气相色谱测定沉积物中多氯联苯的样品处理方法研究

通过比较密闭微波萃取、超声波萃取、索氏提取3种方法对沉积物中多氯联苯(PCBs)提取效率,对比浓硫酸和Florisil小柱两种净化方式的净化效果,在实验基础上建立了密闭微波萃取-Florisil小柱净化-气相色谱(ECD)测定沉积物中多氯联苯的分析方法,加标质量比为0.2ng/g时,其相对标准偏差(RSD)为2.19%～8.71%,回收率为77.3%～94.6%,检出限为0.027～0.064ng/g。采用该方法对威海湾养殖区沉积物中PCBs进行了监测,结果表明本方法适用于海洋沉积物样品中PCBs的测定。     

Sources, pathways and sinks of particulate organic matter in Hudson Bay: Evidence from lignin distributions

Hudson Bay is a large, estuarine, shelf-like sea at the southern margin of the Arctic, where changes in seasonal ice cover and river discharge appear already to be underway. Here we present lignin data for dated sediments from eleven box cores and evaluate sources of terrigenous carbon, transport pathways, and whether terrigenous organic matter has been influenced by recent environmental change. Lignin yields (0.04 to 1.46 mg/100 mg organic carbon) decreased from the margin to the interior and from south to north, broadly reflecting the distribution of river inputs. Lignin compositional patterns indicated distinct regional sources with boreal forest (woody gymnosperm) vegetation an important source in the south, vs. tundra (non-woody angiosperm) in the north. Lignin patterns suggest redistribution of a fine-grained, mineral-associated fraction of the southern-derived terrigenous carbon to the northeast part of the Bay and ultimately into west Hudson Strait with the Bay's cyclonic coastal circulation. A small component of the carbon makes it to the central basins of Hudson Bay but most of the terrigenous organic material in that area appears to derive from resuspension of older, isostatically-rebounding coastal and inner shelf deposits. Most modern plant debris appears to be retained near river mouths due to hydrodynamic sorting, with the exception of the southwest inner shelf, where these materials extend > 30 km from shore. Temporal changes in the composition of terrigenous organic carbon recorded in most of the southern Hudson Bay cores perhaps reflect increases in erosion and cross-shelf transport from coastal deposits, possibly mediated by change in ice climate. In contrast, temporal changes in the northwest may relate to changes in the supply of modern plant debris under recent warmer conditions. On the western shelf, changes may relate to ice climate and the distribution of northern coastal water and/or changes in the delivery of materials by the Churchill River due to water diversion. Although the cores show evidence of change related to the ice climate, there is little evidence that ice itself transports terrigenous organic carbon within the system.     

泥沙捕集器在长江口航槽区域放投放和观测

本文报道了５套泥沙捕集器在１９８７年８月１３－１７日和１９９０年２月２２－２６日期间在长江口北槽航区域现场投放和观测，集沙杯由有机玻璃制成，内径为５ｃｍ，杯高２１ｃｍ。对在小风情形，小风转大风情形和寒潮大风情形下集沙杯捕获沙样的干重和沙样的中值粒径垂直分布的特征分别作了描述，阱而为大风浪引起航槽游积及其底沙粗化提供了确凿证据。     

厦门西港底质耗氧的测定

采用闭合循环实验方法,观测了厦门西港底质耗氧过程。结果显示底质耗氧随时间变化呈非线性,可用指数方程SOD=ρ·exp(—k/t)表示.计算得厦门西港底质耗氧速率均值为405.8mg/(m~2·d)。在底质耗氧过程中,底质释放出有机物质,底质释放COD 速率为93.6mg/(m~2·d),底质耗氧作用与底质有机物质的释放有关.     

