土壤中总汞测定的预处理方法探讨

利用标准样品,将微波消解、水浴消解和直接测定3种预处理方法进行分析比较,分析3种方法的优点和缺点以及对土壤中总汞含量测定的差异。结果表明:3种预处理方法下测定的汞元素含量的大小顺序:微波消解直接测定≈水浴消解,相对误差大小顺序:微波消解水浴消解≈直接进样,各方法测定的汞元素含量都在样品的保证值的不确定度范围内。对ESS-3土壤标样进行加标回收率试验,微波消解、水浴消解和直接测定对汞的加标回收率分别是97.6%、92.2%和95%,微波消解在准确度和精密度方面略优于水浴消解和直接测定。综上,3种预处理方法都能方便、快速、准确地测定土壤中的汞元素,这将为不同实验室选择不同土壤预处理方法提供参考和依据。     

原子荧光法测定生物体中As消解条件改进探讨

以HNO3-H2SO4-HCIO4混合酸进行消解样品,氢化物发生原子荧光光谱法测定生物体中As。本法克服了以HNO3-HCIO4混合酸放置过夜、消解不完全和消解慢等弊端,同时研究了消解方法、酸度、还原剂浓度以及干扰离子等对测定的影响。通过对标准样品消解测定,测定结果满意,相对标准偏差为2.3%,完全满足生物体中As的分析要求,具有分析速度快、操作简便、检验效率高等优点。     

酸溶-微波消解-电感耦合等离子体质谱法测定土壤及沉积物中的钽

采用氢氟酸-硝酸体系、微波消解法进行土壤及沉积物的消解,并使用电感耦合等离子体质谱仪进行测定。优化了消解条件,并确定了仪器使用条件,方法检出限为0.002mg/kg,对有证标准土壤样品进行测定的结果符合准确度要求,实际样品的相对标准偏差为1.9%～3.8%,样品回收率在91.0%～96.2%。方法具有良好的稳定性、灵敏度高、准确度高等特点。适合土壤中钽元素的测定。     

一种快速测定化学需氧量方法的研究

本文对快速测定化学需氧量(COD)方法展开了研究分析,具体设计如下:将快速消解分光光度法作为研究基础,利用自配消解试剂来优化原有COD测定,测定的标准物质为邻苯二甲酸氢钾,通过改变多个影响因素进行重复试验,最终得出最佳测定条件,氧化剂为0.250mol/L重铬酸钾1.00mL,催化剂为硫酸-硫酸银4.0ml,消解时间10分钟,消解温度165℃,测定值为100.59mg/L,与理论值之间的误差为0.59%,这种测定方法通过了验证,具备实践价值。     

无银催化-微波消解快速测定污水中化学需氧量研究

以MgSO4 CuSO4 为催化剂 ,探讨了无银催化微波消解测定污水中化学需氧量的方法。通过对影响污水消解效率的系列条件试验 ,确定了微波消解测定污水CODCr的最佳条件 :微波功率为中强火、消解时间为 5min、混酸介质H3PO4 H2 SO4 配比为 1∶4、消解酸度为 5 0 %、催化剂MgSO4 CuSO4 配比为 1∶1等。用该方法测定污水中的CODCr,与回流法测得结果吻合。该方法采用无银催化剂和微波消解 ,具有精密度高、操作费用低、消解速度快等特点     

微波消解样品-电感耦合等离子体质谱法同时测定土壤中重金属元素和稀土元素

通过优化微波消解条件,调谐电感耦合等离子体质(ICP-MS)工作条件,建立了微波消解-电感耦合等离子体质谱法测定土壤中11种重金属和16种稀土元素的分析方法。研究了样品消解工序、标准溶液配制、外标法对元素测定的影响,对质控样品的检测显示该方法测定值与标准值吻合。方法检出限为0.012~0.711 ng/g,精密度(RSD)为0.33%~4.4%(n=6),加标回收率为86.1%~105.7%,表明该方法准确可靠。     

原子吸收法测定土壤中铜锌铅镉

通过对几种消解体系的对比 ,选择出铅、镉最佳的消解方法为硝酸 氢氟酸 双氧水体系 ;铜锌最佳的消解方法为硝酸 氢氟酸 高氯酸体系。不同方法既能达到全量分析的要求 ,又能使基体干扰降到最小。通过对标准样品的多次测定 ,测定值均在其保证值范围内 ,铅镉相对标准偏差为 2 2 %～ 7 2 % ,加标回收率在 83%～ 116 %之间 ;铜锌相对标准偏差为 2 6 %～ 4 5 % ,加标回收率在 92 %～ 10 3%之间。     

