土壤中酞酸酯类化合物监测方法的质量控制研究

从监测结果控制的角度对近10年的土壤中PAEs监测方法进行了探讨,重点比较了索氏萃取柱净化GC/MS、微波萃取柱净化GC、加速溶剂萃取柱净化GC/MS和加速溶剂萃取GPCGC/MS方法的检出限、精密度和准确度。旨在为中国土壤监测方法的建立提供基础支撑,为开展质量控制工作提供评价依据。     

环境监测实验室方法确认过程中常见问题探讨

根据实验室资质认定对于方法确认的要求,结合环境监测实验室的特点,提出了新项目方法确认的具体步骤,并分析了其中存在的常见问题。指出在方法确认过程中,应严格按照标准方法和监测技术规范进行全过程试验,尤其不能忽视采样现场实验、空白实验和检出限的测定。建议在精密度与准确度检验过程中,使用高、中、低不同浓度的有证标准样品,实际样品加标回收,比对试验（方法比对、人员比对、实验室间比对）,增加分析次数等多种手段,确保新项目开展的可靠性。     

两种吹扫捕集浓缩仪在测定土壤VOCs时的性能比较

从仪器精密度、方法检出限、准确度等角度对吹扫捕集浓缩仪Stratum PTC与Eclipse 4660的性能进行比较。结果表明,大部分分析物用Stratum PTC的方法检出限略高于Eclipse 4660,但精密度比Eclipse 4660稍差;Eclipse 4660用于分析极性的、水溶性物质的效果比Stratum PTC好,回收率更高。两种吹扫捕集仪的测试结果均满足《土壤和沉积物挥发性有机物的测定吹扫捕集/气相色谱-质谱法》(HJ 605-2011)标准方法的指标要求。     

利用重组大肠杆菌SOS法评价污水厂出水的遗传毒性以及工艺去除效果

SOS/umu测试法被广泛应用于化合物和复杂混合物遗传毒性的评价,由于该技术所用菌种为致病菌且操作步骤繁琐等原因,制约了技术的推广应用。研究建立了基于重组大肠杆菌SOS效应的水质遗传毒性检测方法(专利号:ZL201110022476.1),应用该方法评价了某市4座污水厂出水的直接遗传毒性效应,同时以污水处理一厂为例考察了直接遗传毒性效应的季节变化规律以及不同的工艺对水中直接遗传毒性物质的去除情况。结果显示:各污水厂出水均表现出一定的直接遗传毒性,对应的4-NQO毒性当量浓度范围为0.018~0.514 mg·L-1;一年四季中夏季进出水直接遗传毒性效应最高,现有工艺中生化处理工艺段对直接遗传毒性去除效果最佳,去除率为33.33%。该方法操作便利、检测敏感性较高、操作危险性较低,可用于水中直接遗传毒性效应的测试。     

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%.     

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。     

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.     

福建省生产废水和生活污水污染物排放的驱动力及其时空分异

采用对数平均迪氏指数方法,区分生产和生活两个体系,构建时空分解分析模型,追踪了福建省9个设区市2011—2019年水污染物排放变化的关键驱动力及其贡献的时空差异.结果显示：研究期内福建省工业废水污染物排放持续减少,并且各驱动力贡献的区域差距明显变小,趋于平衡;生活污水污染物排放量仍保持高位,各驱动力贡献的区域差距基本保持不变.其中,经济规模扩张是福建省水污染物排放的主导驱动力,主要源于福州、厦门、泉州经济赶超发展影响;城镇化发展对区域生活污水污染物排放的驱动影响表现为增排效应,以福州和厦门尤为显著;工业化发展对区域工业废水污染物排放的影响效应由正驱动逐渐转变为负驱动,这主要归功于三明和泉州产业结构调整优化的拉动 效应;技术效应一直是福建省水污染物排放控制的重要驱动力,但部分地区已逐渐步入生活污染物技术减排攻坚期.