便携式分光光度法现场测定污染场地地下水中铬

在硫酸介质中,用Ce~(4+)将Cr~(3+)氧化成Cr~(6+),用便携式分光光度计现场测定铬污染地下水中的Cr~(3+)、Cr~(6+)和总铬。通过试验,对氧化还原反应的可行性、反应时间、酸度、Ce~(4+)加入量、DPC用量、稳定时间、干扰因素等条件优化,使该方法在0μg/L~1 600μg/L范围内线性良好,当取样量为25 m L时,方法检出限为12.5μg/L。用该方法测定实际样品,RSD为4.4%~8.2%。用该方法与标准方法同时测定Cr~(3+)、Cr~(6+)和总铬,2种方法的相对偏差为-4.4%~4.3%。     

火柴中总铬测定的前处理方法

火柴中总铬测定的前处理方法李华于卫东夏凯（山东济宁市环境监测站，济宁２７２１４５）经试验表明，火柴样品的前处理，以采用硫酸溶液浸泡、加热消解的方法比用硝酸的为好。其步骤：向样品锥形瓶中加１５ｍｏｌ／Ｌ（１／２Ｈ２ＳＯ４）溶液５０ｍｌ，浸泡３０ｍｉｎ...     

过氧化氢氧化-全自动石墨消解仪消解-阳极溶出伏安法测定海水中总铬

采用全自动石墨消解仪加热、在碱性条件下用过氧化氢氧化海水中的三价铬,优化了极谱法测定条件,方法检出限为0.20μg/L,加标回收率为82.8%~105%,相对标准偏差5%,且对有证标准样品测试的结果符合准确度要求。方法具有选择性好、灵敏度高、准确等特点,适用于海水中总铬的测定。     

土壤样品中总铬测定方法的改进

对土壤样品中总铬的测定方法进行了改进,首次使用HNO_3-HCl-HF-HClO_4-H_3PO_4混酸体系对样品进行消解,定容后的试液经离心后用火焰原子吸收分光光度法测定。结果表明,与传统的HCl-HNO_3-HF-HClO_4消解法相比,该方法具有更高的准确度、加标回收率和精密度,可广泛应用于环境土壤中总铬的检测。     

石墨炉原子吸收法测定空气中铬酸雾

采用石墨炉原子吸收法对空气中铬酸雾进行测定,方法在待测液中铬质量浓度为1~10μg/L范围内线性良好,r=0.999 6,检出限为0.001 mg/m~3,测定结果的相对标准差为1.64%~4.53%,样品加标回收率为91.0%~95.4%,且用该方法与《固定污染源排气中铬酸雾的测定二苯基碳酰二肼分光光度法》(HJ/T 29—1999)分别测定实际样品中铬的质量浓度,结果无明显差异。     

火焰原子吸收分光光度法测定生活垃圾堆肥产品中铬

通过试验研究，建立了硝酸-氢氟酸-高氯酸消解、火焰原子吸收分光光度法测定生活垃圾堆肥产品中的铬。该方法的检出限为5mg/kg（按称取0．5g试样消解定容至50ml计算），用于不同地域堆肥样品中铬的测定，其相对标准偏差（RSD）均在8．90％以下，加标回收率介于90．9％～105．8％之间，可作为一种较理想的检验堆肥产品质量的方法。     

密闭微波消解 ICP- AES 法测定大气颗粒物中金属元素

采用过氯乙烯滤膜采集、密闭微波消解、电感耦合等离子发射光谱法测定大气颗粒物中铅、镍、铬、铜、铁、锌、锰、钡、镉,优化了试验条件.方法线性良好,各元素的检出限在0.001 mg/L～0.01 mg/L之间,滤膜样品测定的RSD为0.6%～2.9%,加标回收率为96.0%～105%.     

黄河水中六价铬和总铬的前处理和保存方式试验研究

黄河水中六价铬和总铬的前处理和保存方式试验研究解敏丽（山东省环境监测中心站，济南２５００１３）对含泥沙等悬浮物质的黄河水样，六价铬和总铬的稳定性（１）不受容器材料ＢＧ和ＰＥ的影响，保存２８天，误差＜７％；（２）在室温。４℃冷藏或用ＮａＯＨ调ｐＨｇ一１...     

