离子色谱法测定水中钠、钾、镁、钙

选用IonPAC CS12A色谱柱为分析柱、12 mmol/L甲烷磺酸为淋洗液,抑制电导进行检测,建立了离子色谱检测水中高浓度钠、钾、镁、钙离子的方法。钠、钾、镁、钙离子的标准曲线相关系数均大于0. 999,检测限分别为0. 40,0. 40,0. 05和0. 10 mg/L。分别向纯水、出厂水和水源水中加入这4种离子高、中、低浓度的标准溶液,回收率均在95. 32%～105. 11%,批内标准偏差在0. 000 8～0. 298 7 mg/L,批内相对标准偏差在0. 163 9%～8. 363 5%;批间标准偏差在0. 005 8～0. 177 0 mg/L,批间相对标准偏差在0. 5850%～3. 4913%,具有较好的重复性。该方法操作简便、灵敏度高,检出限、测定下限、精密度和准确度均能达到实验要求且结果可靠,可用于生活饮用水和水源水中钠、钾、镁、钙离子的检测。     

电感耦合等离子体发射光谱(ICP-OES)法测定橘子汁中钙和镁

建立了微波消解和湿法消解对样品进行前处理,电感耦合等离子体发射光谱法(ICP-OES)测定橘子汁样品中钙和镁含量的方法。选择Ca 317.933nm,Mg 285.213nm作为钙和镁的分析线。实验结果表明,钙和镁的检出限分别为0.001 8和0.000 4mg/L,相对标准偏差(RSD<2%),加标回收率为99%~101%,用来测定FAPAS国际比对橘子汁样品,反馈的统计结果显示钙和镁元素的Z值分别为-0.3和0.3,结果均为满意。方法快速、简单、精确,适于橘子汁中钙和镁的测定。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中铜、锌、钙、镁、铁

样品经硝酸-高氯酸消化溶解,高氯酸冒烟,盐酸溶解盐类后,在盐酸(5%)介质中,在选定的测定条件下,用电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中微量元素铜、锌、铁、镁、钙。选择Cu 327.3、Zn 206.2、Fe 238.2、Mg 279.5、Ca 315.8nm分别作为铜、锌、铁、镁、钙的分析线与混合标准溶液同时测定;方法加标回收率为98.6%～101%,铜、锌、铁、镁、钙的精密度(RSD,n=8)为0.37%～2%,准确度(RE)为-3.4%～1.15%,检出限分别为0.002 3、0.001 6、0.004 6、0.003 0、0.001 4μg/mL。方法克服了分光光度法和原子吸收光谱法操作繁琐、周期长、成本高、灵敏度低等缺点。用于测定人发样品中的铜、锌、铁、镁、钙元素,测定结果与原子吸收光谱法测定值基本一致。经GBWO7061标准物质和自制标样分析验证,测定值与标准值吻合,结果准确可靠。     

电感耦合等离子体发射光谱法测定铁矿石中硅、磷、锰、钙、镁、铝、钛

采用电感耦合等离子体发射光谱法测定铁矿石中硅、磷、锰、钙、镁、铝、钛。各种元素选用最佳分析谱线和光谱仪合适的工作条件,采用与试样组成相匹配的标准物质绘制工作曲线,熔剂的最佳用量为1.4g。方法简便,快速,准确,被测元素的检出限为0.003～0.10μg·ml-1,相对标准偏差为0.14%～4.90%。     

饮用淡化海水对大鼠血中铜锌钙镁铁的影响

目的通过对淡化海水卫生学指标进行检测分析及饮用淡化海水大鼠血中铜、锌、钙、镁、铁含量的测定,评价饮用淡化海水对大鼠血中铜、锌、钙、镁、铁的影响。方法首先对所采集的淡化海水的感官性状及一般化学指标20项、73项毒理学指标进行分析,判定其是否符合《生活饮用水卫生标准》(GB 5749-2006)。然后将采集所得淡化海水喂饲大鼠,与饮用市政自来水组大鼠进行对照比较,研究其血中铜、锌、钙、镁、铁含量,并计算铜锌比值、钙镁比值,分析饮用淡化海水对血中这些重要金属元素的影响。结果所采集的受试淡化海水感官性状和一般化学指标均合格,色度<5,p H=6.94,呈现弱酸性。水中溶解性总固体浓度为186 mg/L,总硬度为13 mg/L,符合饮用水卫生标准要求。硼含量为1.3 mg/L高于限值(≤0.5 mg/L),氟化物0.02 mg/L低于限值(≤1 mg/L),其他指标均未检出。饮用淡化海水180 d,大鼠血中铜含量明显高于饮用市政自来水组(F=3.02,P=0.042),其铜/锌也高于饮用市政自来水组(F=4.774,P=0.035)。饮用淡化海水90 d大鼠血中钙含量高于饮用市政自来水组大鼠(F=55.642,P=0.00),其钙/镁也高于饮用市政自来水组大鼠(F=44.933,P=0.00);饮用淡化海水180 d的大鼠血中镁、铁含量低于饮用市政自来水组大鼠(F=19.847,P=0.0007;F=5.309,P=0.027)。饮用淡化海水180 d大鼠血中钙/镁也高于饮用市政自来水组大鼠(F=5.309.P=0.030)。结论饮用淡化海水180 d会引起大鼠血中铜含量及铜/锌升高及血铁含量下降;饮用淡化海水90~180 d均会引起大鼠血中钙/镁升高。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定硒片中的硒、铁、钙和锌

