离子色谱法测定河流中乙酸、丙酸和丁酸含量的研究

建立一种用离子色谱法同时分离测定被污染河流水中微量乙酸、丙酸和丁酸的方法。采用IonPac AS11-HC阴离子分离柱,5mM NaOH淋洗液,流速1.0ml/min。结果表明,乙酸、丙酸、丁酸的检出限按峰高计分别为0.258、0.294、0.374mg/L;按峰面积计分别为0.350、0.421、0.588mg/L。乙酸、丙酸、丁酸的保留时间、峰高、峰面积的变异系数RSD在0.03%~3.92%之间。对某河流水样分析,乙酸、丙酸、丁酸的回收率在99.6%~107.6%间。     

气相分子吸收光谱法测定海水中亚硝酸盐氮

采用气相分子吸收光谱仪测定海水中亚硝酸盐氮,方法在低浓度(0.00~0.50 mg/L)和高浓度(0.00~2.00 mg/L)范围内均具有良好的线性,线性相关系数R2均≥0.999 7,检出限为0.003 mg/L,准确度和精密度良好。用本法与国标法(萘乙二胺分光光度法)同时测定若干实际海水样品中亚硝酸盐氮,两种方法的测定结果相对偏差为0.00%~4.90%。对两组测定结果进行线性拟合,结果显示相关系数R2为0.998 7,说明两组测定结果具有良好的一致性。相比国标法,气相分子吸收光谱法具有操作简单、分析快速准确、干扰少等优点,能够替代国标法。     

离子色谱法测定废气中的丙烯酸

采用离子色谱法测定废气中的丙烯酸，几种常见的无机阴离子对分析无干扰。方法在0．100mg／L～10．0mg／L范围内线性良好，对有组织废气和无组织废气的检出限分别为0．04mg／m3和0．003mg／m3，废气平行样品测定值的相对偏差为3．4％～10．5％，加标样品的回收率为91％～102％。     

离子色谱法测定水中溴离子与碘离子

采用离子色谱法测定水中溴离子与碘离子，选择AS19阴离子交换分离柱、KOH淋洗液自动发生器、抑制型电导检测。溴离子与碘离子分别在14.8 μg/L～100 mg/L与30.4 μg/L～100 mg/L范围内线性良好，检出限分别为3.7 μg/L与7.6 μg/L，环境水样平行测定的RSD分别为0.2%～1.5%与0.3%～1.6%，两个质量浓度水平的加标回收率分别为91.8%～105%与89.5%～93.4%。     

反相高效液相色谱分析空气和废气中己内酰胺的方法研究

研究了反相高效液相色谱分析空气和废气中己内酰胺的方法。该方法以VWD为检测器,检测波长为210nm,流动相为乙腈∶纯水=10∶90,流动相流速为1ml/min。在已选择色谱条件下,连续运行10次,己内酰胺平均出峰时间为4 2min,保留时间和峰面积的相对标准偏差分别为1 5%和3 5%,采样体积为90L时,检测下限为0 01mg/m3,上限为2 20mg/m3,回收率在105 2%-106 3%。     

抑制型电导-离子色谱法测定水中无机阴离子

采用抑制型电导-离子色谱法测定生活饮用水、污水和地表水中F-、Cl-、NO2-、Br-、NO3-、PO43-、SO42-等7种无机阴离子,对清洁水样过滤后直接测定,浑浊样品离心后取上清液过滤测定。F-在0.100 mg/L~1.20 mg/L范围内、其余6种阴离子在1.00 mg/L~12.0 mg/L范围内线性良好,方法检出限为0.031 mg/L~0.47 mg/L,水样平行测定的RSD为0.9%~1.8%,加标回收率为82.6%~110%。     

液液萃取-高效液相色谱法测定水中四乙基铅

采用高效液相色谱紫外检测器测定水中四乙基铅,用二氯甲烷液液萃取,以甲醇/水混合溶液(体积比为95:5)为流动相,Z0RBAX Eclipse XDB-C18色谱柱分离,选择测定波长为280 nm.方法在0.100mg/L～1.00mg/L范围内线性良好,检出限和测定下限分别为0.01μg/L和0.04μg/L,水样平行...     

