原子吸收——氢化物法测定水中的砷

前言原子吸收分光光度法测定砷有火焰法和无火焰法。火焰法灵敏度低;无火焰法灵敏度高,但是干扰严重。通过化学转变As—AsH_3,称之为氢化物法,已发展成为一个重要分支。原子吸收——氢化物法,近年发展很快,以往此法需要载气,自郭小伟提出“双毛细管”方法后,出现了无载气火焰氢化物法。本文采用一种无载气简易氢化物发生器,以空气——乙炔火焰测定地面水中的砷,灵敏度是0.0019μg/ml,比火焰原子吸收(溶液)方法的灵敏度提高了100倍。本法仪器结构简单,操作简便,灵敏快速,干扰少,易于推广。可在不预先富集水样的条件下,监测地面水中的砷含量是否超标。水样经过适当富集,可准确测定水体中的微量砷。     

流动注射-氢化物发生原子荧光法测定海洋沉积物样品中痕量铅

铅是一种具有累积性的有害元素,是海洋监测调查中沉积物介质的必测元素之一,常用测定方法有双硫腙分光光度法、火焰原子吸收光谱法、无火焰原子吸收光谱法等[1],前两种方法灵敏度较低,测定时一般需要预富集,操作较繁琐;后一种方法虽然灵敏度高,但仪器昂贵,对操作人员要求高.氢化物发生原子荧光法由于灵敏度高、检出限低且线性范围宽,在铅的分析中日益被重视.     

极谱催化波测定海水中硒(Ⅳ)

硒是一种人体健康必不可少的痕量元素[1].近年来测定硒的方法很多,例如萤光法[2]、分光光度法[3]、气相色谱法[4]、原子吸收分光光度法[5]、中子活化法[6]及电化学分析法[7]等.这些方法中多以测四价形态的硒为主,并需经富集等处理步骤.本文综合前人的工作,对极谱催化波的底液体系作了研究,并且应甩于海水中Se(Ⅳ)的测定.     

BSPB自动分析法测定海水中硝酸盐的研究

海水中硝酸盐的测定多以比色法为主[1-5],但极谱法与紫外分光光度法也有一定程度的发展,测定方法虽然较多,但结果尚不能令人满意,近期李延创立了BSPB法,它具有操作简便、反应迅速及精度高的优点[9,10].在自动分析系统中,目前多采用铜镉还原法[2,3],虽然精度较高,但还原柱制备复杂且在操作中要经常更换,为此作者对BSPB法用于自动分析仪进行了研究,得到了较满意结果.     

海藻中砷含量的研究 Ⅰ.银盐分光光度法

我国的海藻资源异常丰富,种类多,分布广。海藻中含有多种营养物质,包括海藻多糖、多酚、活性碘、多种维生素、氨基酸等;同时也含有一定数量的重金属元素,其中砷元素与人类健康和生命活动有着至为密切的关系,是毒性金属研究的代表性物质。海藻中砷的含量、分布和形态直接关系到各种海藻的利用价值和方法。 我国国内对海藻中砷的研究较少,而国际上自本世纪初就开始了此项研究。1919年,Cornec 首次对海藻灰分进行定性的光谱分析,发现其中含有砷(Cornec,1919)。以后的大量文献对海藻中的砷及其测定方法进行了较为详细的研究报道,目前研究人员普遍认为,海藻中的砷以有机态和无机态并存,其中有机砷化合物占绝大多数,毒性较小(Whyte et al.,1983; Edmonds et al.,1993; Phillips et al.,1985)。目前国际上测定海藻中砷的方法主要有中子活化法(Lunde,1973)、原子吸收分光光度法(AAS)(Maher,1982,1983;Yasui et al.,1978)、感应耦合等离子体-原子发射分光光度法联用(ICP-AES)(Shinagawa et al.,1983)等,这些方法不仅需要大型仪器,而且样品的前处理过程比较复杂,操作亦难以掌握。 作者应用比较简便、灵敏的银盐分光光度法,使用国产仪器,以海带、鼠尾藻等样品进行实验研究,结果表明,本法非常适合于海藻中砷的测定,具有较高的实用价值。     

