超声波提取-恒波长同步荧光法测定淡水藻中叶绿素a的含量

针对绿藻,采用超声波提取,以荧光激发-发射波长差216nm,建立了同步荧光法测定绿藻叶绿素a含量的新方法,其线性范围为0.02～1.25 mg/L,检出限为1.6ug/L,加标回收率在97.0%～104%之间。与分光光度法测定叶绿素a的对比试验结果表明,两者无显著性差异,但该方法具有快速、灵敏,其他常见色素不干扰测定的优点,能够满足供水中绿藻叶绿素a含量快速检测的需要。     

ASE—GPC—GC—MS快速分析土壤中的PAHs

建立了土壤中多环芳烃的气相色谱—质谱联用的快速检测方法。样品经过加速溶剂萃取、凝胶色谱净化、GC—MS分离测定,优化了加速溶剂萃取和凝胶色谱净化的条件。结果表明,多环芳烃的平均回收率为82.1%~106.4%,相对标准偏差为1.2%~4.8%。方法具有灵敏度高、准确度好、快速、消耗溶剂少的优点,适用于土壤等固体样品中多环芳烃的分离、净化和分析。     

Supercritical Fluid Extraction for Forensic Analysis of Hydrocarbons in Soil

Supercritical fluid extraction (SFE) was investigated to evaluate its potential for obtaining high quality chromatographic fingerprints from soils encountered in environmental investigations. While the volatile and semivolatile fractions of light nonaqueous phase liquid (LNAPL) samples can be “fingerprinted” in a single chromatographic run, it is commonly not possible to obtain samples of LNAPL in the locations of interest. For this and other reasons, it was desirable to develop this method (SFE) of soil extraction, which allows chromatographic fingerprinting of the same quality routinely obtained with LNAPL so that environmental forensic investigations could be extended to areas beyond those containing LNAPL in monitoring wells. In this study, SFE was compared to conventional dichloromethane extraction. Both artificially spiked soil and soil from petroleum release sites were tested. Since water can be a problem when using the SFE method, particular attention was given to handling soils with high moisture contents. The SFE extracts showed excellent retention of low molecular components, including pentanes. Gas chromatography of SFE extracts yielded molecular distributions that showed no significant bias toward either low or high molecular weight components. These results show that SFE can be used to obtain an unbiased, single-run chromatographic “fingerprint” of both volatile and semivolatile hydrocarbons in contaminated soil samples.     

广州市“南肺”果园土壤H g和A s的形态分析

采用Tessier连续提取法、BCR连续提取法和Leleyter连续提取法,研究广州"南肺"果园土壤Hg和As的形态分布和生物可给性。结果表明,果园土壤Hg和As形态分布都以残渣态为主;3种方法的土壤生物可给性分析均表明,Hg和As生物可利用态的含量较少;生物不可利用态是主要形态,其次是潜在可利用态。     

SPME-G C法测试TCE、PCE条件的正交优化试验研究

运用正交设计方法对SPME-GC法测试三氯乙烯、四氯乙烯的固相微萃取条件进行优化。首先选择样品量、NaCl用量、萃取温度、萃取时间、解析温度等因素,设计5因素3水平正交试验方案。分析数据得到优化条件为NaCl用量30 g/L,萃取温度25℃,解析温度210℃,同时得出样品量与萃取时间是对试验结果具有显著意义的影响因素,采用二次回归正交组合设计试验对其进一步优化,并对结果进行回归分析,得到最优条件为样品量为5.5 mL,萃取时间为20.13 min。     

沸石负载介孔TiO_2的制备及其可见光催化性能研究

以人工沸石为载体,采用溶胶-凝胶法,制备出了沸石负载介孔改性TiO2光催化剂。以亚甲基蓝为目标污染物,研究了不同掺杂金属及介孔薄膜制备方法对纳米TiO2可见光催化性能的影响。用扫描电镜(SEM)、紫外-可见吸收光谱(UV-vis)等手段研究了掺杂改性前后TiO2的变化。研究发现,N-Fe掺杂可使催化剂的光吸收谱带红移。当掺杂Fe的比为0.2%,焙烧温度为500℃时制备的TiO2效果最好,在可见光照射2 h后,亚甲基蓝的去除率可达90%。研究表明经十六烷基三甲基溴化铵(CTAB)作为模板剂修饰后的TiO2催化效果有明显提高,通过将经过萃取去除模板剂的共掺TiO2和直接高温焙烧的TiO2对比后发现,前者比后者降解亚甲基蓝的效果要好,原因在于,高温直接焙烧去除模板剂很容易使模板剂形成的骨架塌陷,减小了比表面积,从而影响了其光催化性能。     