荧光光度法测定地表水中阴离子表面活性剂

采用荧光光度法测定地表水中烷基苯磺酸盐类阴离子表面活性剂,讨论了pH值和干扰物质对测定的影响。方法在0.200 mg/L~5.00 mg/L范围内线性良好,检出限为0.081 mg/L,实际水样加标回收率为98.6%~101%。     

石墨消解-电感耦合等离子体发射光谱法测定染整废水中总锑

建立了全自动石墨消解-电感耦合等离子体发射光谱法测定染整企业废水中总锑的测定方法。结果表明,锑的质量浓度在0~10 mg/L范围内线性关系良好,R值为0.999 5,方法检出限和测定下限分别为0.003和0.012 mg/L,相对标准偏差(RSD)为0.17%~2.6%,加标回收率为96.1%~103.8%。该方法操作简单、分析快速,符合技术规范要求。     

气相色谱直接进样法测定水中的N-甲基哌嗪-应急监测分析方法

建立了水中N-甲基哌嗪的应急监测分析方法,在3分钟内完成整个分析过程。采用直接进水样的方法,经毛细管柱分离水中的N-甲基哌嗪,用GC/FID测定,以保留时间定性,峰高定量。在浓度范围为8.44～80.32mg/L时,相对标准偏差在1.8％～2.9％之间,标准偏差在0.19～1.5之间。样品的加标回收率可达81％,标准曲线的相关系数为0.9992。检出限为0.08mg/L     

Health risk assessment of fluoride in drinking water from Anhui Province in China

This study analyzes the concentrations and health risks of fluoride in 249 drinking water samples collected from different regions of Anhui Province in China. Results indicated that fluoride content in drinking water ranged from 0.12 to 1.94 mg L^?1 (mean?=?0.57 mg L^?1) in the following order: Huaibei plain region > Jianghuai hill region ≈ Dabieshan mountainous region > plain along the Yangtze River region > southern Anhui mountainous region. The fluoride contents were less than 0.50 mg L^?1 in 66.66 % of the drinking water samples, 0.51–1.0 mg L^?1 in 23.29 %, and higher than 1.0 mg L^?1 in 12.04 %. The fluoride levels in some samples were lower than the recommended values for controlling dental caries (0.50–1.0 mg L^?1). The total fluoride intake from drinking water was between 0.14 and 2.33 mg per day in different regions of the province, supposing an individual consumes 1.2 L of water per day. Therefore, measures should be taken to increase fluoride intake in the Jianghuai hill region, Dabieshan mountainous region, plain along the Yangtze River, and southern Anhui mountainous region to control dental caries. On the other hand, the fluoride levels must be reduced in the Huaibei plain region to decrease endemic fluorosis. The results serve as crucial guidelines for managing fluoride safety in drinking water and controlling endemic fluorosis in different regions of Anhui Province.     

Evaluation of surface water quality in aquatic bodies under the influence of uranium mining (MG, Brazil)

The quality of the water in a uranium-ore-mining area located in Caldas (Minas Gerais State, Brazil) and in a reservoir (Antas reservoir) that receives the neutralized acid solution leaching from the waste heaps generated by uranium mining was investigated. The samples were collected during four periods (October 2008, January, April and July 2009) from six sampling stations. Physical and chemical analyses were performed on the water samples, and the data obtained were compared with those of the Brazilian Environmental Standards and WHO standard. The water samples obtained from waste rock piles showed high uranium concentrations (5.62 mg L^?1), high manganese values (75 mg L^?1) and low average pH values (3.4). The evaluation of the water quality at the point considered the limit between the Ore Treatment Unit of the Brazilian Nuclear Industries and the environment (Consulta Creek) indicated contamination by fluoride, manganese, uranium and zinc. The Antas reservoir showed seasonal variations in water quality, with mean concentrations for fluoride (0.50 mg L^?1), sulfate (16 mg L^?1) and hardness (20 mg L^?1) which were low in January, evidencing the effect of rainwater flowing into the system. The concentrations for fluoride, sulfate and manganese were close or above to the limits established by current legislation at the point where the treated mining effluent was discharged and downstream from this point. This study demonstrated that the effluent discharged by the UTM affected the quality of the water in the Antas reservoir, and thus the treatments currently used for effluent need to be reviewed.     

