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通过标准曲线、检出限和测定范围、方法精密度、方法准确度、实际海水样品测定结果、加标回收率、分析效率和物料消耗这几方面比较了过硫酸钾氧化法、流动注射分析法和高温氧化-化学发光检测法这3种测定海水中总氮(TN)方法的优缺点。结果表明,流动注射分析法和高温氧化-化学发光检测法的测定范围更宽,精密度、准确度更好,3种样品的加标回收率达到96.2%~101%;高温氧化-化学发光检测法分析效率高、物料消耗少、节能环保,适用于一般海水样品的批量分析,且由于测定范围大,该法也适用于TN浓度较高的海水样品的批量分析,流动注射分析法因其较低的检出限更适用于TN浓度较低的海水样品的批量分析。 相似文献
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采用离子交换树脂XAD-7吸附-毛细管柱气相色谱法测定工作场所空气中乙二醇,结果表明,该方法在0 mg/L~1 116 mg/L范围内线性良好,方法检出限为0.88 mg/L,当采样体积为7.5 L时,最低检出质量浓度为0.11 mg/m3。乙二醇标准溶液测定结果的RSD为1.3%,空白加标回收率为80.1%~107%,方法的采集效率为98.0%。 相似文献
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为建立恒压氮气隔断连续流动分析法测定水样化学需氧量的分析方法,将连续流动分析法恒流空气隔断改为恒压氮气隔断,优化试剂配方和反应模块,结果表明:恒压氮气隔断法注入氮气的压力是0.06 MPa,仪器稳定时间是20~35 min,持续分析样品时间大于4 h,指标均优于恒流空气隔断法;标准曲线在2.5~40.0 mg/L范围内,相关系数大于0.999,方法检出限为0.44 mg/L,相对标准偏差为0.2%~2.6%,加标回收率在93.8%~103.8%之间,检出限优于恒流空气隔断法,精密度和正确度满足质量控制要求;实样和标样方法比对测定结果相对标准偏差小于5%,结果精密度优于标准的手工法。恒压氮气隔断连续流动分析法适用于大批量低浓度水样化学需氧量的快速检测,对于密度大、黏度大液流恒压氮气隔断具有更好的稳定性、灵敏度和正确度。 相似文献
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采用哈希快速光度法测定烟气脱硝装置的氨逃逸浓度,通过优化现场采样时的采样流量、采样枪温度、吸收液浓度和用量,以及选择合适的显色时间,使该方法在0.12 mg/m~3~5.10 mg/m~3范围内精密度与准确度良好,方法检出限为0.03 mg/m~3,2份实际样品6次测定的RSD分别为1.2%和0.1%,氨氮有证标准物质的测定结果在标准值范围内,实际样品2个浓度水平的加标回收率为100%和98.8%。将该方法与国标法同时测定实际样品和标准样品,结果无显著差异。 相似文献
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通过对某焦化厂生产过程环境空气中,可能含有的影响职工身体健康的危害因素开展了职业卫生调查,提出合理的可预防措施和建议。利用定点采样和个体采样相结合的方法对该焦化厂一期练焦生产作业环境周围及行政办公楼周边空气进行每月连续检测7 d,为期11个月的检测与分析。参照相关的职业卫生标准和规范,针对该焦化厂一期生产作业环境空气中存在的潜在有害因素种类及各项浓度及强度,进行综合分析和评价。现场检测结果表明:炼焦评价单元、行政办公楼、测温区所设定检测点的硫化氢、二氧化氮、苯、甲苯、二甲苯浓度均低于我国职业卫生规定的长时间接触允许浓度的十分之一,合格率为100%,所处的风险等级为1。此工作区域空气中所含有的有毒、有害的化学物质对人体健康带来的风险可以忽略不计。 相似文献
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“在线”监测仪与排污总量的监测 总被引:1,自引:1,他引:0
王维德 《环境监测管理与技术》2001,13(3):34-34
<环境监测管理与技术>杂志在1999年第1期发表了"监测污染物排放总量的可行性分析"一文.文中主要叙述了两种监测排污总量的方法:其一为对流量及污染物浓度均实现连续监测;其二为对流量实现连续监测而对污染物浓度的测定则是实现对流量的等比例采样,然后在实验室测定某一等比例采样时段的平均浓度. 相似文献
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A solid phase extraction method for the determination of gold(III) at trace levels by flame atomic absorption spectrometer
(FAAS) was developed. The method was based on retention of gold as chloro complexes through the Amberlite XAD-2000. The effect
of some analytical parameters including hydrochloric acid concentration, sample volume, sample and eluent flow rates, eluent
volume, eluent concentration and interfering ions on the recovery of gold(III) was investigated. The retention of gold(III)
