Development of Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Drop for the Determination of Trace Lead in Water

A new method for determining lead (Pb) content was developed by dispersive liquid–liquid microextraction based on the solidification of floating organic droplets followed by flame atomic absorption spectrometry. Under optimum conditions, the calibration graph was linear within the Pb content range of 8.43–400 µg L^?1 with a detection limit of 2.53 µg L^?1. The relative standard deviation for 10 replicate measurements of 20 and 400 µg L^?1 of Pb were 3.41 and 2.78%, respectively. The proposed method was assessed through the analysis of certified reference water and recovery experiments.     

矿渣磷酸镁水泥的力学性能和水化机理

以高炉矿渣作为磷酸镁水泥(MPC)的活性混合材料,研究了MPC的凝固时间、力学性能、物相组成和显微结构,并探讨了矿渣MPC的作用机理。实验固定磷镁比为25%,硼镁比为7.5%,矿渣掺量分别为磷镁总质量的0%、10%、20%、30%和40%。结果表明,矿渣参与了水化反应并提高了MPC的胶凝性能,随着矿渣掺量增大,矿渣MPC的抗压强度提高,但矿渣水化产生的膨胀应力会破坏MPC的内部结构,因此其抗折强度随矿渣掺量增大而降低。矿渣MPC的主要水化产物为六水合磷酸镁铵(MgNH4PO4.6H2O),矿渣的掺入使凝胶相增加,并有部分Ca2+进入MgNH4PO4.6H2O晶格,使水化产物的形貌、大小发生变化。样品中剩余较多死烧镁和矿渣颗粒,可起骨料作用。     

浙南海域腹泻性贝毒分析

在浙南海域共采集了10种贝类40份样品.运用高效液相色谱方法检测腹泻性贝毒,共检出 9份样品含有腹泻性贝毒.染毒样品检出的腹泻性贝毒(软海绵酸,OA)质量比为0.07～5.85 μg/g,共有7个样品含量超标,超标率为17.5%.无论是检出率还是超标率,都呈现夏季>春季>秋季的规律.浙南海域的南部腹泻性贝毒检出率和超标...     

土壤—水悬浊液体系全量置入红外光度法测定土壤中的总石油烃

从考虑土壤本身复杂性而引起的基体效应出发,建立了土壤—水悬浊液体系以探求更合理可靠的土壤总石油烃测定的前处理过程.研究了土壤—水悬浊液体系中以CCl4为萃取剂全量置入提取土壤中总石油烃(TPH)红外光度法(IR)测定的可行性及其影响因素,阐明了应用该体系提取总石油烃的优化条件为:当水土比例(V/m)为12.5∶1、振荡...     

文蛤(Meretrix meretrix)体内氨基脲含量与环境相关性研究

采用超高效液相色谱-串联质谱法进行了文蛤体内氨基脲含量与环境相关性研究。在(13±1)℃的水温条件下,将文蛤分别浸浴于氨基脲浓度1.0μg/L、5.0μg/L的海水中6天进行吸收试验,第7天起隔天换水进行消除试验,结果表明:文蛤对水体中氨基脲的富集能力较低,蓄积量随时间的延长和给药浓度的增加而增加。氨基脲在不同浓度中具有相似的消除规律:初始阶段均具有较高的消除速率,随后消除趋势趋于平缓,并在一段时间内维持一定质量分数;至试验结束时,低浓度组和高浓度组文蛤体内氨基脲最终降低至低于检出限(0.5μg/kg);本研究所得的药时曲线对贝类氨基脲污染的净化提供了数据支持。     

水产饲料中三聚氰胺检测方法的优化

通过对高效液相色谱法(HPLC)测定水产饲料中三聚氰胺含量的方法进行优化,得到最佳色谱条件和前处理方法,建立了水产饲料中三聚氰胺的检测方法。结果表明:以体积比8∶92的乙腈、庚烷磺酸钠离子对试剂为流动相,柱温40℃,流速1.2 mL/min,以波长236 nm检测;以提取液为18 mL50%(φ)乙腈水+1 mL乙酸锌+1 mL1mol/L盐酸,淋洗液3 mL水和3 mL甲醇,洗脱体积6 mL作样品前处理。三聚氰胺加标回收率为85%～100%,相对标准偏差(RSD)小于5%,线性范围为0.2 mg/L～5.0mg/L,相关系数0.999 8,方法检出限为0.2 mg/kg。     