OBIA与RF结合的龙口市土地利用信息提取方法

为提高中分辨率遥感影像解译精度,本文提出面向对象影像分析（Object Based Image Analysis,OBIA）与随机森林（Random Forest,RF）结合的土地利用信息提取方法。采用Landsat 8 OLI影像,针对不同地物特点,阈值分割和多尺度分割结合创建影像对象,规则集和分类器协同分类,基于Relief F算法分别对光谱特征、纹理特征及所有特征降维筛选特征子集,并与全部特征一起应用RF建模,对龙口市进行土地利用信息提取与比较。结果表明：OBIA与RF结合提取土地利用信息,基于Relief F算法筛选纹理特征,保留完整光谱、几何、空间关系特征构建RF模型,建模错分率为0.0958,分类总体精度和Kappa系数分别为89.37%和0.872,取得较理想结果。该方法可应用于中分辨率遥感影像土地利用信息提取。     

Selective extraction and separation of Fe, Mn oxides and organic materials in river surficial sediments

In order to investigate the adsorption mechanism of trace metals to surficial sediments （SSs）, a selective extraction procedure was improved in the present work. The selective extraction procedure has been proved to selectively remove and separate Fe, Mn oxides and organic materials （OMs） in the non-residual fraction from the SSs collected in Songhua River, China. After screening different kinds of conventional extractants of Fe and Mn oxides and OMs used for separation of heavy metals in the soils and sediments, NH2OH .HCl （0.1 mol/L） ＋ HNO3 （0.1 mol/L）, （NH4）2C2O4 （0.2 mol/L） ＋ H2C2O4 （pH 3.0）, and 30% of H2O2 were respectively applied to selectively extract Mn oxides, Fe/Mn oxides and OMs. After the extraction treatments, the target components were removed with extraction efficiencies between 86.09%--3.36% for the hydroxylamine hydrochloride treatment, 80.63%- 101.09% for the oxalate solution extraction, and 94.76%-102.83% for the hydrogen peroxide digestion, respectively. The results indicate that this selective extraction technology was effective for the extraction and separation ofFe, Mn oxides and OMs in the SSs, and important for further mechanism study of trace metal adsorption onto SSs.     

Investigation on Fe, Mn, Zn, Cu, Pb and Cd fractions in the natural surface coating samples and surficial sediments in the Songhua River, China

Natural surface coating samples （NSCSs） from the surface of shingles and surficial sediments （SSs） in the Songhua River, China were employed to investigate the relationship between NSCSs and SSs in fractions of heavy metals （Fe, Mn, Zn, Cu, Pb, and Cd） using the modified sequential extraction procedure （MSEP）. The results show that the differences between NSCSs and SSs in Fe fi＇actions were insignificant and Fe was dominantly present as residual phase （76.22% for NSCSs and 80.88% for SSs） and Fe-oxides phase （20.33% for NSCSs and 16.15% for SSs）. Significant variation of Mn distribution patterns between NSCSs and SSs was observed with Mn in NSCSs mainly present in Mn-oxides phase （48.27%） and that in SSs present as residual phase （45.44%）. Zn, Cu, Pb and Cd were found dominantly in residual fractions （〉48%）, and next in solid oxides/hydroxides for Zn, Pb and Cd and in easily oxidizable solids/compounds form for Cu, respectively. The heavy metal distribution patterns implied that Fe/Mn oxides both in NSCSs and SSs were more important sinks for binding and adsorption of Zn, Pb and Cd than organic matter （OM）, and inversely, higher affinity of Cu to OM than Fe/Mn oxides in NSCSs and SSs was obtained. Meanwhile, it was found that the distributions of heavy metals in NSCSs and SSs were similar to each other and the pseudo-total concentrations of Zn, Cu, Pb and Cd in NSCSs were greater than those in SSs, highlighting the more importance for NSCSs than SSs in controlling behaviours of heavy metals in aquatic environments.     

Broad range analysis of endocrine disruptors and pharmaceuticals using gas chromatography and liquid chromatography tandem mass spectrometry

Endocrine disrupting compounds (EDCs) and pharmaceuticals and personal care products (PPCPs) have been globally detected in impacted natural waters. The detection of trace quantities of EDCs and PPCPs in the environment is of great concern since some of these compounds have known physiological responses at low concentrations. EDCs can have a wide range of polarities, acidic and basic moieties, and exist in trace quantities, which often requires numerous complex extractions, large sample collection volumes, and multiple instrumental analyses. A comprehensive method has been developed allowing for the analysis of 58 potential EDCs in various water matrices using a single solid-phase extraction (SPE) of a 1 L sample with subsequent analyses using both gas chromatography and liquid chromatography, each coupled with tandem mass spectrometry (GC–MS/MS and LC–MS/MS). Instrument detection limits ranged between 0.12–7.5 pg with corresponding method reporting limits of 1–10 ng l⁻¹ in water. Recoveries for most compounds were between 50% and 112% with good reproducibility (RSD 6–22%).