from 1.5 mol l−1 HCl solution and the recovery of gold with 0.07 mol l−1 NH3 solution were quantitative (≥95%). The relative standard deviation (RSD) was calculated as 3.2% (n = 10). The detection limit for gold was 2 μg l−1. The accuracy was checked with the determination of gold spiked an artificial seawater and a pure copper samples. 相似文献
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José A. Murillo Pulgarín Luisa F. García Bermejo Armando Carrasquero Durán 《Environmental monitoring and assessment》2013,185(1):573-580
A flow injection analysis method based on ion chromatography and luminol chemiluminescence detection was used for the simultaneous determination of copper (II) and cobalt (II) trace levels in soils and sediments following microwave-assisted acid digestion. Detection was based on chemiluminescence (CL) of the luminol–perborate system in an alkaline medium, which is catalyzed by both transition metals. The concentration and pH of the eluent (oxalic acid) was found to affect CL intensities and retention times, both of which were inversely proportional to the oxalic acid concentration. The calibration curves for both metal ions were linear and allowed a limit of detection of 0.003 μg l?1 for cobalt (II) and 0.014 μg l?1 for cooper (II) to be calculated. The proposed method was successfully used to determine both metal ions in certified reference materials of stream and river sediments and soil samples. Based on the results, the determination is free of interferences from the usual concomitant ions. 相似文献
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目前,对固定污染源废气中磷酸雾的检测并无统一的方法,相关含磷污染物的控制指标主要是磷化氢、单质磷以及五氧化二磷。在调研国内外分析方法及相关文献的基础上,通过对几种典型含磷污染源的实样测试,提出了固定污染源废气中磷酸雾的检测方法。结果表明,使用石英滤筒捕集固定污染源废气中的磷酸雾,采样效率可达98%以上。捕集到的总磷酸雾不仅包含磷酸,还包含磷酸盐以及含磷氧化物等,是一项综合指标。该指标能够反映含磷污染物的排放特征,可为未来此类污染物的排放控制提供依据。 相似文献
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Babu SH Kumar KS Suvardhan K Kiran K Rekha D Krishnaiah L Janardhanam K Chiranjeevi P 《Environmental monitoring and assessment》2007,128(1-3):241-249
A procedure was developed for the determination of Cd, Cu, Zn, Co, Ni, Mn, Pb and Mo in water samples by inductively coupled
plasma atomic emission spectrometry (ICP-AES) after preconcentration on a morpholine dithiocarbamate (mor-DTC) supported by
bagasse (Saccharam aphisinaram). The sorbed elements were subsequently eluted with 4,M HNO3 and the acid eluates were analysed by ICP–AES. The influence of various parameters such as pH, flow rate of sample, eluent
concentration, volume of the sample and volume of eluent were investigated to enhance the sensitivity of the present method.