Valorization of harbor dredged sediment activated with blast furnace slag in road layers

The valorization solutions for dredged sediment have been the subject of a great number of investigations over the previous decades.In the current present study,treatment of polluted dredged sediment fom the commercial port of Sfax,Tunisia,is proposed.An industrial byproduct(blast furnace slag)was used to bind raw sediment for a reuse in road engineering.Following standards of this field,the raw sediment first was identified and classified according to the French technical guidance.Then an environmental assessment was applied due to the presence of heavy metals.The concentrations were measured on the raw sediment particles so as to control the binding effect on heavy metals.Sediment mixtures consisted of a mix of sand and a blast furnace slag activated with quicklime.Different mixtures were tested and some were proposed for sub-layer applications.The Sfax commercial port raw sediment is considered as a sandy loam with a very low fraction of clay.The measured concentrations of heavy metals exceed the recommended thresholds for cadmium,copper,lead,and zinc.These can induce hazardous effects in the case of their dumping into the sea.On the other hand,the concentrations of the detected elements after leaching tests run on raw sediment samples are very low compared to the thresholds;such results highlight a possible recycling of the raw sediment in subgrade layers without any negative impact.Suitable formulations were deduced for road engineering tests relying on the ratio the California Bearing Ratio index and the immediate bearing index.If the obtained ratio exceeds one,the treated sediment can be recycled and used in road layers.     

The Ore-forming Mechanism of the Jiajika Pegmatite-Type Rare Metal Deposit in Western Sichuan Province:Evidence from Isotope Dating

Granitic pegmatites are commonly thought to form by fractional crystallization or by liquid immiscibility of granitic magma;however,these proposals are based mainly on analyses of fluid and melt inclusions.Here,we use the Jiajika pegmatite deposit,the largest spodumene deposit in Asia,as a case study to investigate ore forming processes using isotope dating.Dating of a single granite sample from the Jiajika deposit using multiple methods gave a zircon U-Pb SHRIMP age of 208.4±3.9 Ma, an ⁴⁰Ar/³⁹Ar age for muscovite of 182.9±1.7 Ma,and an ⁴⁰Ar/³⁹Ar age for biotite of 169.9±1.6 Ma. Based on these dating results and the ⁴⁰Ar/³⁹Ar age of muscovite from the Jiajika pegmatite,a temperature-time cooling track for the Jiajika granite was constructed using closure temperatures of the different isotope systems.This track indicates that the granite cooled over～40 m.y.,with segregation of the pegmatite fluid from the granitic magma at a temperature of～700℃.This result suggests that the Jiajika pegmatite formed not by fractional crystallization,but by segregation of an immiscible liquid from the granitic magma.When compared with fractional crystallization,the relatively early timing of segregation of an immiscible liquid from a granitic magma can prevent the precipitation of ore-forming elements during crystallization,and suggests that liquid immiscibility could be an important ore-forming process for rare metal pegmatities.We also conclude that isotope dating is a method that can potentially be used to determine the dominant ore-forming processes that occurred during the formation of granite-related ore deposits,and suggest that this method can be employed to determine the formation history of the W-Sn ore deposits found elsewhere within the Nanling Metallogenic Belt.     

A new extraction technique for in situ analyses of amino and carboxylic acids on Mars by gas chromatography mass spectrometry

In order to target key organic compounds in the Martian regolith using gas chromatography mass spectrometry (GC-MS), we have developed a new extraction procedure coupled with chemical derivatization. This new technique was tested on a Mars analog soil sample collected from the Atacama Desert in Chile. We found that amino and carboxylic acids can be extracted from the Atacama soil in a 1:1 mixture of isopropanol and water after ultrasonic treatment for 30 min. The extracted organic compounds were then derivatized in a single-step reaction using N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA) as the silylating agent in order to transform these compounds into volatile species that can then be detected by GC-MS. We are currently developing a miniaturized reaction cell suited for spaceflight, where both organic extraction and chemical derivatization processes can take place in a single step.