环境样品中甲基汞的检测方法综述

综述了常用的环境样品中甲基汞的检测方法和检测步骤,认为在实际的甲基汞检测过程中,选择或评价所选用检测方法的原则通常是,在确保检测限的基础上,首选考虑检测结果的精确度如何,而快捷方便、经济实惠的检测技术也是现实运用中的实际需要。作为定量检测,GC分别与AAS、AES、AFS的联用是目前较常用的技术,而与ICP-MS或ID-ICPMS的联用,在今后的实际检测中将得到更广泛的运用。生物传感器检测到的汞一般是生物可利用的汞,降低其检测限并将其作为对污染水体与沉积物检测的重要方法,也是今后研究的重点。总之,在人类对环境安全和身体健康日益重视的今天,发展高灵敏度、高准确度、快速方便和低成本的检测技术是未来甲基汞检测的重要发展方向。     

Bacterial contribution to manganese oxidation in a deep coastal sediment

The characteristics of Mn(II) removal from sediment porewater and the potential role of manganese-oxidizing bacteria in this process were examined in sediments from a 335-m deep station in the Laurentian Trough of the St. Lawrence estuary. Manganese-oxidizing bacteria were most abundant in the thin layer of oxidized surface sediment, where Mn(II) removal rates were also fastest. The first-order rate constants for Mn(II) removal decreased from 1·2 × 10³ day⁻¹ to 6·6 day⁻¹ over the first 30-mm depth. In experimental slurries, sediments removed Mn(II) from reduced zone porewater by a two-step process: a rapid saturation of Mn(II) binding sites was followed by a slower O₂-enhanced removal rate which paralleled the apparent rate of Mn(II) oxidation. Sodium azide and mercuric chloride were tested specifically for their usefulness as bacterial poisons in sediment slurry systems. Sodium azide interfered with Mn(II) removal at low concentrations and was not an effective poison. Mercuric chloride inhibited bacterial activity at concentrations far lower than those at which significant interference of Mn(II) removal occurred. The response of sediment slurries treated with mercuric chloride indicated that the initial oxidation of sorbed Mn(II) was not bacterially-mediated under the experimental conditions tested.     

天津市沿海警戒潮位核定研究

以《警戒潮位核定规范》为依据,利用塘沽海洋环境监测站的长期验潮资料,以多年一遇的潮位值和防潮设施的防潮标准等为基础,结合核定区域的地理位置、保护目标的社会经济情况、历史风暴潮灾害情况等,对天津市沿海的警戒潮位值进行核定,最终得出天津市沿海的红、橙、黄、蓝四色警戒潮位值分别为283 cm、263 cm、238 cm和213 cm。天津沿海的警戒潮位核定实际工作表明,详实、准确、全面的资料搜集,是警戒潮位核定工作的基础和重点。     

海燕生殖腺中几种营养成分含量的测定

对黄海产海燕(Asterina pectinifera)生殖腺中几种营养成分进行了测定。结果表明,海燕生殖腺中蛋白质含量为43．25％,粗脂肪含量为14．22％,化学元素含量丰富,海燕生殖腺具有开发利用价值。     

Micro-autoradiographic determination of the viability of algae inhabiting deep sediment layers

Examination of sediment cores taken from shallow coastal regions of the Baltic showed that some algae were still alive at depths beyond the depth of light penetration. Their cells contained chlorophyll and photosynthesis resumed when they were exposed to light. Photosynthesis was detected by simultaneous measurement of oxygen production and ¹⁴C uptake. Autoradiography was used to detect incorporated ¹⁴C. The autoradiographic method was improved by a few modifications.     

Gas-liquid chromatographic determination of amino acids and vertical distribution of proteinaceous substances in sea water

Gas-liquid chromatographic method byGehrke et al. was applied to the determination of the dissolved proteinaceous substace. Sea-water samples were evaporated in vacuum to the volume of one twentieth of the initial volume and separated from deposited inorganic salt crystals. Thirteen kinds of amino acids except histidine, arginine and cystine were quantitatively determined for artificial sea water containing sixteen standard amino acids with accuracy of about five percent and with yield of 80 to 103 percent. This method has advantage comparing with paper or thin layer chromatography on the precision and comparing with ion-exchange method on sensitivity.The difference of amino acid concentration between the sea-water samples of different depth and different region was observed. The total amounts of dissolved amino acids were found to be between 33 and 92g per liter in sea water of Pacific Ocean taken at the surface to 1,500 m in depth.Contribution No. 41, from The Research Institute of North Pacific Fisheries, Hokkaido University.     