海水中碘的动力学分光光度法测定——砷(Ⅲ)-铈(Ⅳ)-番木鳖碱直接法

测定海水中碘含量的方法很多,利用砷(Ⅲ)-铈(Ⅳ)氧化还原体系的动力学分光光度法是其中之一。Dubravčič[1,2]用亚铁离子抑制该反应,生成的高铁离子用KCNS显色,然后以测得的吸光度的对数值对碘含量作图得标准曲线。此法的缺点是要制作高碘含量和低碘含量两条标准曲线,而且受氯度、酸度、温度等条件的影响较严重,使得标准曲线经常变动。后来,Barkley等[3]用番木鳖碱作抑制剂,通过测定经不同反应时间后剩余量的铈(Ⅳ)与番木鳖碱形成的红色络合物的吸光度求出反应速率常数,并以多次测得的反应速率常数对碘含量作图绘制标准曲线。此法虽克服了前法标准曲线容易变动的弱点,但操作十分繁琐,而且水样和试剂的用量都比前法大得多。     

砷化氢-硝酸银分光光度法直接测定海水中痕量砷

一、前言 砷与二乙基二硫代氨基甲酸银(SDDC)络合物的分光光度法作为常用的标准分析法,文献中已有大量报道。由于该法灵敏度欠佳,测定范围为1—100μg,限制了其在痕量分析方面的应用。目前,原子吸收分光光度法(AAS)、中子活化分析、差示脉冲极谱法和阳极解吸极谱法所提供的最佳检出限达到了1ng或更低。然而,这几种方法,尤其是中子活化     

示差脉冲极谱法测定海水中痕量锗

海水中Ge(Ⅳ)含量很低,一般为ng/dm3数量级[1-3]。目前用于海水中Ge(Ⅳ)的分析方法不多。早年有人用共沉淀富集-苯基芴酮盐光度法,近年则采用氢化物发生石墨炉原子吸收法[1]。80年代以来,我国一些研究者陆续利用Ge(Ⅳ)与某些多元酚(如邻苯三酚,邻苯二酚等)的络合物在V(Ⅳ)等氧化剂存在下产生的灵敏吸附催化波,进行矿石,合金等样品中微量锗的测定[4,5]。但至今尚未见应用电分析法于海水中锗的分析。本文拟提出一个灵敏的示差脉冲极谱法,以测定海水中痕量Ge(Ⅳ),并避免通常多次分离手续[6,7]。     

海水中臭氧总残留氧化物三种检测方法的比较研究

对臭氧总残留氧化物(TRO)常用3种检测方法(碘化钾-N,N-二乙基-1,4-苯二胺(KI-DPD)分光光度法、硼酸碘化钾(H3BO3-KI)比色法、靛蓝二磺酸钠(IDS)分光光度法)进行了比较研究。结果表明:在0~0.5 mg/L的TRO浓度范围内,KI-DPD分光光度法和H3BO3-KI比色法线性关系良好,检出限分别为0.040 mg/L和0.034 mg/L,并且这两种测定方法的准确性和重复性较佳,相对标准偏差(RSD)均小于5.0%,低于传统碘量法;而IDS分光光度法只有在高浓度臭氧海水样品(0.6~1.2 mg/L)检测时,RSD才小于5.0%,且测定浓度明显低于另外两种方法。故对于海水养殖水体中的TRO检测,KI-DPD分光光度法和H3BO3-KI比色法均准确有效,并且H3BO3-KI比色法在检测操作上更为简便快捷。     

海水中硼的示波极谱测定法

海水中微量硼的测定.通常是用分光光度法[1]和光谱法。硼在通常条件下不会产生极谱波。因此不能用极谱法直接测定硼。B(Ⅲ)与铍试剂Ⅲ可形成较稳定的配合物。     

Microbial Biomass and Organic Nutrients in the Deep-Sea Sediments of the Central Indian Ocean Basin

In order to assess the impact of deep-sea mining on the in situ benthic life, we measured the microbial standing stock and concentration of organic nutrients in the deep-sea sediments of the Central Indian Ocean Basin in the Indian pioneer area. Sediments were collected using box core and grab samples during September 1996. The total bacterial numbers ranged from 10 10 -10 11 cells per g -1 dry weight sediment. There was a marginal decrease in the number of bacteria from surface to 30 cm depth, though the subsurface section registered a higher number than did the surface. The highest numbers were encountered at depths of 4-8 cm. The retrievable number of bacteria were two orders less in comparison with the direct total counts of bacteria. An almost homogeneous distribution of bacteria, total organic carbon, living biomass, and lipids throughout the depth of cores indicates active microbial and benthic processes in the deep sea sediments. On the other hand, a uniform distribution of total counts of bacteria, carbohydrates, and total organic carbon in all the cores indicates their stable nature and suggests that they can serve as useful parameters for long-term monitoring of the area after the benthic disturbance. Further studies on temporal variability in this region would not only verify the observed norms of distribution of these variables but would also help to understand restabilization processes after the simulated benthic disturbance.     

