便携式XRF在污染地块土壤金属元素调查中的应用

研究了便携式X荧光光谱仪（PXRF）测定土壤中砷、铅、铬、铜、锌和镍的性能，评估其检出限、精密度和准确度，探索了土壤水分和粒径对测定结果的影响程度，并与常规实验室分析方法测定结果进行比对。结果表明，PXRF测定土壤中砷、铅、铬、铜、锌和镍的检出限为5~15mg/kg，标准物质测定结果的相对标准偏差（RSD）≤8.6%，相对误差在±15%以内。随着土壤水分含量的增加，各金属元素测定结果均呈下降趋势，而RSD有上升趋势。土壤粒径对测定结果的影响较小，随着土壤粒径减少，各金属元素测定结果的RSD略有下降趋势。PXRF可以简单、快速地测定多种重金属元素，适用于污染地块重金属元素的现场实时监测。     

火焰原子吸收法测定水中总铬的干扰与消除

考察采用《水质铬的测定火焰原子吸收分光光度法》(HJ757-2015)测定水中总铬时,前处理过程中硝酸的加入量对测定结果的影响,同时考察了Fe、Co、Ni、K、Ca、Na、Mg、Al八种共存离子对铬测定的干扰及消除情况,结果表明:20%以上的硝酸对铬的测定有负干扰,1mg/L的Fe和Ni、2mg/L的Co、5mg/L的Mg、20mg/L的Al、100mg/L的Ca对铬的测定有负干扰,500mg/L的Na和K对铬的测定没有干扰,加入氯化铵后上述干扰均可消除。     

AMA254汞分析仪测定颗粒物中痕量总汞的研究

采用AMA254汞分析仪测定大气颗粒物和煤中的痕量总汞,建立了直接测定颗粒物中痕量总汞的分析方法.测定结果表明,在汞绝对含量为0～35ng范围内线性良好,测定大气颗粒物和煤中的痕量总汞的检出限分别为0.06ng/m3和0.02ng/g,标准样品测定的RSD≤0.78%,加标回收率为92%～108%.该方法具有无需消解直接进样测定、极其简便、省时等特点,适合多种固体样品中痕量汞的测定.     

固体废物氰化物总量和浸出毒性测定方法的比较

中国现行的固体废物氰化物总量和氰化物浸出毒性的分析方法存在缺陷，不便于广泛指导监测工作，笔者优化了固体废物氰化物测定的前处理方法，明确了固体废物氰化物总量、氰化物浸出毒性测定时的样品粒径、浸提方法和消解方法，建立了容量法、分光光度法、流动注射法测定固体废物氰化物总量和浸出毒性的方法，并与标准方法（离子色谱法）进行比较。实验结果表明：容量法、分光光度法、流动注射法测定结果与离子色谱法无显著差异，3种方法测定固体废物氰化物总量加标回收率为80.5%~102%，平行样测定相对标准偏差为3.0%~6.9%，3种方法测定固体废物氰化物浸出毒性加标回收率为80.1%~107%，平行样测定相对标准偏差为7.8%~9.5%，3种方法测定结果精密度和准确度良好，均能够满足固体废物氰化物总量和氰化物浸出毒性的测定要求。其中容量法、分光光度法由于其仪器设备简单、操作简便，可用于突发环境事件应急监测等情况下固体废物氰化物的测定。但容量法检出限较高，不能满足评价标准较低的分析测试工作要求，离子色谱法、分光光度法和流动注射法检出限均能满足一般分析测试要求。     