消解体系对TSP滤膜重金属测定的影响研究

大气降尘中重金属成分复杂,消解体系直接影响重金属元素测试准确性。于2016年12月采集辽宁工程技术大学校区31个大气TSP样品,选用4种不同微波消解体系:HNO_3(放置过夜)、HNO_3(放置过夜)+H_2O_2(3∶1)、HCl+HNO_3(3∶1)、HCl+HNO_3+HF(3∶1∶1),对聚四氟乙烯(PTFE)滤膜采集的大气TSP消解,利用电感耦合等离子体质谱仪(ICP-MS)对其中Pb、Cr、Cd、As、Cu、Ni、Mn 7种主要重金属元素进行测定。精密度对比实验与准确度对比实验结果表明:4种微波消解体系下,测定结果的相对标准差(RSD)范围为2.85%~13.46%,空白加标回收率范围为94.2%~115.00%,样品加标回收率范围为92.2%~115.3%。HNO_3+H_2O_2消解体系下的测定结果精密度良好(RSD≤2.85%);准确度较好(空白加标回收率为96.80%~102.8%,样品加标回收率为96.3%~100.4%);确定ICP-MS测定PTFE滤膜上TSP重金属含量的最优消解体系为HNO_3+H_2O_2。且此消解体系具有污染程度小、背景值低、消解充分、可大批量测试、对仪器及其测定影响较小等特点;实验结果为ICP-MS测定PTFE滤膜上TSP重金属分析工作提供理论与实验依据。     

淡水鱼肌肉组织内砷含量测定方法探究

用湿式消解法对淡水鱼的肌肉组织进行消解,处理后用原子荧光光度计测定其砷元素的含量,最低检出质量浓度为0.002mg/kg,测定样品砷含量0.056 mg/kg-0.084 mg/kg,相对标准偏差(RSD)2.21%,回收率93.0%-103%。     

密封消解法测定高盐废水COD时的最佳实验条件选择

通过对密封消解法测定高盐废水COD的消解时间、氧化剂浓度、掩蔽剂比例等实验条件研究 ,确定了适合高盐废水COD测定的最佳实验条件 ,并用混配水样和实际水样进行验证。研究结果表明 :消解时间为 30min ,掩蔽剂比例为 10 1,对不同范围的COD采用不同浓度的氧化剂 ,混配水样和实际水样中的氯离子对COD测定干扰很小 ,方法的准确度较好 ,相对误差 <8 3% ,加标回收率 >92 %。     

Degradation of metabolites accumulated of benzo[a]pyrene by coupling Penicillium Chrysogenum with KMnO4

Several main metabolites of benzo[a]pyrene （BaP） formed by Penicillium chrysogenum, Benzo[a]pyrene-1,6-quinone （BP 1,6- quinone）, trans-7,8-dihydroxy-7,8-dihydrobenzo[a]pyrene （BP 7,8-diol）, 3-hydroxybenzo[a]pyrene （3-OHBP）, were identified by high-performance liquid chromatography （HPLC）. The three metabolites were liable to be accumulated and were hardly further metabolized because of their toxicity to microorganisms. However, their further degradation was essential for the complete degradation of BaP. To enhance their degradation, two methods, degradation by coupling Penicillium chrysogenum with KMnO4 and degradation only by Penicillium chrysogenum, were compared; Meanwhile, the parameters of degradation in the superior method were optimized. The results showed that （1） the method of coupling Penicillium chrysogenum with KMnO4 was better and was the first method to be used in the degradation of BaP and its metabolites; （2） the metabolite, BP 1,6-quinone was the most liable to be accumulated in pure cultures; （3） the effect of degradation was the best when the concentration of KMnO4 in the cultures was 0.01% （w/v）, concentration of the three compounds was 5 mg/L and pH was 6.2. Based on the experimental results, a novel concept with regard to the bioremediation of BaP-contaminated environment was discussed, considering the influence on environmental toxicity of the accumulated metabolites.     

Impact of atrazine and nitrogen fertilizers on the sorption of chlorotoluron in soil and model sorbents

Sorption of chlorotoluron in ammonium sulfate, urea and atrazine multi-solutes system was investigated by batch experiments. The results showed application of nitrogen fertilizers to the soil could affect the behavior of chlorotoluron. At the same concentration of N, sorption of chlorotoluron decreased as the concentration of atrazine increased on the day 0 and 6 in soil, respectively. The sorption of chlorotoluron increased from 0 to 6 d when soils were preincubated with deionized water, ammonium sulfate and urea solution for 6 d. That indicated incubation time was one of the most important factors for the sorption of chlorotoluron in nitrogen fertilizers treatments. The individual sorption isotherms of chlorotoluron in rubbery polymer and silica were strictly linear in single solute system, but there were competition sorption between pesticides or between pesticides and nitrogen fertilizers. That indicated the sorption taken place by concurrent solid-phase dissolution mechanism and sorption on the interface of water-organic matter or water-mineral matter.     