厦门水库水体颗粒物分布特征及其与环境因子的关系研究

研究了厦门湖边水库、石兜-坂头水库水体颗粒物的分布特征及其与环境因子之间的关系。结果表明:(1)水体颗粒物平均含量以坂头库区最高,石兜库区次之,湖边水库最低,平均含量分别为31.9、27.7和23.1mg/L;在空间分布上,不同水库或库区、不同采样站位间,由于水体颗粒物的来源成因不同,其分布规律呈现出明显的差异。(2)从水体颗粒物与环境因子的关联度分析,湖边水库及石兜-坂头水库两个库区的水体颗粒物与总氮和总磷都有较大关联性。(3)利用Pearson积矩相关系数(两尾)进行检验,湖边水库及石兜-坂头水库两个库区的水体颗粒物均与总氮呈显著或极显著相关,与透明度呈显著负相关,与叶绿素a均呈负相关,与其它因子的相关规律性不明显。(4)水体颗粒物与环境因子的逐步回归分析表明,在不同的水库或库区,对水体颗粒物有显著影响的环境因子各不相同,湖边水库是高锰酸盐指数和总氮,石兜库区是高锰酸盐指数、总氮和总磷,坂头库区是pH、溶解氧和总磷。     

Determination of ultra-trace amounts of cadmium by ET-AAS after column preconcentration with a new sorbent of modified MWCNTs

The present research reports on the application of modified multiwalled carbon nanotubes as a new, easily prepared, and stable solid sorbent for the column preconcentration of ultra-trace amounts of cadmium in aqueous solution. Multiwalled carbon nanotubes were oxidized with concentrated HNO₃ and modified with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol and then were used as a solid phase for the column preconcentration of Cd(II). Elution was carried out with 0.5 mol?L^?1 HNO₃. The amount of eluted Cd(II) was measured using electrothermal atomic absorption spectrometry. Various parameters such as pH, sample and eluent flow rate, eluent concentration, breakthrough volume, and interference of a great number of anions and cations on the retention of analyte on sorbent were studied. Under the optimized conditions, the calibration graph was linear in the range of 0.67 ng?L^?1 to 5.0 μg?L^?1 and the detection limit (3S_b, n?=?7) was 0.14 ng?L^?1 in initial solution. A preconcentration factor of 300 and relative standard deviations of ±3.6 % for seven successive determinations of 3 ng of Cd(II) were achieved. The column preconcentration was successfully applied to the analysis of river water, waste water, and Persian Gulf water sample.     

Flow injection online spectrophotometric determination of uranium after preconcentration on XAD-4 resin impregnated with nalidixic acid

In this work, spectrophotometer was used as a detector for the determination of uranium from water, biological, and ore samples with a flow injection system coupled with solid phase extraction. In order to promote the online preconcentration of uranium, a minicolumn packed with XAD-4 resin impregnated with nalidixic acid was utilized. The system operation was based on U(VI) ion retention at pH 6 in the minicolumn at flow rate of 15.2 mL min^?1. The uranium complex was removed from the resin by 0.1 mol dm^?3 HCl at flow rate of 3.2 mL min^?1 and was mixed with arsenazo III solution (0.05 % solution in 0.1 mol dm^?3 HCl, 3.2 mL min^?1) and driven to flow through cell of spectrophotometer where its absorbance was measured at 651 nm. The influence of chemical (pH and HCl (as eluent and reagent medium) concentration) and flow (sample and eluent flow rate and preconcentration time) parameters that could affect the performance of the system as well as the possible interferents was investigated. At the optimum conditions for 60 s preconcentration time (15.2 mL of sample volume), the method presented a detection limit of 1.1 μg L^?1, a relative standard deviation (RSD) of 0.8 % at 100 μg L^?1, enrichment factor of 30, and a sample throughput of 42 h^?1, whereas for 300 s of the preconcentration time (76 mL of sample volume), a detection limit of 0.22 μg L^?1, a RSD of 1.32 % at 10 μg L^?1, enrichment factor of 150, and a sampling frequency of 11 h^?1 were reported.     