用火焰原子吸收法测定镀铬泥渣中的铁、镍、铜、锌、铅

我们曾对镀铬泥渣中铬的原子吸收测定进行了研究,本文重点研究镀铬泥渣中Fe、Ni、Cu、Zn、Pb测定时共存元素的干扰及其消除方法。 实验证明,大量Ni、Si的存在严重干扰铁的测定,大量Cu的存在严重干扰Ni的测定。采用标准加入法以消除Ni对Fe的干扰;采用沉淀法,萃取法分离铁与镍;在标液中加入等量铜来消除大量铜对测定镍的干扰,都难免繁琐费时。本文采用加入十二烷基硫酸钠或柠檬酸作干扰抑制剂,消除了大量铜对镍及大量硅对铁、锌测定的干扰;用降低乙炔流量,提高火焰温度的方法消除了二倍量的镍对铁测定的干扰,拟定了用火焰原子吸收法,不经分离直接测定镀铬废水处理后的泥渣中铁、镍、铜、锌、铅的测定程序。样品分析精密度均小于±4％,铁、镍、铜、铅的标准加入回收率为96—106％,锌为90—115％,用于实际样     

气相色谱法测定元素磷时应注意的几个问题

阐述了气相色谱法测定水中元素磷时盐析剂、振荡次数（幅度）、振荡时间和干扰物对测定的影响，确定了最佳测定条件及消除干扰的方法。     

影响地表水中总磷测定的因素探讨

总磷是评价水质的一项重要指标,现对样品中悬浮物(泥沙)含量、加酸保存样品保存时间与调节pH值对总磷测定的影响进行研究。结果表明,随着沉降时间的延长总磷测定值逐渐降低,加酸保存的样品总磷测定值随保存时间的延长而增高,且测定时是否调回中性对测定结果基本无影响。故进行地表水中总磷的测定需严格按照标准规定的样品采样过程控制采样沉降时间,加酸保存,24 h以内进行测定,测定时无需调回中性。     

离子色谱法测定环境空气中氯化氢降低空白值的方法

用离子色谱法测定环境空气中低浓度氯化氢,是通过测定氯离子质量浓度间接测定氯化氢的质量浓度,测定过程极易受外来氯离子的干扰,使空白值偏高。通过试验确定测定过程中可能存在氯离子干扰的环节,并采取一系列方法消除前期准备、采样和分析全过程中的干扰,以降低空白值。     

便携式XRF土壤重金属检测仪在环境应急监测中的应用探讨

系统评估了便携式XRF重金属检测仪的精密度、准确度及测定影响因素,开展了该方法测定土壤中Cu、Zn、As、Pb、Cr与国标分析方法的系统比对。结果表明:上述5种元素的方法检出限为5.7 mg/kg~16.0 mg/kg,土壤标准样品测定6次结果的RSD为1.0%~4.7%,Zn、Pb和As测定结果的相对误差10%;与国标法相比,便携式XRF重金属检测仪测定Cu、Zn、As、Pb的准确度较好,测定Cr的准确度波动较大。将该方法用于应急污染事故监测,可迅速锁定污染物及污染区域,实现野外分析的预判。     

用正交试验确定游离性余氯最佳测定条件

在用DPD光度法测定水中余氯时，对水样的pH值、显色时间、显色剂用量和反应温度进行了研究，通过正交试验系统地分析了各因素影响测定结果准确性的程度，并获得最佳的反应条件，表明在该条件下测定水中余氯的准确性优于其他条件下测定的结果。     

Assessment and spatial distribution of groundwater quality in industrial areas of Ghaziabad, India