气质联用技术分析鉴定海洋琼胶液化弧菌脂多糖的脂肪酸

利用气质联用技术 (GC- MS)对海洋琼胶液化弧菌脂多糖的脂肪酸组成和结构进行了分析鉴定。结果表明 ,该脂多糖的脂质 A部分含有 7种脂肪酸。其中饱和脂肪酸 3种 :正十二碳烷酸 ,正十四碳烷酸和正十六碳烷酸 ;不饱和脂肪酸 4种 ,分别为 9-十六碳烯酸 ,9-十七碳烯酸 ,11-十八碳烯酸和 9,12 -十八碳二烯酸     

Liquid waveguide capillary cell for the spectrophotometric determination of nanomolar iodate concentrations in marine waters

A new spectrophotometric method based on a liquid waveguide capillary cell for an enhanced detection was developed to measure nanomolar iodate concentrations. This method has a detection limit and precision of 1–2 nmol/L, which is equivalent to 10% that of conventional methods, a recovery of 97.7%–104.0%, and a working range of 10–120 nmol/L. Water samples were collected from three estuaries and one coastal ocean for testing, and the proposed technique detected as low as 11 nmol/L and 18 nmol/L ...     

海水中磷氮不同形态的同时测定

采用过硫酸钾-硼酸-氢氧化钠混合试剂作为氧化剂,同时测定海水中总磷、氮和总溶解态磷、氮,从而建立了海水中磷、氮不同形态的分析流程及步骤。总磷、总溶解态磷浓度为0.35～1.09μmol/dm3时,相对标准偏差小于6.6%;总氮、总溶解态氮浓度为11.8～54.8μmol/dm3时,相对标准偏差小于5.6%。总磷、总溶解态磷和总氮、总溶解态氮的回收率分别为95.0%～106.0%和94.0%～106.0%。本文的分析方法可用于对近岸海水及河口水中磷、氮不同形态的同时测定。     

光谱法测定海水中溶解态无机氮的研究进展

溶解态无机氮(dissolved inorganic nitrogen,DIN)主要由亚硝酸盐-氮(NO^-₂-N)、硝酸盐-氮(NO^-₃-N)和铵氮(NH⁺₄-N)组成,它们在海洋的生物地球化学循环过程中起重要作用。但人类活动向海洋输入了大量无机氮,导致一系列环境问题。为了更好地开展海洋氮循环研究和环境污染管理,需对海水中的DIN进行测定。在众多分析方法中,光谱法因其通用性好、适用范围广、所需设备简单,成为测定海水DIN的首选。本文总结了近10年来基于光谱法测定海水DIN的研究进展,包括紫外分光光度法测定NO^-₃-N、萘乙二胺分光光度法测定NO^-₂-N和NO^-₃-N、次溴酸盐氧化-分光光度法测定NH⁺₄-N、靛酚蓝分光光度法测定NH⁺₄-N...     

海水中硝酸盐铜镉柱还原测定操作步骤的优化研究

本文比较了硝酸盐测定的铜镉柱还原法在两个规范中技术指标和操作工艺的差异.针对本实验室具体条件,对该测定方法的某些步骤(如镉柱制备、蠕动泵、流速选择、加氯化铵缓冲液方法等)进行优化研究,选择适宜的改进方法,以便将硝酸盐铜镉柱还原测定方法结合进本实验室已有的营养盐测定系统中.     

