重金属离子-二乙基二硫代氨基甲酸钠螯合体系的HPLC分析方法研究

采用二乙基二硫代氨基甲酸钠(NaDDC)为螯合剂,对Cu(Ⅱ)、Hg(Ⅱ)、Pb(Ⅱ)、Zn(Ⅱ)、Cd(Ⅱ)、Cr(Ⅵ)六种重金属离子进行了螯合萃取分离体系的方法研究,用HPLC方法建立了上述金属离子的最佳分离条件及定性定量分析方法.结果表明,用C18反相柱(5μm,150×4.6mmi.d.)和流动相(V(乙腈):V(甲醇):V(水)=55:15:30)能有效分离上述重金属离子,最低检测限在0.1～1.6ng范围内,线性范围及线性关系满足定量分析要求.     

Flame Propagation Across Gelled Alkane-In-Water Emulsions

Flame propagation rates were measured for flames spreading across surfaces of gel-like alkane-in-water emulsions. A long, slender, water-cooled trough was used to contain the mixtures. Abrupt changes in the flame propagation velocities - of nearly two orders of magnitude - were observed to occur near ‘critical’ concentrations of certain alkane/water mixtures. Four alkanes were used - pentane, hexane, heptane, and octane - and fuel rich emulsions (in which water was the continuous phase) were employed. The ability of the aqueous phase of the emulsion to inhibit the release of fuel into the vapor phase plays an important role in the observed behavior. That is, the rate at which fuel can diffuse through both the emulsion and the thin liquid layers that reside on it, is an essential kinetic aspect of the phenomena which determine the flame propagation rate across gelled alkane-in-water emulsions.     

石油石化挥发性有机液体装载源项VOCs排放管控现状及减排策略建议

综合消费量、真实蒸气压和单物质最大增量反应活性 (MIR) 等影响挥发性有机物 (VOCs) 光化学反应的关键因素,筛选10种大宗挥发性有机液体,对其载运工具、装载方式、装载环节VOCs排放和治理现状进行调研。结果显示,10种大宗挥发性有机液体整体以汽车装载为主,其次为船舶和火车,占比依次为53.6%、26.5%、19.8%;汽车装车基本建成油气回收,多数实现底部装载;火车装车油气回收较为普遍,但全部为上装,收集效率较低;装船建成油气回收设施较少。根据装载源项VOCs的治理现状、标准要求及减排潜力分析,提出我国当前装载环节VOCs减排策略：原油是目前装载环节重点管控物质,应加快各类装载方式油气回收进程;装载工具方面,应加快装船VOCs治理进度;治理措施方面,应重点加强VOCs收集效果的优化和监管。本研究可为我国石油石化领域装载环节的VOCs污染管控提供参考。     

醇胺离子液体对烟气硫的高效脱除

燃煤烟气中的SO2对人体健康和生态环境危害很大,传统的除硫装置大都存在二次污染。离子液体作为新型吸收剂有着广泛的应用前景。制备柠檬酸三乙醇胺离子液体作为脱硫剂,在模拟烟气条件下对SO2的吸收性能进行研究。结果表明：柠檬酸三乙醇胺离子液体具有高效脱硫性能,在70 min时脱硫率仍能达到80%以上;温度升高不利于脱硫过程的进行;而SO2浓度增加,离子液体的吸收量增加;离子液体的解吸工艺简单,在90 ℃下加热80 min可完全解吸,再生性能良好。柠檬酸三乙醇胺离子液体对SO2的吸收主要以化学吸收为主,同时伴有物理吸收过程,吸收摩尔比达到3.38～3.68 mol·mol-1。     

冠醚-离子液体体系对水相中铀酰离子的萃取

以二环己基-18-冠醚-6（DCH18C6）为萃取剂,一系列离子液体为溶剂的冠醚-离子液体萃取体系对水相中铀酰离子（UO22+）进行萃取实验。结果表明：UO22+在1-丁基-3-甲基咪唑双三氟磺酰亚胺盐（NTf2）体系的去除效率明显高于六氟磷酸盐类（PF6-）离子液体。在水相中当硝酸浓度在3 mol·L-1左右时萃取效率最高,体系的萃取效率随着萃取剂浓度的增加而变大,共存离子的加入会降低体系的萃取效率,但是当加入的是硝酸根离子时,萃取率会相应增大。根据实验结果分析可以判断此萃取体系主要为阳离子交换过程。     

中型污水处理厂中药物和个人护理品的分布与去除

为了解15种药物及个人护理用品(PPCPs)在中小型污水处理厂中的分布及其去除效果,采用液相色谱-串联质谱(LC-MS/MS)技术对3座A2/O工艺的污水处理厂水样进行分析研究。结果显示,除普萘洛尔、吉非罗平和吲哚美辛在3座中小型污水处理厂各个工艺单元中均未被检出外,其余12种目标化合物的检出频率在90%~100%之间。进水水样中PPCPs的平均检出浓度为2 285.4 ng/L,其中咖啡因(CF)的平均检出浓度最高为973.3 ng/L,酮洛芬(KP)的平均检出浓度次之为844.7 ng/L,两者之和占进水水样中PPCPs平均含量的79.5%,表明污水处理厂的主要污染物为CF和KP。3座污水处理厂对CF的去除效果最为显著,平均去除率为95.3%,对15种PPCPs总去除效率在39.3%~82.8%之间。     