An attempt has been made in this study to evaluate the groundwater quality in two industrial blocks of Ghaziabad district. Groundwater samples were collected from shallow wells, deep wells and hand pumps of two heavily industrialized blocks, namely Bulandshahar road industrial area and Meerut road industrial area in Ghaziabad district for assessing their suitability for various uses. Samples were collected from 30 sites in each block before and after monsoon. They were analyzed for a total of 23 elements, namely, Ag, Al, As, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, Se, U, V, and Zn. In addition to these elements, some other parameters were also studied viz: color, odor, turbidity, biological oxygen demand, chemical oxygen demand (COD), dissolved oxygen, total dissolved solids and total suspended solid. The water quality index was also calculated based on some of the parameters estimated. Out of the 23 elements, the mean values of 12 elements, namely, Al, As, Ca, Cd, Cr, Mg, Mn, Na, Ni, Pb, Se, and U, were higher than the prescribed standard limits. The concentrations (in milligram per liter) of highly toxic metals viz., Al, As, Cd, Cr, Ni, Pb, Se, and U, ranged from 1.33–6.30, 0.04–0.54, 0.005–0.013, 4.51–7.09, 0.14–0.27, 0.13–0.32, 0.16–2.11, and 0.10–1.21, respectively, in all groundwater samples, while the permissible limits of these elements as per WHO/BIS standards for drinking are 0.2, 0.01, 0.003, 0.05, 0.07, 0.01, 0.04, and 0.03 mg L^?1, respectively. The EC, pH, and COD in all samples varied from 0.74–4.21, 6.05–7.72, and 4.5–20.0 while their permissible limits are 0.7 dS m^?1, 6.5–8.5, and 10 mg L^?1, respectively. On the basis of the above-mentioned parameters, the water quality index of all groundwater samples ranged from 101 to 491, and 871 to 2904 with mean value of 265 and 1,174 based on two criteria, i.e., physico-chemical and metal contaminations, respectively while the prescribed safe limit for drinking is below 50. The results revealed that the groundwater in the two blocks is unfit for drinking as per WHO/BIS guidelines. The presence of elements like As, Se, and U in toxic amounts is a matter of serious concern.     

Monitoring of pesticide residues in market basket samples of vegetable from Lucknow City, India: QuEChERS method

The study was conducted on 20 vegetables including leafy, root, modified stem, and fruity vegetables like bitter gourd, jack fruit, french-bean, onion, colocassia, pointed gourd, capsicum, spinach, potato, fenugreek seeds, carrot, radish, cucumber, beetroot, brinjal, cauliflower, cabbage, tomato, okra, and bottle gourd. Forty-eight pesticides including 13 organochlorines (OCs), 17 organophosphates (OPs), 10 synthetic pyrethriods (SPs), and eight herbicides (H) pesticides were analyzed. A total number of 60 samples, each in triplicates, were analyzed using Quick, Easy, Cheap, Effective, Rugged, and Safe method. The quantification was done by GC-ECD/NPD. The recovery varies from 70.22% to 96.32% with relative standard deviation (RSD) of 15%. However the limit of detection ranged from 0.001?C0.009 mg kg^???1 for OCs, SPs, OPs, and H, respectively. Twenty-three pesticides were detected from total 48 analyzed pesticides in the samples with the range of 0.005?C12.35 mg kg^???1. The detected pesticides were: ??-HCH, Dicofol, ??-Endosulfan, Fenpropathrin, Permethrin-II, ??-cyfluthrin-II, Fenvalerate-I, Dichlorvos, Dimethoate, Diazinon, Malathion, Chlorofenvinfos, Anilophos, and Dimethachlor. In some vegetables like radish, cucumber, cauliflower, cabbage, and okra, the detected pesticides (??-HCH, Permethrin-II, Dichlorvos, and Chlorofenvinfos) were above maximum residues limit (MRL) (PFA 1954). However, in other vegetables the level of pesticide residues was either below detection limit or MRL.     

Community air monitoring for pesticides—part 2: multiresidue determination of pesticides in air by gas chromatography,gas chromatography–mass spectrometry,and liquid chromatography–mass spectrometry

Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography–mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37–104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70–170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air.     