Solid phase extraction and determination of Cr(III) by spectrophotometry using cefaclor as a complexing reagent and FAAS

The present study reports on the application of modified groundnut shell as a new, easily prepared, and stable sorbent for the extraction of trace amount of Cr(III) in aqueous solution. 2-Hydroxybenzaldiminoglycine was immobilized on groundnut shells in alkaline medium and then used as a solid phase for the column preconcentration of Cr(III). The elution was carried out with 3 mL of 2 mol?L^?1 HCl. The amount of eluted Cr(III) was determined by spectrophotometry using cefaclor as a complexing reagent and by flame atomic absorption spectrometry (FAAS). Different experimental variables such as pH, amount of solid sorbent, volume and concentration of eluent, sample and eluent flow rate, and interference of other metal ions on the retention of Cr(III) were studied. Under the optimized conditions, the calibration curves were found to be linear over the concentration range of 13–104 and 10–75 μg?L^?1 with a detection limit of 3.64 and 1.24 μg?L^?1 for spectrophotometric method and FAAS, respectively. An enrichment factor of 200 and RSD of ±1.19–1.49 % for five successive determinations of 25 μg?L^?1 were achieved. The column preconcentration was successfully applied to the analysis of tap water and underground water samples.     

Mobilization of aluminum by the acid percolates within unsaturated zone of sandstones

The area of the Black Triangle has been exposed to extreme levels of acid deposition in the twentieth century. The chemical weathering of sandstones found within the Black Triangle became well-known phenomenon. Infiltration of acid rain solutions into the sandstone represents the main input of salt components into the sandstone. The infiltrated solutions–sandstone percolates–react with sandstone matrix and previously deposited materials such as salt efflorescence. Acidic sandstone percolates pH?3.2–4.8 found at ten sites within the National Park Bohemian Switzerland contained high Al-tot (0.8–10 mg?L^?1) concentrations and high concentrations of anions SO₄ (5–66 mg?L^?1) and NO₃ (2–42 mg?L^?1). A high proportion (50–98 %) of Al-tot concentration in acid percolates was represented by toxic reactive Alⁿ⁺. Chemical equilibrium modeling indicated as the most abundant Al species Al³⁺, AlSO₄ ⁺, and AlF²⁺. The remaining 2–50 % of Al-tot concentration was present in the form of complexes with dissolved organic matter Al-org. Mobilization and transport of Al from the upper zones of sandstone causes chemical weathering and sandstone structure deterioration. The most acidic percolates contained the highest concentrations of dissolved organic material (estimated up to 42 mg?L^?1) suggesting the contribution of vegetation on sandstone weathering processes. Very low concentrations of Al-tot in springs at BSNP suggest that Al mobilized in unsaturated zone is transported deeper into the sandstone. This process of mobilization could represent a threat for the water quality small-perched aquifers.     

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS)

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L^-1 HNO₃ and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L^?1 and 3.91 μg L^?1, respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.     

Multiple metal tolerance and biosorption of cadmium by Candida tropicalis isolated from industrial effluents: glutathione as detoxifying agent

The ability of cadmium uptake by metal-resistant yeast, Candida tropicalis, from the liquid medium and wastewater was evaluated. The minimum inhibitory concentration of Cd^2?+? against C. tropicalis was 2,500 mg L^???1. The yeast also showed tolerance toward Zn^2?+? (1,400 mg L^???1), Ni^2?+? (1,000 mg L^???1), Hg^2?+? (1,400 mg L^???1), Cu^2?+? (1,000 mg L^???1), Cr^6?+? (1,200 mg L^???1), and Pb^2?+? (1,000 mg L^???1). The yeast isolate showed typical growth curves, but lag and log phases extended in the presence of cadmium. The yeast isolate showed optimum growth at 30°C and pH 8. The metal processing ability of the isolate was determined in a medium containing 100 mg L^???1 of Cd^2?+?. C. tropicalis could decline Cd^2?+? 70%, 85%, and 92% from the medium after 48, 96, and 144 h, respectively. C. tropicalis was also able to remove Cd^2?+? 40% and 78% from the wastewater after 6 and 12 days, respectively. Cd produced an increase in glutathione (GSH) and nonprotein thiol levels by 135% and 134% at 100-mg L^???1 concentration, respectively. An increase in the synthesis of GSH is involved in metal tolerance, and the presence of increasing GSH concentrations may be a marker for high metal stress in C. tropicalis. C. tropicalis, which is resistant to heavy metal ions and is adaptable to the local environmental conditions, may be employed for metal detoxification operations.