气相色谱—质谱联用技术在环境分析中的应用

气相色谱与质谱联用技术(GC—MS)的研究始于五十年代后期,到六十年代末己趋成熟,并有商品仪器出现。1970年以后发展更为迅速,与计算机联用,组成了色谱—质谱—数据处理系统(GC-MS-DS)。由于GC-MS具有灵敏度高,分析速度快,应用范围广等特点,因此很快就被应用于环境样品的分析,为环境分析开辟了一条新的途径。本文就近年来GC-MS联用技术在环境样品分析中的应用作一介绍。     

水中10种挥发性有机物的快速检测

采用吹扫捕集与快速气相色谱-飞行时间质谱联用,建立测定水中10种石化行业常见挥发性有机物(VOCs)的吹扫捕集-快速气相色谱-飞行时间质谱的分析方法。通过质谱定性,选定目标物的特征离子,运用内标法定量,采用DN-624(20m×0.18mm×1μm)快速毛细管色谱柱,在10min内完成对水中10种VOCs的分析,在保证各目标物灵敏度和分辨率不受影响的同时,分析时间从标准方法的17min降至10min。该方法的线性、精密度与检出限满足标准方法 HJ 639—2012《水质挥发性有机物的测定吹扫捕集/气相色谱-质谱法》要求,通过实验验证,能够广泛应用于石化行业环境监测与应急监测。     

落新妇地下部分挥发油化学成分GC—MS分析

利用水蒸汽蒸馏法提取落新妇地下部分的挥发油,测得含量为0．10％;采用气相色谱－质谱联用技术（GC—MS）对落新妇的挥发性成分进行了分离鉴定,分离出57种成分,鉴定了其中50种;运用峰面积归一法确定了各成分的相对含量,检出率为87．71％。落新妇地下部分挥发油的主要成分为邻苯二甲酸二丁酯、十六甲基八环硅氧烷。     

HPLC—ICP—MS法测定农业废水中有机砷与无机砷的方法研究

建立了应用高效液相色谱（HPLC）和电感耦合等离子质谱（ICP—Ms）联用技术测定农业水环境样品中三价砷（Aslll）、一甲基砷（MMA）、二甲基砷（DMA）、五价砷（AsV）4种砷形态的分析方法。试验表明,4种砷形态的线性范围宽（1-300μg·L-1）,相关系数（r）均大于0．9990,方法检出限低（0．7～0．98μg·L-1）,精密度好,重复测定7次结果的RSD均小于5％。通过计算加标回收率验证方法的准确性,加标回收率为94％～112％。实际样品的测定结果显示,农田废水中砷的主要存在形态为As（V）,其次为As（Ⅲ）。     

中药川附子非金属元素分析

本文论述了川附子非金属元素的分析：用ICP—AES法测定S、P和Si；离子色谱法测定Cl、S、P；极谱法和HG—AFS法测定痕量砷；ICP—AES和荧光法测定硒；GB法测定氯、氟和碘。应用提出的方法弄清了川附子用传统工艺食盐-胆巴混合溶液炮制前后非金属元素的含量与浓度变化，从而为中药化学成分进一步研究增添新内容一非金属元素及检测方法。     

色谱质谱联用技术在一起农药污染事故应急监测中的应用

在一起污染源应急事故中,色谱质谱联用技术在确定污染源类型,并快速做出准确定性定量分析中发挥了重要作用。通过气相色谱-质谱联用技术,首先确定可能污染物类型为三嗪类化合物;之后,通过液相色谱-串连质谱全扫描,推断可能为三嗪类除草剂——甲磺隆。正、负ESI子离子全扫描后图谱与甲磺隆标准物质图谱相对照,完全吻合。最后,通过SRM模式下对380.0→139.0的母、子离子选择反应监测,测定了农田灌溉水源和土壤中甲磺隆的含量。     

吹扫捕集气质联用测定水中嗅味物质的研究

文章建立了一种用吹扫捕集—气相色谱质谱联用技术测定饮用水中土臭素(GSM)和二甲基异冰片(2-MIB)等嗅味物质的分析方法,确定了最佳的色谱条件、质谱条件和水样处理方法。当取样量为25mL时,回收率分别为96%和89%,RSD<10%,检出限为0.002mg/L。     

落新妇地下部分挥发油化学成分GC-MS分析

利用水蒸汽蒸馏法提取落新妇地下部分的挥发油,测得含量为0.10%;采用气相色谱-质谱联用技术(GC-MS)对落新妇的挥发性成分进行了分离鉴定,分离出57种成分,鉴定了其中50种;运用峰面积归一法确定了各成分的相对含量,检出率为87.71%.落新妇地下部分挥发油的主要成分为邻苯二甲酸二丁酯、十六甲基八环硅氧烷.     