高效液相色谱-串联质谱法同时检测地表水中13种药物及个人护理品

采用高效液相色谱-串联质谱(HPLC-MS/MS)检测,建立了地表水中13种药物及个人护理品的测定方法。水样用盐酸与氢氧化钠溶液调pH值至7.0左右,过固相萃取小柱进行富集,用14 mL甲醇洗脱。以C18柱为分离柱,0.01%甲酸的甲醇-0.01%甲酸水溶液为流动相,目标物在10 min内分离,在0.50~250 μg/L范围内,13种化合物峰面积与内标物质峰面积之比与质量浓度的线性关系良好(>0.99),检出限在0.05~0.5 ng/L范围内。基质加标实验结果表明,13种化合物在水中的回收率分别在56.2%~123.2%之间(加标水平5 ng/mL)和58.0%~107.8%(加标水平50 ng/mL),相对标准偏差在1.60%~19.9%(n=6)之间。应用该方法测定了从2条纳污河流采集的10份水样,结果表明,除美托诺尔和普洛萘尔未被检出外,其余11药物的检出频率在30%~100%之间。在13种目标物质中,咖啡因的检测浓度最高达287.5 ng/L,舒必利次之,为277.5 ng/L。本方法快速、准确,适用于地表水中PPCPs类的快速测定。     

通过式固相萃取/超高效液相色谱-串联质谱法测定蔬菜中18种农药残留

建立了超高效液相色谱-串联质谱(UPLC-MS;MS)快速测定蔬菜中18种农药残留的方法.样品经乙腈提取后,经Oasis PRiME HLB固相萃取柱净化,采用ACQUITY UPLC HSS T3 C18(50 mm×2.1 mm,1.8μm)色谱柱进行分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱.采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定性和定量分析.结果表明,18种农药在0.5—50μg·L^-1范围内线性关系良好(r2>0.995),方法最低检出限为0.4—1.5μg·kg^-1,最低定量限为1.4—5.0μg·kg^-1.在韭菜、芹菜、番茄、白菜基质中,5、10、50μg·kg^-1添加水平下的加标回收率为60.2%—126.9%,相对标准偏差(RSD)为0.4%—21.6%(n=3).     

Ein Indikator für den Einsatz gef?hrlicher Stoffe in Produkten und Prozessen: Monoethylenglykol-?quivalente

Zusammenfassung  Zur Quantifizierung des Gefahrstoffeinsatzes in der Produktion ist im Rahmen der integrierten ?kologischen Bewertung des ?ko-Institutes (EcoGrade) eine eigene Methodik entwickelt worden. Indikator für den Gefahrstoffeinsatz sind Monoethylenglykol (‘MEG’)-?quivalente. Sie erm?glichen einen direkten, schadstoffbezogenen Prozess- und Produktvergleich (Bunke 2001). Die Bewertung basiert auf den R-S?tzen (Gefahrenhinweise) der Inhaltsstoffe. Die Methodik der MEG-?quivalente stellt eine Weiterentwicklung und Anwendung des Wirkfaktorenmodells der Technischen Regel für Gefahrstoffe (TRGS) 440 dar (AGS 2001). Die zur Bewertung erforderlichen Daten sind im Unternehmen vorhanden (Sicherheitsdatenbl?tter) bzw. ?ffentlich leicht zug?nglich (Gefahrstoffdatenbanken). Die Bilanzierung von Gefahrstoffen mit Hilfe der hier vorgestellten Methode erm?glicht es auch, in ?kobilanziellen Untersuchungen systematisch den Gefahrstoffeinsatz zu berücksichtigen. Die Methodik ist am Beispiel von Wohngeb?uden erprobt worden. Anmerkung: Als Gefahrstoffe, Schadstoffe, gef?hrliche Inhaltsstoffe bzw. gef?hrliche Stoffe werden in dieser Arbeit solche Stoffe definiert, die eines der Gef?hrlichkeitsmerkmale nach § 3 Chemikaliengesetz besitzen. OnlineFirst: 19. 12. 2001     

Laboratory evidence of natural remobilization of multicomponent DNAPL pools due to dissolution

Mixtures of dense non-aqueous phase liquids (DNAPLs) trapped in the subsurface can act as long-term sources of contamination by dissolving into flowing groundwater. In general, the components of higher solubility are removed more quickly, thus altering the composition of the remaining DNAPL, and possibly leading to changes in its physical properties. Through the development of a simple compositional model, Roy et al. [J. Contam. Hydrol. 2002 (59) 163] showed that preferential dissolution of a mixed DNAPL could potentially result in changes in density and interfacial tension that could subsequently lead to remobilization of an initially static DNAPL pool. The laboratory experiments presented in this next paper provide a proof-of-concept for the previously presented theory, demonstrating and quantifying this process of remobilization. In addition, the experiments provide a data set for evaluation of the model presented by Roy et al. [J. Contam. Hydrol. 2002 (59) 163]. In the four experiments, a DNAPL pool comprised of tetrachloroethene and benzene was created as an open pool overlying glass beads within a water-saturated 2-D flow box. Experiments included rectangular and triangular pools. In each of the experiments, remobilization (as breakthrough) was observed more than 2 weeks after formation of the initial pool. During each experiment, the pool height declined as mass was lost by dissolution, while sampling indicated a decrease in the mole fraction of benzene, the more soluble component. Small protuberances formed along the bottom of the pool as its composition changed with time and the displacement pressure was achieved for various pore throats. Eventually one of the protuberances extended further, forming a finger (breakthrough). In general, the pool emptied as the finger proceeded further into the beads. It was also shown theoretically and experimentally that remobilization will occur sooner for pools with a triangular (pointing down), rather than rectangular, shape. The experimental results were simulated using the model developed by Roy et al. [J. Contam. Hydrol. 2002 (59) 163]. The model matched the observations well, suggesting that it accurately represents the primary mechanisms involved with natural remobilization under the conditions of the study.