Toxicity assessing for chlorpyrifos-contaminated soil with three different earthworm test methods

Earthworm toxicity tests are useful tools for terrestrial risk assessment but require a hierarchy of test designs that differ in effect levels (behavior, sublethal, lethal). In this study, the toxicity of chlorpyrifos contaminated soil on earthworms was assessed. In addition to the acute and chronic tests, an avoidance response test was applied. Earthworms were exposed to sublethal and lethal concentration of chlorpyrifos, and evaluated for acute toxicity, growth, fecundity and avoidance response after a certain exposure period. The test methods covered all important ecological relevant endpoints (acute, chronic, behavioral). Concentration of 78.91 mg/kg, chlorpyrifos caused significant toxic effects in all test methods, but at lower test concentrations, only significant chronic toxic effects could be observed. In the present study, chlorpyrifos had adverse effect on growth and fecundity in earthworm exposed to 5 mg/kg chlorpyrifos after eight weeks. The avoidance response test, however, showed significant repellent effects concentration of 40 mg/kg chlorpyrifos. For chlorpyrifos, concentration affecting avoidance response was far greater than growth and fecundity, it seemed likely that earthworms were not able to escape from pesticide-contaminated soil into the clean soil in field and hence were exposed continuously to elevated concentrations of pesticides.     

Leaching of styrene and other aromatic compounds in drinking water from PS bottles

Bottled water may not be safer, or healthier, than tap water. The present studies have proved that styrene and some other aromatic compounds leach continuously from polystyrene （PS） bottles used locally for packaging. Water sapmles in contact with PS were extracted by a preconcentration technique called as ＂purge and trap＂ and analysed by gas chromatograph-mass spectrometer （GC/MS）. Eleven aromatic compounds were identified in these studies. Maximum concentration of styrene in PS bottles was 29.5 μg/L. Apart from styrene, ethyl benzene, toluene and benzene were also quantified but their concentrations were much less than WHO guide line values. All other compounds were in traces. Quality of plastic and storage time were the major factor in leaching of styrene. Concentration of styrene was increased to 69.53 μg/L after one-year storage. In Styrofoam and PS cups studies, hot water was found to be contaminated with styrene and other aromatic compounds. It was observed that temperature played a major role in the leaching of styrene monomer from Styrofoam cups. Paper cups were found to be safe for hot drinks.     

Sludge concentration dynamic distribution and its impact on the performance of UNITANK

UNITANK is a biological wastewater treatment process that combines the advantages of traditional activated sludge process and sequencing batch reactor, which is divided into Tank A, B and C. In this study, the sludge distribution and its impact on performance of UNITANK were carried out in Liede Wastewater Plant （WWTP） of Guangzhou, China. Results showed that there was a strong affiliation between Tank A and B of the system in sludge concentration distribution. The initial sludge concentration in Tank A could present the sludge distribution of the whole system. The sludge distribution was mainly influenced by hydraulic condition. Unsteady sludge distribution had an impact on variations of substrates in reactors, especially in decisive reactor, and this could lead to failure of system. Settler could partially remove substrates such as COD and NO3-N, but there was adventure of sludge deterioration. The rational initial sludge concentration in Tank A should be 4000-6000 mg/L MLSS.     

Treated wastewater irrigation effect on soil, crop and environment： Wastewater recycling in the loess area of China

A study was carried out at the Loess Plateau in Dongzhi,China,to test the feasibility of using secondary treatment sewage effluent and to determine whether the water quality would then meet the recommended irrigation norm.Seven crops,including celery,wheat, maize,millet,apples,rapeseed and yellow beans,were tested in the study.Physical and chemical properties of the soil,crop yield and quality and leachate at different soil depths were measured.In most cases,the quality of the crops that made use of treated sewage was not distinctively different from those that did not use treated sewage.However,yields for the former were much higher than they were for the latter.Leachates at different soil depths were analyzed and the results did not show alarming levels of constituents.For a period of approximately 14 months,the treated sewage irrigation had no significant effect on the loess soil and no cases of illness resulting from contact with the treated sewage were reported.With treated sewage irrigation,a slight increase in the organic content of the soil was observed.     