树舌灵芝菌丝体不皂化物GC—MS分析

在树舌灵芝菌丝体化学成分研究中,采用乙醚抽提法获取树舌灵芝菌丝体脂溶性物质,经皂化后使用气相色谱一质谱联用技术（CC—MS）进行分析,共鉴定出19种物质,所得到的丁羟甲苯、乙酰菲、5,6-二氢麦角甾醇对树舌灵芝菌丝体化学成分研究具有较高价值。     

超高效液相色谱-串联四极杆质谱分析环境水样中对苯二胺

本文建立了超高效液相色谱-串联四极杆质谱分析环境水样中对苯二胺的分析方法。方法使用C18反相柱为分离柱,柱温30℃,流速0.3ml/min,80%甲醇+20%纯水作流动相,保留时间1.92min,使用具ESI(+)源的质谱作检测器。在此条件下,水样过0.45μm滤膜后可直接进样,进样体积10μl,检出限可达0.028μg/L,在0.10～4.00μg/L范围内线性良好(R=0.9998);相对标准偏差在0.7%～4.9%之间,样品加标回收率在88.2%～118%之间,应用到实际环境水样分析中也具有令人满意的结果。该方法灵敏度高,快速简单,适用于环境水样中对苯二胺的分析。     

饮用水中砷去除技术综述

自从1996年孟加拉国和印度报道慢性砷中毒事件以来，饮用水砷污染和砷中毒问题就受到全世界的关注。如何解决这一难题，研究人员进行了大量研究。本文综述了饮用水中砷的去除方法，包括混凝／沉淀、吸附、离子交换技术等，对各种除砷技术进行了总结和比较。     

Concentrations of additive arsenic in Beijing pig feeds and the residues in pig manure

The swine industry in China has grown rapidly over last two decades. Great amount of pig manure is generated in China, which can be used as organic fertilizers on agricultural lands. Meanwhile, the organic arsenic compounds have been used as feed additives for swine disease control and weight improvement. Once the excessive additives are released in the environment, arsenic may compromise food safety and environmental quality. There is a growing public concern about the arsenic residues accumulation in pig manure, however, little work has been done to investigate the exact arsenic content in pig feed and the residues in manure in China This study investigates the concentrations of arsenic in 29 pig feed samples and 29 manure samples collected from eight pig farms in the Chaoyang district, Beijing city. The detected rate of arsenic in 29 couples of samples was 100%. The concentrations of arsenic in pig feeds and manures ranged from 0.15 to 37.8 mg/kg and 0.42 to 119.0 mg/kg, respectively. The result showed that arsenic concentration in pig manure will be greatly elevated when the arsenic in pig feed was largely increased. The loading rates of pig manure in fourteen Beijing counties and districts were in the range of 2.7–57.2 t/ha yr. Accordingly, the potential soil arsenic increase rates resulting from land application of pig manure might range between 11.8 and 78.9 μg/kg yr. Despite these findings, it is too early to draw the conclusion that arsenic pollution from pig manure is serious in Beijing farmland; therefore, longitudinal studies about the chemical form transformation and the environmental behaviors of pig manure arsenic are required in order to come up with more definitive conclusions.     

Iron and aluminium based adsorption strategies for removing arsenic from water

Arsenic is a commonly occurring toxic metal in natural systems and is the root cause of many diseases and disorders. Occurrence of arsenic contaminated water is reported from several countries all over the world. A great deal of research over recent decades has been motivated by the requirement to lower the concentration of arsenic in drinking water and the need to develop low cost techniques which can be widely applied for arsenic removal from contaminated water. This review briefly presents iron and aluminium based adsorbents for arsenic removal. Studies carried out on oxidation of arsenic(III) to arsenic(V) employing various oxidising agents to facilitate arsenic removal are briefly mentioned. Effects of competing ions, As:Fe ratios, arsenic(V) vs. arsenic(III) removal using ferrihydrite as the adsorbent have been discussed. Recent efforts made for investigating arsenic adsorption on iron hydroxides/oxyhydroxides/oxides such as granular ferric hydroxide, goethite, akaganeite, magnetite and haematite have been reviewed. The adsorption behaviours of activated alumina, gibbsite, bauxite, activated bauxite, layered double hydroxides are discussed. Point-of-use adsorptive remediation methods indicate that Sono Arsenic filter and Kanchan™ Arsenic filter are in operation at various locations of Bangladesh and Nepal. The relative merits and demerits of such filters have been discussed. Evaluation of kits used for at-site arsenic estimation by various researchers also forms a part of this review.     