Heavy Metal Pollution of Surface Soil in the Thrace Region, Turkey

Abstact Samples of surface soil were collected at 73 sites in the Thrace region, northwest part of Turkey. Two complementary analytical techniques, epithermal neutron activation analysis (ENAA) and atomic absorption spectrometry (AAS) with flame and graphite furnace atomization were used to determine 35 elements in the soil samples. Concentrations of As, Cd, Co, Cu, Mn, Ni, Pb and Zn were determined using AAS and GF AAS, and ENAA was used for the remaining 27 elements. Results for As, Ba, Br, Ca, Cd, Ce, Co, Cr, Cs, Cu Eu, Fe, Hf, I, In, K, La, Mn, Mo, Na, Nd, Ni, Pb, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Th, Ti, U, V and Zn are reported for the first time for soils from this region. The results show that concentrations of most elements were little affected by the industrial and other anthropogenic activities performed in region. Except for distinctly higher levels of Pb, Cu, Cd and Zn in Istanbul district than the median values for the Thrace region, the observed distributions seem to be mainly associated with lithogenic variations. Spatial distributions of As, Cd, Cr, Cu, Ni, Pb and Zn were plotted in relation to the concentration values in soil using Geographic Information System (GIS) technology     

石河子市地下水环境背景值

采集并测定了石河子市１９个地下水背景水样，分别确定了该市潜水和承压—自流水中Ｋ＋、Ｎａ＋、Ｃａ２＋、Ｍｇ２＋、Ｃｌ－、ＳＯ、ＨＣＯ、ＮＯ、Ｆ－、总硬度、矿化度、可溶性ＳｉＯ２、ＣＯＤ、ｐＨ、Ｃｕ、Ｐｂ、Ｚｎ、Ｃｄ、Ｍｎ、Ｖ、Ｌｉ、Ｍｏ、Ｓｅ、Ｈｇ、Ｉ、Ａｓ、Ｃｒ＋５、Ｃ６Ｈ５ＯＨ、ＣＮ－、ＡＢＳ的环境背景值．     

Variation of heavy metal and micro and macro element concentrations of bread and durum wheats and their relationship in grain of Turkish wheat cultivars

The 64 varieties displayed a large variation for all mineral elements, investigated Fe, Mn and Zn, ranging from 24.2 to 43.1 mg/kg, 27.6 to 64.8 mg/kg and 10.4 to 38.2 mg/kg, respectively. The mean Ca, K, Mg, Na, P and S concentrations in wheat rain varieties amounted to 378, 4,266, 1,183, 317, 3,513 and 1,542 mg/kg, respectively. Ca, K, Mg, Na, P and S contents of wheat varieties changed at the levels between 266 and 531 mg/kg, 3,029 and 5,566 mg/kg, 972 and 1,525 mg/kg, 277 and 368 mg/kg, 2,422 and 4,610 mg/kg and 1,241 to 2,052 mg/kg, respectively. The concentrations of Al, Cu, Fe, Mn and Zn of durum wheat samples were found at high levels. The mean Al, Cr, Mo, Ni, Cu, Fe, Mn and Zn concentrations in durum wheat varieties amounted to 10.93, 0.47, 0.72, 0.72, 5.37, 34.9, 37.28 and 20.88 mg/kg, respectively.     

Community air monitoring for pesticides. Part 3: using health-based screening levels to evaluate results collected for a year

The CA Department of Pesticide Regulation (CDPR) and the CA Air Resources Board monitored 40 pesticides, including five degradation products, in Parlier, CA, to determine if its residents were exposed to any of these pesticides and, if so, in what amounts. They included 1,3-dichloropropene, acrolein, arsenic, azinphos-methyl, carbon disulfide, chlorpyrifos and its degradation product, chlorthalonil, copper, cypermethrin, diazinon and its degradation product, dichlorvos, dicofol, dimethoate and its degradation product, diuron, endosulfan and its degradation product, S-ethyl dipropylcarbamothioate (EPTC), formaldehyde, malathion and its degradation product, methyl isothiocyanate (MITC), methyl bromide, metolachlor, molinate, norflurazon, oryzalin, oxyfluorfen, permethrin, phosmet, propanil, propargite, simazine, SSS-tributylphosphorotrithioate, sulfur, thiobencarb, trifluralin, and xylene. Monitoring was conducted 3 days per week for a year. Twenty-three pesticides and degradation products were detected. Acrolein, arsenic, carbon disulfide, chlorpyrifos, copper, formaldehyde, methyl bromide, MITC, and sulfur were detected in more than half the samples. Since no regulatory ambient air standards exist for these pesticides, CDPR developed advisory, health-based non-cancer screening levels (SLs) to assess acute, subchronic, and chronic exposures. For carcinogenic pesticides, CDPR assessed risk using cancer potency values. Amongst non-carcinogenic agricultural use pesticides, only diazinon exceeded its SL. For carcinogens, 1,3-dichloropropene concentrations exceeded its cancer potency value. Based on these findings, CDPR has undertaken a more comprehensive evaluation of 1,3-dichloropropene, diazinon, and the closely related chlorpyrifos that was frequently detected. Four chemicals—acrolein, arsenic, carbon disulfide, and formaldehyde—sometimes used as pesticides were detected, although no pesticidal use was reported in the area during this study. Their presence was most likely due to vehicular or industrial emissions.     