A simplified resorcinol method for direct spectrophotometric determination of nitrate in seawater

A direct, spectrophotometric method has been adapted for quantitative determination of nitrate concentrations in seawater. The method is based on nitration of resorcinol in acidified seawater, resulting in a color product. The absorption spectrum obtained for the reaction product shows a maximum absorption at 505 nm, with a molar absorptivity of 1.7 × 10⁴ L mol^− 1 cm^− 1. This method has a detection limit of 0.5 μM and is linear up to 400 μM for nitrate. The advantage of this method is that all reagents are in aqueous solutions without involving cadmium granules as a heterogeneous reactant, as in conventional methods, and therefore is simple to implement. Application of the resorcinol to seawater analysis demonstrated that the results obtained are in good agreement with the conventional approach involving the reduction of nitrate by cadmium followed by diazotization.     

A comparison of sample handling and analytical methods for determination of acid volatile sulfides in sediment

Proper sample storage and analytical techniques are required when analyzing anoxic sediment for acid volatile sulfide (AVS), because a change in redox state may alter sediment parameters. The goal of this study was to determine the optimum sample handling, storage, and analytical techniques to adopt when determining AVS concentrations in sediment. To determine the correct handling and storage protocols for use with anoxic sediment, samples of three different AVS levels were manipulated under a combination of the following handling and storage plans: handled on benchtop or under nitrogen atmosphere; preserved with zinc acetate (ZnAc) or not preserved, and stored at 4 °C or frozen (< − 20 °C). The data indicate that sulfide levels are best maintained when samples are handled under a nitrogen atmosphere, stored at 4 °C or frozen, and analyzed within 2 weeks of collection. To determine the best analytical procedure for the determination of AVS in sediment, the following methods were compared: colorimetric, gravimetric, ion-selective electrode, and photoionization detection. The colorimetric method was preferred.     

Using sediment geochemistry to infer temporal variation of methane flux at a cold seep in the South China Sea

Release of methane from the seafloor throughout the world's oceans and the biogeochemical processes involved may have significant effects on the marine sedimentary environment. Identification of such methane release events in marine sediment records can hence provide a window into the magnitude of ancient seeps. Here, we report on analysis of the geochemical composition of samples in a 12.3 m long sediment core (DH-5) collected from a seep site in the South China Sea (SCS). Our aim has been to investigate whether the evidence for the presence of methane release event within sediments is discernible from solid-phase sediment geochemistry. We show that sedimentary total sulfur (TS), δ³⁴S values of chromium reducible sulfur (δ³⁴S_CRS) along with total organic carbon (TOC) and total inorganic carbon (TIC) content can be used to infer the presence of methane release events in cold seep settings. At least three methane release events were identified in the studied core (Unit I at 400–550 cm, Unit II at 740–820 cm, and Unit III at 1000–1150 cm). According to the characteristic of redox-sensitive elements (eg., Mo, U and Mn), we suggest that methane flux has been changed from relatively high (Unit I) to low (Unit II and III) rates. This inference is supported by the coupled occurrence of ³⁴S-enriched sulfides in Unit II and III. AMS ¹⁴C dates from planktonic foraminifera in Unit I suggest that high methane flux event occurred at ∼15.4–24.8 kyr BP, which probably resulted in locally-focused aerobic methane oxidation. Overall, our results suggest that TS, TOC, TIC and δ³⁴S_CRS have potential for identifying present and fossil methane release events in marine sediments.     

Colorimetric determination of nanomolar concentrations of silicate in natural waters after liquid-liquid extraction using methyl isobutyl ketone

A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by the reaction between silicate and ammoni- um molydate and reduced by metol-sulfite reagent is extracted by methyl isobutyl ketone. The absorbance can be enhanced substantially up to 10-folds. The detection limit of silicate is 8 nmol/dm^3 , which is one tenth smaller than the traditional method, with the precision of 4.0% at a silicate level of 50 nmol/dm^3 and 3.2% at a silicate level of 6 μmol/dm^3. Comparing the calibration curves in the distilled water and seawater, it can be seen that the salt effect also exists in the extraction method. However, the salt effect is a linear function of the salinity and can be corrected by simple calibration. The proposed method is successfully applied to the determination of silicate in natural waters. Natural concentrations of arsenate, arsenite and phosphate cause negligible interference.