Method Development for Determination of Fluroxypyr in Soil

Abstract

Four methods were developed for the analysis of fluroxypyr in soil samples from oil palm plantations. The first method involved the extraction of the herbicide with 0.05 M NaOH in methanol followed by purification using acid base partition. The concentrated material was subjected to derivatization and then cleaning process using a florisil column and finally analyzed by gas chromatography (GC) equipped with electron capture detector (ECD). By this method, the recovery of fluroxypyr from the spiked soil ranged from 70 to 104% with the minimum detection limit at 5 µg/kg. The second method involved solid liquid extraction of fluroxypyr using a horizontal shaker followed by quantification using high performance liquid chromatography (HPLC) equipped with UV detector. The recovery of fluroxypyr using this method, ranged from 80 to 120% when the soil was spiked with fluroxypyr at 0.1–0.2 µg/g soil. In the third method, the recovery of fluroxypyr was determined by solid liquid extraction using an ultrasonic bath. The recovery of fluroxypyr at spiking levels of 4–50 µg/L ranged from 88 to 98% with relative standard deviations of 3.0–5.8% with a minimum detection limit of 4 µg/kg. In the fourth method, fluroxypyr was extracted using the solid liquid extraction method followed by the cleaning up step with OASIS® HLB (polyvinyl dibenzene). The recovery of fluroxypyr was between 91 and 95% with relative standard deviations of 4.2–6.2%, respectively. The limit of detection in method 4 was further improved to 1 µg/kg. When the weight of soil used was increased 4 fold, the recovery of fluroxypyr at spiking level of 1–50 µg/kg ranged from 82–107% with relative standard deviations of 0.5–4.7%.     

An Approach for Evaluating the Repeatability of Rapid Wetland Assessment Methods: The Effects of Training and Experience

We sampled 92 wetlands from four different basins in the United States to quantify observer repeatability in rapid wetland condition assessment using the Delaware Rapid Assessment Protocol (DERAP). In the Inland Bays basin of Delaware, 58 wetland sites were sampled by multiple observers with varying levels of experience (novice to expert) following a thorough training workshop. In the Nanticoke (Delaware/Maryland), Cuyahoga (Ohio), and John Day (Oregon) basins, 34 wetlands were sampled by two expert teams of observers with minimal protocol training. The variance in observer to observer scoring at each site was used to calculate pooled standard deviations (SD_pool), coefficients of variation, and signal-to-noise ratios for each survey. The results showed that the experience level of the observer had little impact on the repeatability of the final rapid assessment score. Training, however, had a large impact on observer to observer repeatability. The SD_pool in the Inland Bay survey with training (2.2 points out of a 0–30 score) was about half that observed in the other three basins where observers had minimal training (SD_pool = 4.2 points). Using the results from the survey with training, we would expect that two sites assessed by different, trained observers who obtain DERAP scores differing by more than 4 points are highly likely to differ in ecological condition, and that sites with scores that differ by 2 or fewer points are within variability that can be attributed to observer differences.     

OPTIMAL IDENTIFICATION OF MUSKINGUM ROUTING COEFFICIENTS1

Traditionally, identification of the Muskingum routing coefficients has been based on observations of the linearity of a loop formed by graphically plotting a forward and a reverse path. This graphical procedure is time-consuming and may not minimize the error of estimation. A procedure was developed to improve the drawbacks of the graphical method. This procedure calls for (a) the use of least square regression on the forward and reverse paths to determine their respective slopes, and (b) the use of statistical t-test to evaluate the hypothesis that these two slopes are equal. The computational procedure is repeated, using incremental values of the flow weighting coefficient, x. A graph of the computed t-value versus x can be constructed. The optimal value of x, as read from the graph, occurs at the minimum computed t-value. The procedure has been demonstrated superior to the graphical method for three illustrative examples, resulting in a reduction of the error squares by factors ranging from 5 to 6.     