微波消解-电感耦合等离子体质谱法同时测定废水中20种元素

采用微波消解-电感耦合等离子体质谱法,同时测定了废水中Be、V、Cr、Mn、Co、Ni、Cu、Zn、As、Se、Mo、Ag、Cd、Sb、Ba、Hg、Tl、Pb、Th、U等20种元素,比较了5种不同消解体系对废水样品的加标回收结果,确定采用硝酸+过氧化氢消解体系。Hg在0.050μg/L～2.00μg/L、其他元素在5.00μg/L～500μg/L范围内线性良好,检出限为0.01μg/L～0.2μg/L,国家有证标准物质的测定结果符合要求,废水样品平行测定的RSD为2.6%～6.5%,加标回收率为84%～110%。     

Monitoring of trace elements in honey from the Republic of Macedonia by atomic absorption spectrometry

Contents of Zn, Cu, Fe, Mn, Cd, Na, K, Ca and Mg in 123 honey samples from different regions of the Republic of Macedonia were determined by atomic absorption spectrometry. A microwave digestion system was applied for digestion of the samples. The mean content for the elements determined was found to be: 2.252, 0.696, 1.885, 1.752, 0.004, 29.52, 984.8, 40.11, 18.24 mg kg(-1) for Zn, Cu, Fe, Mn, Cd, Na, K, Ca and Mg, respectively. Based on a comparison of statistical parameters, the spatial distribution of particular elements in Macedonian honey and the results of factor analysis, two natural and one anthropogenic geochemical associations were identified. The natural geochemical associations (Mg, Mn, Ca, K and Fe, Zn, Ca, -K, -Na) are influenced mainly by lithology. The anthropogenic associations (Cd and -Cu) are mostly a result of metallurgical activities, namely lead production in the town of Veles.     

Trace metals in aerosol at Terra Nova Bay, Antarctica

Atmospheric particulate with an aerodynamic diameter <10 microm (PM10) was sampled continuously during the austral summers of 2000-2001 and 2001-2002 at a coastal site near to the Italian base of Terra Nova, Antarctica. Li, Pb, Cd, U, Ba, Bi, Cs, Rb, Tl, Sr, Al, V, Fe, Cu, Mn, Zn, Co, Ag were determined by inductively coupled sector field mass spectroscopy (ICP-SFMS) after sample digestion by a combination of HF, HNO3, and H2O2 in ultraclean conditions. Quality control of the analytical procedure was carried out by blank control, by evaluating the limits of detection, recoveries and repeatability. Concentrations found are extremely low for most metals, confirming the high purity of Antarctic aerosol. Principal Component Analysis (PCA) highlights high correlations among Pb, Cr, Bi, Cu and Zn concentration values and among Li, U, Ba, Cs, Rb, Al, V, Fe, Mn, Co concentration values permitting the identification of two principal source groups, namely crustal dust and human emission activities. Elements of anthropogenic origins (Pb, Cr, Cu, Zn) were highly enriched with respect to their crustal composition.