用HNO_3-HClO_4(4∶1)溶解硒片,电感耦合等离子体原子发射光谱(ICP-AES)法测定其中的硒、铁、钙和锌,实验表明硒片中硒、铁、钙和锌的含量较为丰富,与外包装承诺的含量一致。方法灵敏可靠,测量相对标准偏差<3%,加标回收率在96.5%~101%,实验结果为探讨硒片对人体的保健作用提供了参考数据。     

原子吸收光谱法和电感耦合等离子体发射光谱法测定岩棉板中钾、钠含量的比较

用ICP-OES法和AAS法对样品中的K₂O、Na₂O进行测试,通过比对样品前处理、测定结果等,证实两种方法均满足建材行业岩棉板分析的测定要求,可根据实际情况选用。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定硅锆合金中的铝和钙

通过硝酸、氢氟酸和盐酸分解试样,高氯酸冒烟驱走硅和氟,最后用盐酸溶解盐类,选择Al(396.152nm)、Ca(315.887nm)作为分析谱线,电感耦合等离子体原子发射光谱(ICP-AES)法测定硅锆合金中的铝和钙。研究了锆离子(0.3mg/mL)和铁离子(0.2mg/mL)共存体系中基体效应和光谱干扰对待测元素测定的影响。结果表明,该质量浓度的锆离子和铁离子对待测元素的测定结果不产生影响。铝和钙的质量浓度在10~50μg/mL,其线性相关系数均不小于0.999,方法中铝和钙的检出限分别为0.009μg/mL和0.006μg/mL。按照实验方法测定硅锆合金中的铝和钙,结果的相对标准偏差(RSD,n=10)分别为0.85%和1.4%。方法适用,结果令人满意。     

等离子体发射光谱法直接测定海水中总磷

采用等离子体发射光谱法(ICP-AES)直接测定海水中总磷,海水样品不需氧化消解,直接测定。该方法采用基体匹配法消除物理干扰,标准曲线线性良好,测量的相对标准偏差1%,相对误差1%,总磷的加标回收率达100.8%～101.6%,方法检出限为0.015mg/L。并对同一海水样品采用该法和传统的消解-磷钼蓝分光光度法同时测定,测定结果没有明显差异。     

ICP-MS法检测水中锂、锶、钴、钒、硼的方法研究

目前对于水中锂、锶、钴、钒、硼所采用的检测方法存在一些不足,而采用电感耦合等离子体质谱法(ICP-MS法)检测优势明显。此次采用ICP-MS法对水中锂、锶、钴、钒、硼五种元素进行检测,并对该方法的适用性进行研究。     

火焰原子吸收光谱法测定玻璃中钾、钠含量

建立了一种火焰原子吸收光谱法（FASS）测定玻璃中的钾、钠含量的方法,对火焰原子吸收的狭缝宽度、燃烧头角度和元素的测定波长进行了优化。结果表明,该方法测定钾含量的相对标准偏差（RSD）为3.4%~4.8%,加标回收率为95%~102%;测定钠含量的相对标准偏差（RSD）为0.8%~4.8%,加标回收率为92%~105%。     

电感耦合等离子体-质谱法测定内墙漆中8种重金属杂质

文章建立了用电感耦合等离子体-质谱(ICP-MS)法测定内墙漆中Se、Cd、Sb、Cr、Pb、Hg、As、Ba等8种重金属含量的方法。样品经过预处理用盐酸溶解,得到样品溶液后用电感耦合等离子体质谱进行测定。8种重金属杂质元素的方法检出限为0.02-0.5ng/g。利用建立的方法,对市场上某种墙面漆中的8种金属元素进行测定,并进行了加标回收实验,加标回收率为94%-106%。各杂质元素均为10 ng/mL的混合标准溶液平行7次进样的相对标准偏差均小于5%。该方法操作简便,能够满足内墙漆中有害重金属杂质测定的需要。     

Simultaneous multielement determination of trace metals in lake waters by ICP emission spectrometry with preconcentration and their background levels in Japan

