the most toxic (NOEC = 3 to 12% plume sample), and the toxicity decreased with distance from the creek mouth. The toxicity of plume samples was directly proportional to the magnitude of plume mixing and dilution until, once outside the plume margin, no toxicity was observed. Trace metals, most likely zinc, were responsible for the observed plume toxicity based upon toxicity identification evaluations (TIEs). Zinc was also the constituent identified from in-channel samples of Chollas Creek stormwater using TIEs on the storms sampled in this study, and in storms sampled during the previous storm season.     

Evaluation of the methyl ester O-methyl acetate derivative of muramic acid for the determination of peptidoglycan in environmental samples by ion-trap GC-MS-MS

Muramic acid (MA) is a unique amino sugar that is a constituent of the peptidoglycan (PG) present in prokaryotic cell walls. MA can serve as a marker for quantifying bacterial load, e.g. in indoor environments, by using gas chromatography-tandem mass spectrometry (GC-MS-MS). We demonstrated recently that the methyl ester O-methyl acetate (MMA) derivative can be used to detect MA in house dust by ion-trap GC-MS-MS. However, since the MMA derivative is not formed from free MA quantification was not optimal. Here we report 1) significant improvements in sample preparation of the MMA derivative and 2) an evaluation of the performance of derivative, using for comparison the alditol acetate derivative, the gold standard in quantitative trace analysis of MA in complex matrices. The MMA derivative was analysed using an MS instrument with internal ionization and the alditol acetate derivative was analysed using an instrument with external ionization. 13C-labelled cyanobacteria, containing MA in their PG, were used as the internal standard. A linear relationship was found between the two methods in studies on 27 parallel samples of airborne dust from school classes collected on filters. Although the analytical sensitivity of the MMA derivatives was somewhat slightly lower than of the alditol acetate derivative, this may be due to differences in yield of derivative, sample clean-up efficiency, or different performance of the GC columns or MS instruments. However preparation of the MMA derivative is quick and compatible with preparation of methyl esters of 3-hydroxy fatty acids (used as markers of Gram negative endotoxin) allowing the levels of both markers to be determined in the same dust sample. In conclusion, the MMA procedure can be used to determine MA in environmental samples with good reproducibility provided the concentration of the 13C-labelled MA internal standard in the cyanobacteria is first determined with an alternative method.     

Ozone Destruction on Solid Particles

Ozone (O3) is an important constituent of the Earth atmosphere, either stratosphere, where it has a beneficial role to protect Earth's surface from harmful UV-B radiation, or troposphere where it is considered an air pollutant. We investigated the ozone destruction on solid particles of natural or anthropogenic origin as: silica-gel, pollen, coal fly ash, titanium dioxide with different specific surface (s) and sodium halides (NaCl, NaBr and NaI). The experiments were conducted in a fluidized bed reactor with elevated ambient concentrations of O3 (100 ppb) employed. The results indicate that the destruction of O3 depends upon: sample quantity (silica-gel with equal s), sample surface (TiO2 with different s) and chemical composition (coal fly ash comparative to wood ash). Interesting results were obtained with sodium halides: no effect on O3 concentrations was detected with NaCl, NaBr shows a certain destruction, while NaI removes completely O3 from the air stream. In the experiments with NaI doped NaCl, the destruction of O3 was dependent on NaI quantity.     

Assessing uncertainty in annual nitrogen,phosphorus, and suspended sediment load estimates in three agricultural streams using a 21-year dataset

Accurate estimation of constituent loads is important for studies of ecosystem mass balance or total maximum daily loads. In response, there has been an effort to develop methods to increase both accuracy and precision of constituent load estimates. The relationship between constituent concentration and stream discharge is often complicated, potentially leading to high uncertainty in load estimates for certain constituents, especially at longer-term (annual) scales. We used the loadflex R package to compare uncertainty in annual load estimates from concentration vs. discharge relationships in constituents of interest in agricultural systems, including ammonium as nitrogen (NH₄-N), nitrate as nitrogen (NO₃-N), soluble reactive phosphorus (SRP), and suspended sediments (SS). We predicted that uncertainty would be greatest in NO₃-N and SS due to complex relationships between constituent concentration and discharge. We also predicted lower uncertainty with a composite method compared to regression or interpolation methods. Contrary to predictions, we observed the lowest uncertainty in annual NO₃-N load estimates (relative error 1.5–23%); however, uncertainty was greatest in SS load estimates, consistent with predictions (relative error 19–96%). For all constituents, we also generally observed reductions in uncertainty by up to 34% using the composite method compared to regression and interpolation approaches, as predicted. These results highlight differences in uncertainty among different constituents and will aid in model selection for future studies requiring accurate and precise estimates of constituent load.     