ICP- AES法测定防腐处理后木材中可溶性铜铬砷

采用电感耦合等离子发射光谱法同时测定防腐处理后木材中可溶性铜、铬、砷，优化了试验条件，确定了最佳分析线。方法在0.500mg／L—10.0mg／L范围内线性良好，铜、铬、砷的检出限分别为0.003mg／L、0.01mg／L、0.07mg／L.木材样品平行测定的RSD为0.5％—1.2％，加标回收率为97.0％—102％，与原子吸收光谱法的测定结果相吻合。     

X-荧光光谱法在土壤调查中的应用

采用硼酸镶边、垫底压制土壤粉末样品,用X-荧光光谱仪分析其中铜、铅、铬、锌、镍等元素浓度。主要讨论了样品粒度对分析元素测定结果的影响。分析了标准样品及实际样品,其结果与标准值及化学法、原子吸收法测定结果相吻合。用土壤标准物质作精密度试验,统计结果表明,各组分RSD均小于3.74%。     

电感耦合等离子体质谱法测定水中痕量元素

应用电感耦合等离子体质谱法对水样(地表水、饮用水等)中铜、锌、硒、砷、镉、铬、铅、铁、锰等痕量元素进行分析测定。结果表明,方法检出限为0.01~0.78μg/L,平行测定的相对标准偏差为0.6%~7.9%,实际水样加标回收率为90.5%~103%。该方法快速、简便、线性范围大,具有良好的检出限和准确度。     

基于智能手机比色测定水环境中的六价铬

在酸性条件下,水样中的六价铬能够和显色剂二苯碳酰二肼反应生成紫红色络合物,该络合物溶液用自制的数字图像比色装置测定颜色值实现六价铬的现场快速检测。该方法在0.05 mg/L~1.00 mg/L范围内线性良好,方法检出限为0.02 mg/L,标准溶液10次测定结果的RSD为1.6%~7.9%,实际水样加标回收率为94.7%~102%。用该方法与国标法同时测定实际水样,结果无显著差异。     

离子色谱法测定地表水中总氮

采用碱性过硫酸钾消解水样，OnGuardⅡBa柱萃取、过滤，去除消解液中大量硫酸盐，离子色谱法测定地表水中总氮含量。试验表明，方法在0ms／L～20．0mg／L之间线性良好，相关系数r为0．9994，方法检出限为0．007mg／L。该方法与国标法同时测定标准物质，测定值均在定值范围内，6次平行测定结果的RSD分别为2．3％和1．8％，地表水样的加标回收率为95．7％～105％。实际水样的测定结果与国标法比对，无明显差异。     

Determination of total chromium by flame atomic absorption spectrometry after coprecipitation by cerium (IV) hydroxide

A method for the preconcentration of the total chromium based on coprecipitation with cerium (IV) hydroxide is proposed for determination of chromium by flame atomic absorption spectrometry. Different factors including carrier element amount, pH, sample volume and matrix ion effects for the precipitation were examined. The detection limit of the total chromium (k = 3, N = 15) was 0.18 μg l⁻¹. The presented method was applied for the determination of chromium in the wastewater samples from Kayseri and Nigde Organized Industrial Region-Turkey and in drinking water from our laboratory, Kayseri with satisfactory results (relative standard deviations below 8%, recoveries 95%). The analytical results obtained by the proposed method for certified copper sample was in good agreement with the certified value.     

Preconcentration and speciation of Cr(III) and Cr(VI) in water and soil samples by spectrometric detection via use of nanosized alumina-coated magnetite solid phase

A novel nanomaterial has been developed for speciation of Cr(III) and Cr(VI) in water and soil samples. In this study, a new type of alumina-coated magnetite nanoparticles (Fe₃O₄/Al₂O₃ NPs) modified by the surfactant Triton X-114 has been successfully synthesized and used in magnetic mixed hemimicelles solid-phase extraction procedure. The procedure was based on the reaction of chromium(III) with 1-(2-pyridilazo)-2-naphtol as a ligand, yielding a complex, which was entrapped “in situ” in the surfactant hemimicelles. The concentration of chromium(III) was determined using flame atomic absorption spectrometry. After reduction of Cr(VI) to Cr(III) by ascorbic acid, the system was applied to the total chromium. Cr(VI) was then calculated as the difference between the total Cr and the Cr(III) content. This method can also be used for complicated matrices such as soil samples without any special pretreatment. Under the optimum conditions of parameters, the recoveries of Cr(III) by analyzing the spiked water and soil samples were between 98.6 and 100.8 % and between 96.5 and 100.7 %, respectively. Detection limits of Cr(III) were between 1.4 and 3.6 ng?mL^?1 for water samples and 5.6 ng?mg^?1 for soil samples.     

吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯

采用吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯。当进样体积为20 mL时,方法在0.100μg/L~50.0μg/L范围内线性良好,检出限为0.05μg/L,标准溶液平行测定的RSD≤3.7%,地表水样加标回收率为91.0%~101%,方法可用于地表水中卤代烃、苯系物等其他21种挥发性有机物的同时测定。     

EDTA滴定法测定水中总硬度缓冲溶液配制的改进

针对EDTA滴定法测定水中总硬度(简称"标准法")时,存在的缓冲溶液配制繁琐、耗时长的问题,提出了缓冲溶液配制的改进方法(简称"改进法").改进法很好地克服了标准法的不足.通过地表水、地下水以及总硬度标准样品的比对测定,两法测定结果无显著差异.     

Iron-rich Oklahoma clays as a natural source of chromium in monitoring wells

Water samples, drawn from groundwater monitoring wells located southeast of Oklahoma City, OK, were found to contain elevated concentrations of total chromium with an apparent source localized to the area surrounding each well. Since these monitoring wells are located in areas with no historic chromium usage, industrial sources of chromium were ruled out. Water testing was performed on twelve monitoring wells in the area that historically had elevated total chromium concentrations ranging from 10-4900 micrograms per litre. Filtered water samples were found to be free of chromium contamination, indicating that the source of the chromium is the suspended solids. Analysis of these solids by acid digestion and a sequential extraction technique revealed that the chromium was primarily associated with iron-containing solids. X-ray diffraction identified goethite, an iron oxide hydroxide, as the dominant iron-containing phase in the suspended solids. The mineralogy in this region is dominated by interbedded red-bed sandstone and mudstone whose mineral content includes mixed-layer illite-smectite, hematite, goethite, gypsum and dolomite. Elemental analysis of soil samples collected as a function of depth in the locale of the monitoring wells indicated that the iron rich clays contain a natural source of chromium. The elevated levels of total chromium are most likely due to the dissolution of silica and alumina from the chromium containing iron clays in the basic well water, resulting in the release of fine suspended solids that naturally have high chromium concentrations. These results should be applicable to other areas containing iron-rich clays.     

荧光法快速测定水中粪大肠菌群

为研究荧光法测定水中粪大肠菌群的适用性,在6家实验室使用荧光法对粪大肠菌群的标准菌株和实际水样进行测定,并与多管发酵法进行比对。结果表明:6家实验室对标准菌株的监测结果均在误差范围内,实验室内相对误差为-2. 75%～1. 71%,准确度较高;对3个不同浓度实际水样进行精密度测定,实验室内相对标准偏差分别为1. 30%～3. 93%、1. 94%～4. 72%、1. 88%～4. 54%,实验室间的相对标准偏差分别为1. 14%、1. 59%、1. 72%,精密度较高;用荧光法与多管发酵法同时测定实际水样,2种方法测试结果线性相关性良好且变化趋势相同,对测试数据进行t检验,2种方法测试结果无显著差异。     

高效液相色谱-串联质谱法同时测定地表水中33种药物

采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)建立了地表水中25种抗生素类药物和8种非抗生素类药物的分析方法。通过重点优化质谱参数、色谱条件、样品pH、洗脱溶剂组成及用量等确定了最佳分析条件。水样经过滤、固相萃取柱富集净化后，选择Shim-pack XR-ODS为色谱柱，以乙腈和0.2%甲酸-2 mmol/L乙酸铵-水溶液为流动相进行梯度洗脱，采用电喷雾电离源，在多反应监测模式下(MRM)分析测定，内标法定量。33种药物的仪器定量限为0.012～4.68 ng/L,方法检出限为0.011～7.60 ng/L,地表水加标回收率为53.7%～122%,相对标准偏差为1.22%～32.1%(n=6)。方法成功应用于北京市凉水河12个地表水样分析，共检出32种药物，检出质量浓度为未检出～239 ng/L。利托那韦(RTV)作为新型冠状病毒诊疗方案中推荐的药物在凉水河检出率为100%。