An analytical method combining a preconcentration followed by determination with inductively coupled plasma emission spectrometry (ICPES) was developed for monitoring background levels of trace metals in natural waters. Complexes of trace metals (Al, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, Cd and Pb) and 8-hydroxyquinoline were absorbed to a C₁₈ chemically bonded silica gel disposable plastic column. They were eluted with methanol and digested with nitric acid. With this preconcentration procedure, about 500-fold preconcentration is possible. Simultaneous multielement analysis with ICPES ensures the necessary sensitivity to measure the trace metals in Lake Mashu water at concentration ranges from μg l^?1 (ppb) to ng l^?1 (ppt).Lake Mashu is a deep oligotrophic lake in Hokkaido, Japan and famous for the highest transparency in the world. The trace metal concentrations in Lake Mashu were extremely low: Fe 2.6; Al 1.2; Mn 0.76; Zn 0.63; V 0.15; Cu 0.069; Ti 0.06; Pb 0.05; Ni 0.027; Cd < 0.006; and Co < 0.004 μg l^?1. The suitability of Lake Mashu for a background level monitoring station for global environmental pollution was assessed by the comparison to reference data for other lakes in the world.     

IC—ICP—MS法测定水中BrO_3~-和Br~-

采用离子色谱--电感耦合等离子体质谱联用法分析了水中溴酸根和溴离子的含量,对流动相、进样量和干扰因素进行了研究.试验表明,以IonPac AS14柱为分离柱、30 mmol/L的(NH4)2CO3为淋洗液,当流速为1 mL/min、进样量为1 mL时,该方法对BrO3-和Br-的检测限(MDL)分别为0.12、0.21μg/L,回收率分别为96.0%、100.8%,相对标准偏差分别为3.71%、2.72%.     

Depleted uranium contamination by inhalation exposure and its detection after approximately 20 years: implications for human health assessment

Inhaled depleted uranium (DU) aerosols are recognised as a distinct human health hazard and DU has been suggested to be responsible in part for illness in both military and civilian populations that may have been exposed. This study aimed to develop and use a testing procedure capable of detecting an individual's historic milligram-quantity aerosol exposure to DU up to 20 years after the event. This method was applied to individuals associated with or living proximal to a DU munitions plant in Colonie New York that were likely to have had a significant DU aerosol inhalation exposure, in order to improve DU-exposure screening reliability and gain insight into the residence time of DU in humans. We show using sensitive mass spectrometric techniques that when exposure to aerosol has been unambiguous and in sufficient quantity, urinary excretion of DU can be detected more than 20 years after primary DU inhalation contamination ceased, even when DU constitutes only approximately 1% of the total excreted uranium. It seems reasonable to conclude that a chronically DU-exposed population exists within the contamination 'footprint' of the munitions plant in Colonie, New York. The method allows even a modest DU exposure to be identified where other less sensitive methods would have failed entirely. This should allow better assessment of historical exposure incidence than currently exists.     

Post mortem changes of the elemental composition of autopsy specimens: Variations of K,Na, Mg,Ca, Cl,Fe, Zn,Cu, Mn and Rb in rat liver

Retaining the liver inside the intact dead body for different periods of time at ambient temperature induced significant differences in its weight due to post mortem tissue degeneration. Livers from animals that were frozen at ?15°C also showed significant decrease in weight upon thawing on the third day. The effect of these changes on the concentrations of various elements was reflected differently depending upon the association of the elements with extracellular fluids and intracellular components. Thus, concentration of K was more affected by the lysis of the cell and sustained losses up to 30 per cent in relation to the control values, while the total content was reduced by more than 40 per cent as a result of both lysis and partial liquefaction. For Na, differences ranging from +10 to ?20 per cent in concentrations, and +20 to ?40 per cent in total content were observed which could be explained by fluid movements in and out of the organ. Mg and Cl essentially resembled K and Na, respectively. Ca concentration from the animals exposed to ambient temperature was unpredictable due to its mobilization from the decaying residual food in the GI-Tract. Among the trace elements, variations observed for Fe ranged from ?20 and +40 per cent, while both Cu and Zn were found to fluctuate between ?20 and +20 per cent. The loss observed in the total content in liver for the 5 trace elements studied (Cu, Fe, Mn, Rb and Zn) was found to be about 20 to 40 per cent. Rinsing of the liver samples with distilled water depleted the electrolyte concentration up to 30 per cent. Among the trace elements, while Cu, Fe and Zn were relatively unaffected, the losses were up to 20 per cent both for Mn and Rb. It is concluded that livers autopsied on different days are apt to introduce serious systematic errors and that, it is very important to standardize the sampling time for autopsy cases.     