Groundwater quality under the influence of spent mushroom substrate weathering

Nitrate and other solutes resulting from field-weathering of spent mushroom substrate (SMS) percolate into underlying soils and may migrate to groundwater. A field trial was conducted to investigate the potential influences of SMS weathering on groundwater quality. Spent mushroom substrate was deposited at 90 and 150 cm pile depths over a Typic Hapludult and weathered for 2 years. Eight casing wells were installed around the SMS piles to monitor the quality changes of groundwater with a high seasonal water table of 760 cm below the surface. Although leachate solutes had moved more than 200 cm deep in soil from the surface, no significant changes of groundwater quality caused by SMS weathering were observed even one year after removal of the SMS piles (3 years total). The groundwater had pH, electrical conductivity (EC) and dissolved organic carbon (DOC) of 4.3-5.7, 0.2-0.3 dS m(-1) and 0.7-2.2 mg L(-1), respectively. The major inorganic ions were Mg(2+), Ca(2+), Na(+), Cl(-), SO(4)(2-) and NO(3)(-), with a concentration range of 2.5-68.3 mg L(-1). The results suggest that SMS leachate solutes migrated fairly slow in deep subsurface soils of the experimental field. Considering that leachate solutes may move several meters in soil through preferential flow channels, weathering of SMS in fields with a high seasonal groundwater table >or=5 m below the ground is recommended. Conservatively, SMS weathering should be conducted on compact surfaces and leachate be collected and reused as liquid fertilizers.     

Acidification of soil-water in low base-saturated sand soils of the superior uplands under acid and normal precipitation

Lakes and streams are acidified by direct precipitation and water channeled through nearby soils, but water in low base-saturation soils can produce highly acidic percolate after prolonged contact and subsequent degassing in surface waters. Theories advanced by Reuss (1983), Reuss and Johnson (1985), and Seip and Rustad (1984) suggest that soils with less than 15% base saturation are susceptible to soil-water pH depression of up to 0.4 unit, which is sufficient to cause negative alkalinity in soil solutions. High concentrations of mobile anions (notably sulfate) are responsible for the negative alkalinity and these solutions on CO₂ degassing in surface waters can retain acidities equivalent to a pH value of 5.0 or less. This mechanism purports to explain why some lakes acidify when they are surrounded by acid soils and cation leaching is not required.Ambient precipitation set to pH 5.4 and pH 4.2 was applied to columns of low base-saturated, sand, soils, starting in 1985. The columns (15 cm diameter and 150 cm long) were collected from soils with base saturations falling into one of three groups (0–10, 10–20, and 20–40%) from national forests in the Superior Uplands area (includes Boundary Waters Canoe Area, Rainbow Lakes, Sylvania, Moquah Barrens, and other Wilderness and Natural areas). The soils were Haplorthods and Udipsamments mainly from outwash plains.The soil columns were instrumented and reburied around a subterranean structure used to collect leachate water and to maintain natural temperature, air, and light conditions. Three humus treatments were applied to soil column (none, northern hardwood, and jack pine) to measure the effect of natural acidification compared to acidification by acid precipitation. The cores were treated with precipitation buffered to pH 5.4 to simulate natural rain and pH 4.2 to simulate acid rain.Columns were treated in 1985 and 1986 with approximately 200 cm of buffered precipitation each year over the frost-free season. Data is now being analyzed for the 1986 treatment year. In leachate collected from the upper horizons of the soil colums, there was a significant difference in pH, alkalinity, nitrate, and sulfate concentrations between the pH 5.4 and pH 4.2 precipitation treatments. This difference, however, disappears at the bottom of the columns. This could be partly due to exchange reactions in the B horizon. The pH and alkalinities are higher in bottom leachate. Chloride and nitrate also increased significantly due mainly to concentrating effects. Even with a pickup of sulfate in the B horizon, sulfate adsorption decreased bottom leachate concentrations well below surface values.Alkalinity, pH, and sulfate concentration in the leachate decreased over the treatment season. Nitrate concentration increased by 4- to 5-fold over the season. Leachate from the bottom of the soil columns is becoming more acidic with time with negative alkalinities appearing more frequently in columns with soils of lower base saturation. There were some significant alkalinity differences due to humus treatments; however, these were not consistent between pH treatments, and need further study. This research will eventually answer whether soil processes can be important to the acidification of lakes in poor, sandy, outwash plains of the Superior Uplands, and whether a reduction in acid sulfate deposition will reverse the percolate alkalinity from negative to positive.Contribution from Fourth World Wilderness Congress-Acid Rain Symposium, Denver (Estes Park), Colorado, September 11–18, 1987.     