基于道化学法的大型合成氨装置安全评价

根据道化学公司火灾、爆炸危险指数的基本原理。用VH6．0开发的安全评价软件DowSE1．0，对某大型合成氨装置进行安全评价，得出其安全措施补偿前后的火灾、爆炸指数F＆EI以及危险暴露面积，危害系数，危险等级，实际可能财产损失程度等指数。结果表明。合成氨装置中实际最大可能财产损失值都没有超过200万美元，气化系统在合成氨装置中实际最大可能财产损失值占损失替换值比例高达53％，超过了10％的相对危险值界限。说明在引进国外技术时应注重其安全防范配套措施消化吸收，并结合实际采取切实可行的安全措施，降低合成氨装置的风险程度。     

盲样考核浓度预判及稀释方法——以原子荧光法测定水中砷为例

以原子荧光法测定水中砷为例,探讨了实验室盲样考核浓度预判及稀释方法.分析了3个砷盲样考核实例,归纳了“直接稀释法”“系列稀释法”“最大稀释法”3种方法,分别适用于盲样浓度范围窄、适中、宽3种情况,检测人员可根据考核机构给定的浓度范围合理选用.     

高效液相色谱-原子荧光光谱联用分析土壤中形态砷

采用高效液相色谱(HPLC)-原子荧光光谱(AFS)联用技术分析土壤中亚砷酸盐[As(Ⅲ)]、二甲基砷(DMA)、一甲基砷(MMA)和砷酸盐[As(Ⅴ)]等4种形态砷,以磷酸为提取剂、抗坏血酸为还原剂,优化了水浴提取条件。As(Ⅲ)、DMA、MMA和As(Ⅴ)在7 min之内实现了完全分离,在1.00μg/L～100μg/L范围内线性良好,实验室检出限分别为0.25μg/L、0.36μg/L、0.39μg/L和0.51μg/L,土壤标准样品平行测定的RSD≤7.4%,加标回收率为79.5%～95.0%,提取率为74.6%～90.4%。     

IMS Method Performance Analyses for Giardia in Water Under Differing Conditions

Immunomagnetic separation (IMS) has been specified as a standard method for the measurement of Giardia under USEPA Method 1623. In this study, IMS was evaluated on the basis of recovery efficiencies for Giardia cysts under various IMS operation conditions. Significant change in recovery was observed by altering the debris ratio of water samples. Notably, cyst recovery efficiencies utilizing IMS dropped with increased turbidity, and results for varying dosages of magnetic beads and cysts indicate that 1 / 100 immunomagnetic beads is sufficient to conjugate large numbers of cysts. Changing vessel volume and replacing the sample buffer had no significant effect on cyst recovery efficiencies.     

纳污湿地上覆水中重金属的监测及评价

以武河湿地为研究区域采集上覆水水样,采用ICP-AES法测定湿地水体中重金属的含量,参照有关标准用水质标准级别法对水中重金属污染情况进行了评价。结果表明:武河湿地中重金属Hg污染十分严重,各采样点均有分布且水质属劣Ⅴ类。重金属元素Cd污染并不严重,总体水质较好。重金属元素As、Cr、Cu、Pb在武河湿地中污染较轻近乎无污染,水质为Ⅰ类。由于重金属Hg的污染十分严重所以研究区内综合质量等级在4以上,水质为Ⅴ类和劣Ⅴ类,污染严重。     

关于重量法测定硫酸盐化速率的不确定度分析

碳酸钾溶液浸渍过的玻璃纤维滤膜曝露于空气中,与空气中的二氧化硫、硫酸雾、硫化氢等发生反应,生成硫酸盐。测定生成的硫酸盐含量,计算硫酸盐化速率。不确定度的来源主要包括:样品重复性分析、电子天平称量等。评定结果为硫酸盐化速率的不确定度(2.90±0.06)(SO3),mg/(100cm2碱片·d),k=2。     

泰来县庄园式治沙做法及效益浅析

黑龙江省西部泰来县在典型风沙干旱区,环境极其恶劣的沙带上,通过多年的探索和实践,已创建了庄园式生态经济型治沙的有效成功模式,明显地改善了当地生产、生存、生态环境,同时取得了显著的经济效益和社会效益.