Toxic effects of Cu on growth, nutrition, root morphology, and distribution of Cu in roots of Sabi grass

Sabi grass (Urochloa mosambicensis (Hack.) Dandy) (a C4 species of Poaceae) is commonly used to revegetate disturbed sites in low-rainfall environments, but comparatively little is known regarding copper (Cu) toxicity in this species. A dilute nutrient solution culture experiment was conducted for 10 d to examine the effects of elevated Cu²⁺ activities ({Cu²⁺}) on the growth of Sabi grass. Growth was inhibited by high Cu in solution, with a 50% reduction in the relative fresh mass occurring at 1.0 μM {Cu²⁺} for the roots and 1.2 μM {Cu²⁺} for the shoots. In solutions containing 1.2-1.9 μM {Cu²⁺}, many of the roots ruptured due to the tearing and separation of the rhizodermis and outer cortex from the underlying tissues. Transmission electron microscopy revealed that Cu-rich deposits were found to accumulate predominantly within vacuoles. Due to limited translocation of Cu from the roots to the shoots, phytotoxicity is likely to be more of a problem in remediation of Cu-toxic sites than is Cu toxicity of fauna consuming the above-ground biomass.     

Daily concentrations of trace metals in aerosols in Beijing, China, determined by using inductively coupled plasma mass spectrometry equipped with laser ablation analysis, and source identification of aerosols

This paper describes the daily concentrations of trace metals and ionic constituents in the aerosol of Beijing, China from March 2001 to August 2003. Daily PM10 concentrations were also measured from September 2001 to August 2003. The daily average PM10 concentration at Beijing, China from September 2001 to August 2003 was 171+/-117 microg m(-3) (n = 673), which is 5-fold higher than at Yokohama, Japan. Trace metal concentrations were analyzed by using inductively coupled plasma mass spectrometry equipped with a laser ablation sample introduction (LA/ICP-MS), which is a rapid and simultaneous method for multi-element analysis. The daily average metal concentrations in TSP in Beijing from March 2001 to August 2003 were: Al: 3.5+/-2.4 (n = 727), Ti: 0.47+/-0.35 (n = 720), V: 0.013+/-0.010 (n = 716), Cr: 0.019+/-0.015 (n = 618), Mn: 0.24+/-0.16 (n = 730), Fe: 5.5+/-3.9 (n = 728), Co: 0.0046+/-0.0055 (n = 629), Ni: 0.022+/-0.024 (n = 680), Cu: 0.11+/-0.11 (n = 660), Zn: 0.77+/-0.60 (n = 726), As: 0.048+/-0.047 (n = 731), Se: 0.010+/-0.010 (n = 550), Cd: 0.0068+/-0.0082 (n = 709), Sb: 0.033+/-0.036 (n = 687), and Pb: 0.43+/-0.50 (n = 728) (unit, microg m(-3)). All the metal concentrations in TSP in Beijing, China were 1.7-21.8 times higher than those in TSP in the center of Tokyo, Japan. Notably, As concentrations in TSP in Beijing were 20-fold higher than those in Tokyo. Source identification of aerosols in Beijing was carried out by using the chemical mass balance (CMB) receptor model, with the daily concentration of metals in the aerosol. The major primary sources of the aerosol of Beijing were considered to be soil dust and coal combustion. Vehicle exhaust contribution tended to increase.     

Quantum dot transport in soil, plants, and insects

Environmental risk assessment of nanomaterials requires information not only on their toxicity to non-target organisms, but also on their potential exposure pathways. Here we report on the transport and fate of quantum dots (QDs) in the total environment: from soils, through their uptake into plants, to their passage through insects following ingestion. Our QDs are nanoparticles with an average particle size of 6.5 nm. Breakthrough curves obtained with CdTe/mercaptopropionic acid QDs applied to columns of top soil from a New Zealand organic apple orchard, a Hastings silt loam, showed there to be preferential flow through the soil's macropores. Yet the effluent recovery of QDs was just 60%, even after several pore volumes, indicating that about 40% of the influent QDs were filtered and retained by the soil column via some unknown exchange/adsorption/sequestration mechanism. Glycine-, mercaptosuccinic acid-, cysteine-, and amine-conjugated CdSe/ZnS QDs were visibly transported to a limited extent in the vasculature of ryegrass (Lolium perenne), onion (Allium cepa) and chrysanthemum (Chrysanthemum sp.) plants when cut stems were placed in aqueous QD solutions. However, they were not seen to be taken up at all by rooted whole plants of ryegrass, onion, or Arabidopsis thaliana placed in these solutions. Leafroller (Lepidoptera: Tortricidae) larvae fed with these QDs for two or four days, showed fluorescence along the entire gut, in their frass (larval feces), and, at a lower intensity, in their haemolymph. Fluorescent QDs were also observed and elevated cadmium levels detected inside the bodies of adult moths that had been fed QDs as larvae. These results suggest that exposure scenarios for QDs in the total environment could be quite complex and variable in each environmental domain.