Spatial variability of organochlorine pesticides （DDTs and HCHs） in surface soils from the alluvial region of Beijing, China

The spatial variability in the concentrations of 1,2,3,4,5,6-hexachlorocyclohexane (HCH) and 1,1,1-trichloro-2,2-bis-(p-chlorophenyl) ethane (DDT) in surface soils was studied on the basis of the analysis of 131 soil samples collected from the surface layer (0-20 cm depth) of the alluvial region of Beijing, China. The concentrations of total HCHs (including α-, β-, γ-, and δ-isomers) and total DDTs (i ncluding p,p'-DDT, p,p'-DDD, p,p'-DDE, and o,p'-DDT) in the surface soils tested were in the range from nondetectable to 31.72 μg/kg dry soil, with a mean value of 0.91, and from nondetectable to 5910.83 μg/kg dry soil, with a mean value of 32.13,respectively. It was observed that concentrations of HCHs in all soil samples and concentrations of DDTs in 112 soil samples were much lower than the first grade (50 μg/kg) permitted in "Environment quality standard for soils in China (GB15618-1995)". This suggests that the pollution due to organochlorine pesticides was generally not significant in the farmland soils in the Beijing alluvial region. In this study, the spatial distribution and trend of HCHs and DDTs were analyzed using Geostatistical Analyst and GS (513).Spatial distribution indicated how these pesticides had been applied in the past. Trend analysis showed that the concentrations of HCHs,DDTs, and their related metabolites followed an obvious distribution trend in the surface soils from the alluvial region of Beijing.     

Heavy metal availability and impact on activity of soil microorganisms along a Cu/Zn contamination gradient

All the regulations that define a maximum concentration of metals in the receiving soil are based on total soil metal concentration. However, the potential toxicity of a heavy metal in the soil depends on its speciation and availability. We studied the effects of heavy metal speciation and availability on soil microorganism activities along a Cu/Zn contamination gradient. Microbial biomass and enzyme activity of soil contaminated with both Cu and Zn were investigated. The results showed that microbial biomass was negatively affected by the elevated metal levels. The microbial biomass-C （Cmic）/organic C （Corg） ratio was closely correlated to heavy metal stress. There were negative correlations between soil microbial biomass, phosphatase activity and NH4NO3 extractable heavy metals. The soil microorganism activity could be predicted using empirical models with the availability of Cu and Zn. We observed that 72% of the variation in phosphatase activity could be explained by the NH4NO3-extractable and total heavy metal concentration. By considering different monitoring approaches and different viewpoints, this set of methods applied in this study seemed sensitive to site differences and contributed to a better understanding of the effects of heavy metals on the size and activity of microorganisms in soils. The data presented demonstrate the relationship between heavy metals availability and heavy metal toxicity to soil microorganism along a contamination gradient.     

Bioaccumulation of heavy metals in fishes from Taihu Lake, China

The Cr,Zn,Cu,Cd,Pb contents were determined in Cyprinus carpio Linnaeus,Carassius auratus Linnaeus,Hypophthalmichthys molitrix and Aristichthys nobilis,which were caught from Meiliang Bay,Taihu Lake,a large,shallow and eutrophic lake of China.The results showed that:(1)the Cr,Cu,Pb,Cd contents in the edible parts of the four fish species were much lower than Chinese Food Health Criterion(1994),but the Zn contents were higher than the Criterion;(2)Cd contents were the highest in the liver of fish,Pb contents were almost the same in all organs of fish,Cr contents mainly enriched in the skin and gonads,Zn contents were the highest in the gonad(♀),and Cu contents were the highest in the liver;(3)the total metal accumulation was the greatest in the liver and the lowest in the muscle.The total metal accumulation was the highest in C.auratus L.This investigation indicated that fish products in Taihu Lake were still safe for human consumption,but the amount consumed should be controlled under the Chinese Food Health Criterion to avoid excessive intake of Zn.     

Biological control experiment of excess propagation of Cyclops for drinking water security

Cyclops of zooplankton propagated excessively in eutrophic water body and could not be effectively inactivated by the conventional disinfections process like chlorination due to its stronger resistance to oxidation. In this study, an ecological project was put forward for the excess propagation control of Cyclops by stocking the filter-feeding fishes such as silver carp and bighead carp under the condition of no extraneous nutrient feeding. The results of experiments with different stocking biomass showed that the propagation of Cyclops could be controlled effectively, and the water quality was improved simultaneously by impacting on nutriment level and plankton community structure at proper stocking density of 30 g/m^3 of water. The growth of Cyclops may not be effectually controlled with lower biomass of fish （10 g）, and the natural food chain relation may be destroyed for Cyclops dying out in water while the intense stocking of 120 g per cubic meter of water. In addition, the high predator pressure may accelerate supplemental rate of nutrients from bottom sediments to water body to add the content of total nitrogen and phosphorus in water.