A 20,mL disposable syringe served as preconcentration column. Under the optimal conditions Cd, Cu, Zn, Co, Ni, Mn, Pb and
Mo in aqueous sample was concentrated about 100-fold. The sorption recoveries of elements were higher than 99.6%. The method
is also applied for the analysis of natural and spiked water samples. 相似文献
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采用直接进样法和萃取浓缩法2种前处理方式,通过超高效液相色谱-串联质谱法对水中20种拟除虫菊酯类和有机磷类农药进行了测定,并对仪器条件的选择和前处理条件的优化进行了探讨。结果表明,20种农药的线性关系良好,相关系数均>0.999,直接进样法检出限为0.21~2.47μg/L,回收率为81.0%~119%,相对标准偏差<10%。萃取浓缩法检出限为0.0022~0.0043μg/L,回收率为71.5%~115%,相对标准偏差<15%。该方法简便、快捷,精密度和准确度较高,可满足水中拟除虫菊酯类和有机磷类农药的检测要求。 相似文献
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In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L-1 HNO3 and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L?1 and 3.91 μg L?1, respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples. 相似文献
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Shabnam Shahida Akbar Ali Muhammad Haleem Khan Muhammad Mufazzal Saeed 《Environmental monitoring and assessment》2013,185(2):1613-1626
In this work, spectrophotometer was used as a detector for the determination of uranium from water, biological, and ore samples with a flow injection system coupled with solid phase extraction. In order to promote the online preconcentration of uranium, a minicolumn packed with XAD-4 resin impregnated with nalidixic acid was utilized. The system operation was based on U(VI) ion retention at pH 6 in the minicolumn at flow rate of 15.2 mL min?1. The uranium complex was removed from the resin by 0.1 mol dm?3 HCl at flow rate of 3.2 mL min?1 and was mixed with arsenazo III solution (0.05 % solution in 0.1 mol dm?3 HCl, 3.2 mL min?1) and driven to flow through cell of spectrophotometer where its absorbance was measured at 651 nm. The influence of chemical (pH and HCl (as eluent and reagent medium) concentration) and flow (sample and eluent flow rate and preconcentration time) parameters that could affect the performance of the system as well as the possible interferents was investigated. At the optimum conditions for 60 s preconcentration time (15.2 mL of sample volume), the method presented a detection limit of 1.1 μg L?1, a relative standard deviation (RSD) of 0.8 % at 100 μg L?1, enrichment factor of 30, and a sample throughput of 42 h?1, whereas for 300 s of the preconcentration time (76 mL of sample volume), a detection limit of 0.22 μg L?1, a RSD of 1.32 % at 10 μg L?1, enrichment factor of 150, and a sampling frequency of 11 h?1 were reported. 相似文献
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Ezzat M. Soliman Hadi M. Marwani Hassan M. Albishri 《Environmental monitoring and assessment》2013,185(12):10269-10280
New solid-phase extractor (MWCNTs-5-ASA) was synthesized via covalent immobilization of 5-aminsalicylic acid onto multi-walled carbon nanotubes (MWCNs). The success of the functionalization process was confirmed using Fourier transform infrared spectroscopy, scanning electron microscope, and surface coverage determination. Batch experiments were conducted as a function of pH to explore MWCNTs-5-ASA efficiency to extract several metal ions viz., Cr(III), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Pb(II). It was found that Pb(II) exhibits the highest extraction percentage with maximum adsorption capacity 32.75 mg g?1. Its binding performance was well fitted with Langmuir sorption isotherm. On the other hand, the selective separation and preconcentration of trace Pb(II) under dynamic conditions prior to determination by inductively coupled plasma-optical emission spectrometry was investigated under different parameters. These included the rate of flow and volume of sample solution, in addition to the type of the eluate, its volume and concentration. The effect of a variety of foreign ions on the recovery percentage was also evaluated. Trace Pb(II) ions present in 500 mL aqueous solution adjusted to pH 4.0 were retained on 50 mg of MWCNTs-5-ASA and completely eluted using 4.0 mL of 2 M HNO3. The limit of detection and the precision of the method were 0.25 ng mL?1 and 2.8 %, respectively (N?=?5). This methodology has been applied for the determination of Pb(II) in water samples with good results. 相似文献