海上大直径钢管桩打桩过程中桩周土强度弱化研究

海上大直径钢管桩打桩过程中,桩周土体受到强烈扰动而发生强度弱化,掌握桩周土体强度弱化规律对于准确预测打桩过程、保证工程安全具有重要意义。为研究土体强度弱化规律,开展了环剪试验模拟打桩对桩周土体的扰动,测试土体强度随剪切速率的变化规律,建立了描述土体强度弱化规律的拟合公式,引入到打桩分析软件中。研究结果表明：土体的强度折减程度不仅与土体本身的性质有关还受到土体的埋深和剪切速率的影响,埋深越深土体强度折减程度越低,剪切速率越高土体强度折减越高,在打桩分析中可采用这里推荐的线性折减方法来模拟不同深度处土体强度的折减规律。     

Geoacoustic Inversion via Genetic Algorithm and Its Application to Manganese Sediment Identification

An acoustic inversion method using a wide-band signal and two near field receivers is proposed and applied to multiple layered seabed models including a manganese sediment. The inversion problem can be formulated into a probabilistic model comprised of signals, a forward model, and additive noise. The forward model simulates wide-band signals, such as chirp signals, and is chosen to be the source-waveletconvolution plane wave modeling method. The wavelet matching technique, using weighted least-squares fitting, estimates the sediment sound-speed and thickness on which determination of the possible numerical ranges for a priori uniform distribution is based. The genetic algorithm is applied to a global optimization problem to find a maximum a posteriori solution for determined a priori search space. Here the object function is defined by an L 2 norm of the difference between measured and modeled signals. Not only the marginal pdf but also its statistics are calculated by numerical evaluation of integrals using the samples selected during importance sampling process of the genetic algorithm.     

A Review of Some Environmental Issues Affecting Marine Mining

This article reviews information recently available from existing marine and coastal mining for responses to environmental issues affecting marine mining at different depths. It is particularly but not exclusively concerned with those issues affecting seabed biodiversity impact and recovery. Much information has been gathered in the past 10 years from shallow mining operations for construction aggregate, diamonds, and gold, from coastal mines discharging tailings to shallow and deep water, and from experimental deep mining tests. The responses to issues identified are summarized in a series of eight tables intended to facilitate site-specific consideration. Since impacts can spread widely in the surface mixing layer SML, and can affect the biologically productive euphotic zone, the main issues considered arise from the depth of mining relative to the SML of the sea. Where mining is below the SML, the issue is whether it is environmentally better to bring the extraction products to the surface vessel for processing (and waste discharge), or to process the extraction products as much as possible on the seabed. Responses to the issues need to be sitespecific, and dependent on adequate preoperational environmental impact and recovery prediction. For deep tailings disposal from a surface vessel, there are four important environmental unknowns: (1) the possible growth of "marine snow" (bacterial flocs) utilizing the enormous quantities of fine tailings particles (hundreds or thousands of metric tons per day) as nuclei for growth, (2) the possibility that local keystone plankton and nekton species may migrate diurnally down to and beyond the depth of deep discharge and hence be subjected to tailings impact at depth, (3) the burrow-up capability of deep benthos and their ability to survive high rates of tailings deposition, and (4) the pattern and rate of dispersion of a tailings density current through the deep water column from discharge point to seabed. Actions to obtain relevant information in general and site-specifically are suggested.     