气相色谱法测定气田产出水中的甲醇含量

文章建立了使用气相色谱仪分析气田产出水中甲醇含量的方法。通过实验在设定不同分流比的情况下,能有效监测出气田产出水中不同浓度的甲醇含量,此方法灵敏度高,最低检出限为0.02%,测定气田产出水中甲醇加标回收率达到93%～94%。     

砷的毒性及其环境卫生标准

砷广泛分布于自然界，而且是一种重要的环境污染物，国内外曾多次发生过砷中毒事件。本文主要报道了砷的毒性，特别是致癌性，致突变性和致畸性，同时介绍了各国砷的现行环境卫生标准。     

Preservative leaching from weathered CCA-treated wood

Disposal of discarded chromated copper arsenate (CCA)-treated wood in landfills raises concerns with respect to leaching of preservative compounds. When unweathered CCA-treated wood is leached using the toxicity characteristic leaching procedure (TCLP), arsenic concentrations exceed the toxicity characteristic (TC) limit of 5mg/L in most cases. The majority of discarded CCA-treated wood, however, results from demolition activities, where the wood has typically been subjected to weathering. Since preservatives do migrate from the wood during its normal use, leaching characteristics of weathered and aged CCA-treated wood may differ from unweathered wood. To evaluate this, CCA-treated wood removed from service after various degrees of weathering was collected from multiple sources and leached with the TCLP, the synthetic precipitation leaching procedure (SPLP) and California's waste extraction test (WET). Five to seven individual pieces of wood were analyzed from each source. The average TCLP arsenic concentration for the 14 sources ranged from 3.2 to 13 mg/L. The average TCLP concentrations of the 100 wood pieces tested were 6.4, 5.9 and 3.2 mg/L for arsenic, copper and chromium, respectively. Overall, in 60 out of 100 samples tested by the TCLP, arsenic concentrations exceeded 5 mg/L (the TC regulatory value). SPLP leachate concentrations were similar to TCLP concentrations, although copper leached somewhat more with the TCLP. WET leachate concentrations were approximately a factor of 10 higher than TCLP concentrations. Discarded CCA-treated wood, even after exposure to years of weathering, often exceeds the TC limit for arsenic and without the current regulatory exemption would possibly require management as a TC hazardous waste in the US.     

Biological filtration for removal of arsenic from drinking water

The main objective of the study was to find a suitable iron to arsenic ratio in water to reduce arsenic to 5 μg/L or lower through sand filtration. Experiments were conducted by varying the quantity of iron(II) while keeping the arsenic concentration at 100 μg/L. A mixture of iron (II) and arsenic at different ratios (10:1, 20:1, 30:1 and 40:1) was pumped to the sand filters in a down flow mode and effluent arsenic and iron were analyzed. It was found that a ratio of iron to arsenic of 40:1 was necessary to ensure an effluent arsenic concentration of 5 μg/L or lower. Iron in the filtrate was found to be below 0.1 mg/L at all times.     

CO-KRIGING TO INCORPORATE SCREENING DATA: HUDSON RIVER SEDIMENT PCBs1

ABSTRACT: Kriging methods of geostatistical analysis provide valuable techniques for analysis of sediment contamination problems, including interpolation of concentration maps from point data and estimation of global mean concentrations. Sample collection efforts frequently include preliminary screening data of considerably more extensive coverage than the laboratory analyses on which estimation is usually based. How should these be incorporated in kriging? Screening and laboratory analysis constitute two separate estimates of the same spatial field but of very different characteristics. A modified version of co-kriging is developed to include the imprecise screening information in the analysis of contaminant distribution. Use of the method is demonstrated on a data set of sediment PCB samples from the Upper Hudson River, for which preliminary categorical mass spectrometry screening was used to select a smaller set of samples for gas chromatograph analysis. The method is widely applicable to many situations of contaminant and natural resource estimation.