Near-real-time determination of hydrogen peroxide generated from cigarette smoke

The ability to monitor hydrogen peroxide (H2O2) in aqueous smoke extracts will advance our understanding of the relationship between cigarette smoke-induced oxidative stress, inflammation, and disease and help elucidate the pathways by which the various smoke constituents exert their pathogenic effects. We have demonstrated, for the first time, the measurement of H2O2 production from cigarette smoke without prior separation of the sample. Cigarettes were tested on a commercial smoking machine, such that the whole smoke or gas vapor phase was bubbled through phosphate buffered saline solution at pH 7.4. Aliquots of these solutions were analyzed using an Amplex Red/horseradish peroxidase fluorimetric assay that required only a 2 minute incubation time, facilitating the rapid, facile collection of data. Catalase was used to demonstrate the selectivity and specificity of the assay for H2O2 in the complex smoke matrix. We measured approximately 7-8 microM H2O2 from two reference cigarettes (i.e., 1R4F and 2R4F). We also observed 9x more H2O2 from whole smoke bubbled samples compared to the gas vapor phase, indicating that the major constituent(s) responsible for H2O2 formation reside in the particulate phase of cigarette smoke. Aqueous solutions of hydroquinone and catechol, both of which are particulate phase constituents of cigarette smoke, generated no H2O2 even though they are free radical precursors involved in the production of reactive oxygen species in the smoke matrix.     

大力推广清洁能源——甲醇(M15)汽油

随着国际原油价格持续高位运行,实施能源的多元化战略已是当前世界各国政府做出的重要抉择.我国是一个缺油少气、相对富煤的国家,合理、高效、节能、安全的发展煤基替代燃料是我国能源发展的惟一出路,甲醇汽油是车用燃料替代,是新能源的重要组成部分.本文对此进行了论述.     

Evaluating performance of stormwater sampling approaches using a dynamic watershed model

Accurate quantification of stormwater pollutant levels is essential for estimating overall contaminant discharge to receiving waters. Numerous sampling approaches exist that attempt to balance accuracy against the costs associated with the sampling method. This study employs a novel and practical approach of evaluating the accuracy of different stormwater monitoring methodologies using stormflows and constituent concentrations produced by a fully validated continuous simulation watershed model. A major advantage of using a watershed model to simulate pollutant concentrations is that a large number of storms representing a broad range of conditions can be applied in testing the various sampling approaches. Seventy-eight distinct methodologies were evaluated by "virtual samplings" of 166 simulated storms of varying size, intensity and duration, representing 14 years of storms in Ballona Creek near Los Angeles, California. The 78 methods can be grouped into four general strategies: volume-paced compositing, time-paced compositing, pollutograph sampling, and microsampling. The performances of each sampling strategy was evaluated by comparing the (1) median relative error between the virtually sampled and the true modeled event mean concentration (EMC) of each storm (accuracy), (2) median absolute deviation about the median or "MAD" of the relative error or (precision), and (3) the percentage of storms where sampling methods were within 10% of the true EMC (combined measures of accuracy and precision). Finally, costs associated with site setup, sampling, and laboratory analysis were estimated for each method. Pollutograph sampling consistently outperformed the other three methods both in terms of accuracy and precision, but was the most costly method evaluated. Time-paced sampling consistently underestimated while volume-paced sampling over estimated the storm EMCs. Microsampling performance approached that of pollutograph sampling at a substantial cost savings. The most efficient method for routine stormwater monitoring in terms of a balance between performance and cost was volume-paced microsampling, with variable sample pacing to ensure that the entirety of the storm was captured. Pollutograph sampling is recommended if the data are to be used for detailed analysis of runoff dynamics.