Increased Particle Fluxes at the INDEX Site Attributable to Simulated Benthic Disturbance

Particle fluxes were measured 7 m above the sea bottom during the predisturbance, disturbance, and postdisturbance periods by using time series sediment traps attached to seven deep-sea moorings deployed in the INDEX experiment site in the Central Indian Basin. The predisturbance particle fluxes varied between 22.3 to 55.1 mg m -2 day -1 . Increased and variable particle fluxes were recorded by the sediment traps during the disturbance period. The increase observed was 0.5 to 4 times more than the background predisturbance fluxes. The increases in particle fluxes (~4 times) recorded by the sediment trap located in the southwestern direction (DMS-1) were the greatest, which could be the result of preferential movement of resuspended particles generated during the deep-sea benthic disturbance along the general current direction prevailing in this area during the experimental period. Also, the traps located closer to the disturbance area recorded greater fluxes than did the traps far away, across the Deep Sea Sediment Resuspension System path. This variability in recorded particle fluxes by the traps around the disturbance area clearly indicates that physical characteristics such as grain size and density of the resuspended particles produced during the disturbance had an important effect on particle movement. The postdisturbance measurements during ~5 days showed a reduction in particle fluxes of ~50%, indicating rapid particle settlement.     

Determination of In Situ Sediment Shear Strength from Advanced Piston Corer Pullout Forces

The advanced piston corer (APC) has been used by the Ocean Drilling Program since 1985 for recovering soft sediments from the ocean floor. The pullout force measured on extracting the core barrel from the sediment is shown to correlate with the average shear strength of the sediment core measured in the ship's laboratory. A simple rule of thumb is derived relating the shear strength of the sediment to the pullout force. Multiple APC holes at individual sites allow the consistency of the pullout measurements to be assessed. The effects of different operational procedures during APC coring are also explored. Although generally applicable, the correlation between pullout force and laboratory measurements of shear strength breaks down for some APC holes, possibly because of the disturbance of some sediment types during the APC coring process. A better understanding of the physical process of APC coring, and its effect on the properties of the sediment both inside and immediately outside the core barrel, would indicate what confidence can be put on the measurement of pullout force as a way of evaluating the in situ shear strength of deep sea sediments.     

Phylogenetic diversity and phenotypic characterization of cultivable bacterioplankton isolated from polar oceans

A set of 27 marine planktonic bacteria isolated from the polar regions was characterized by 16S rDNA sequencing and physiological and biochemical testing. More than half of these bacteria were positive for caseinase, gelatinase and 13-glucosidase, and could utilize glucose, maltose or malic acid as carbon source for cell growth. Twelve isolates expressed nitrate reduction activities. Except for one antarctic isolate BSwlO175 belonging to Actinobacteria phylum, these isolates were classified as γ-Proteobacteria, suggesting that γ-Proteobacteria dominated in cultivable marine bacterioplankton at both poles. Genus Pseudoalteromonas was the predominant group in the Chukchi Sea and the Bering Sea, and genus ShewaneUa dominated in cultivable bacterioplankton in the Prydz Bay. With sequence similarities above 97%, genus Psychrobacter was found at both poles. These 27 isolates were psychrotolerant, and significant 16S rDNA sequence similarities were found not only between arctic and antarctic marine bacteria （ 〉 99% ）, but also between polar marine bacteria and bacteria from other aquatic environments （ ≥ 98.8% ）, including temperate ocean, deep sea, pond and lake, suggesting that in the polar oceans less temperature-sensitive bacteria may be cosmopolitan and have a bipolar, even global, distribution at the species level.     

Deep-Sea Sediment Compression Curves: Some Controlling Factors, Spurious Overconsolidation, Predictions, and Geophysical Reproduction

Oedometer tests have been carried out on 70 undisturbed surficial clays (at approximately 250 mm below the mudline), mostly collected by free-fall corers from sites widely scattered throughout the deep-sea North Atlantic. Acoustic measurements were also made, initially on contiguous samples and ultimately on the same sample using a geophysically instrumented oedometer which also collected electrical resistivity data. Apart from those quiescent areas below the carbonate compensation depth, such as north of the West Indies where very fine clays exist, most of the samples are silty clays whose geotechnical-geophysical properties are dependent on the type of clay minerals present (and their ability to take in moisture), the sand-size fraction, and the quantity of carbonate present. Thus the pure clays have high compressibilities which decrease on the addition of coarse particles, while the converse is true for the acoustic parameters, these increasing with the sand fraction. Using the notion of the intrinsic compression line for all samples, and comparison to it of the measured compression curves, it is clear that, contrary to some previously held ideas, most deep-sea clays are normally consolidated; the addition of carbonate has the effect of creating an open, stronger sediment skeleton. Interestingly, where information is available, the variation with depth of a sample's acoustic velocity follows the void ratio pressure relationship of the compression curve. This allows the construction of an in-situ sediment compression curve using the in-situ geophysical observations.