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杨峻 《广东微量元素科学》2005,12(2):27-34
对氢化物发生-原子荧光法测定土壤中砷的不确定度进行了分析,找出影响不确定度的因素,对不确定度进行评估,给出不确定度,能如实反映测量的置信度和准确度。 相似文献
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对用氢化物发生原子荧光光谱法联合测定水中砷、硒的测量结果进行了不确定度评定。分析了测量不确定度的来源,如标准物质、样品取样体积、样品稀释体积、工作曲线的非线性及测量结果的重复性,对各不确定度分量进行了评定和计算。砷、硒含量测量的扩展不确定度均为5.28%。 相似文献
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根据原子荧光光度法,用AFS-9700双道原子荧光光度计测定水样中的总锑含量,并且分析了主要的测量不确定度来源,即标准溶液引入的不确定度、建立工作曲线引入的不确定度、回收率引入的不确定度和重复测量样品引入的不确定度,对测量不确定度进行计算和评定,合成测得总锑含量的不确定度为0.10?g/L。 相似文献
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原子荧光光谱法测定方便米饭中砷的测量不确定度评定 总被引:2,自引:0,他引:2
蔡秋 《理化检验(化学分册)》2007,43(2):122-126
介绍了原子荧光光谱法测定方便米饭中砷的测量不确定度评定方法,该法根据最小二乘法原理计算校准曲线的标准不确定度,并充分分析和识别分析过程中的不确定度来源,较为全面地评定了测量不确定度,该法对原子吸收光谱法、电感耦合等离子发射光谱法和原子荧光光谱法等测定结果的不确定度评定具有参考作用。 相似文献
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依据JJF 1059-1999,对氢化物发生原子荧光法测定聚氯化铝中的砷含量进行不确定度评定。建立了数学模型,对各不确定度分量进行了分析和量化。计算出相对合成标准不确定度为0.0095,扩展不确定度为0.032mg/kg。砷含量测量不确定度主要来源于测量样品测试液中砷浓度产生的不确定度。 相似文献
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通过建立数学模型,分析了原子荧光法测定金矿中砷和铋的测量不确定度的影响因素,计算各影响因素的不确定度分量,并计算金矿中砷和铋的合成标准不确定度和扩展不确定度.结果表明:测量不确定度主要由样品制备过程和标准曲线拟合构成.金矿中砷的含量为18.398μg/g,其扩展不确定度为0.555 3μg/g(k=2),结果符合测试规范要求.铋的含量为0.359 3μg/g,扩展不确定度为0.441 1μg/g(k=2),铋的不确定度偏大,不符合测试规范要求,应通过降低铋标准溶液的浓度和减少待测液的稀释倍数来降低标准曲线拟合产生的不确定度. 相似文献
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玩具材料和玩具部件按《玩具安全》(GB6675—2014)规定的程序制样和用盐酸提取后,加入硫脲-抗坏血酸将提取溶液中砷预还原为适合氢化物发生的价态As(Ⅲ),再加入硼氢化钾使其还原成砷氢化物,建立了原子荧光光谱法测定玩具材料中可迁移砷含量的方法。方法的检出限为0.017mg/kg,多种代表性玩具材料的砷元素加标回收率在94.4%~104%。方法适用于各种玩具材料中可迁移砷的分析。 相似文献
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A simple, sensitive and interference-free method was proposed for the determination of arsenic, based on the generation of volatile arsenic trichloride coupled with atomic fluorescence spectrometry. Thiourea, together with l-ascorbic acid, was used to reduce As(V) to As(III), and the chloride generation was based on the reaction between As(III) and hydrochloric acid. Under the optimized experimental conditions, the present procedure allows for the quantification of arsenic in the concentration range of 0.01–4.0 mg L−1, with a limit of detection (3σ) of 6.0 μg L−1. The relative standard deviation (R.S.D.) is 4.0% for 0.1 mg L−1 arsenic (n = 7). Finally, the proposed method was successfully applied to the determination of arsenic in several certified reference samples (stainless steel, alloy steel, copper alloy and water sample) and real samples (brass material and spiked cobalt material), with analytical results well-agreed with those by ICP-MS. 相似文献
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改变原子荧光光谱法以稀酸为载流的进样方式,以水为载流在新型双道原子荧光光谱仪上同时测定了土壤中的痕量砷(As)、汞(Hg)。方法采用王水水浴加热溶解样品,用50 g/L硫脲-抗坏血酸混合溶液预先将砷还原为+3价,保持10%(体积分数)以上盐酸浓度,不转移直接定容静置后测定。优化了仪器工作条件,详细考察了以水为载流测定的可行性,选择了同时测定As、Hg所需的硼氢化钾浓度和盐酸浓度。方法节省了酸试剂用量,操作快速,单个样品测定仅需20s左右。方法检出限As为0.005 mg/kg,Hg为0.0008 mg/kg,相对标准偏差(RSD%,n=7)在1.0%~7.4%,经土壤国家标准物质和实际样品验证,适合土壤中痕量As、Hg的同时快速测定。 相似文献
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Concentrated perchloric acid is used to digest coal for subsequent determination of arsenic and selenium by hydride-generation atomic absorption and fluorescence spectrometry. Arsenic and selenium are removed from potentially interfering metal ions by coprecipitation with lanthanum hydroxide. The detection limits, 58 and 36 ng g?1 by atomic absorption and 25 and 10 ng g?1 by atomic fluorescence, for arsenic and selenium in coal, respectively, are adequate for the normal levels of these metals. 相似文献
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A procedure is described for simultaneous determination of arsenic, selenium, tin and mercury in aqueous solution by non-dispersive atomic-fluorescence spectrometry. Radiofrequency-excited EDLs, 100% modulated in the kHz region, were used for atom excitation. Sodium tetrahydroborate was used as reductant and a hydrogen-argon miniflame as atomizer. In the optimized procedure, which uses 1 ml of sample, the limits of detection (three times the standard deviation of the blank) were 0.04, 0.08, 0.1 and 0.1 ng ml for arsenic, selenium, tin and mercury respectively. The linear dynamic range was greater than three decades for all analytes and the precision was better than 7% (typically 3%) for concentrations 1 ng ml . Results for mutual interference effects are reported. Copper, nickel, lead and cobalt interfered only with selenium (5 ng ml ), when present in at least 200-fold weight ratio to it. Using 5 ml of sample improved the limits of detection for selenium and arsenic (0.01 and 0.02 ng ml respectively), but at the expense of greater interference. Recovery from spiked natural water samples was better than 95% at the ng ml level, except for selenium in sea-water, when the recovery was only 85%. Determination of the four elements, including standard-addition and background measurements, requires about 10 min. 相似文献
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应用自行设计的化学蒸气发生-四通道无色散原子荧光光谱仪,建立了同时测定水样中As、Sb、Se、Hg的新方法.在实验中优化了四元素同时化学蒸气发生条件和测定的最佳工作参数.在样品预处理阶段用HCl将Se6+还原为Se4+,然后用质量浓度5 g/L硫脲将As5+和Sb5+还原为As3+和Sb3+.在最佳条件下,方法对As、Sb、Se、Hg的检出限分别为0.05、0.03、0.05、0.01 ng/mL(3d);RSD分别为0.42%、0.74%、0.97%、1.0%(对5 ng/mL As、Sb、Se和0.5ng/mL Hg混合标准,n=7).用所建立的方法对不同类型水样中的As、Sb、Se、Hg进行了同时测定,测定结果与用标准方法测定所得结果之间无明显差异,各元素的加标回收率在93%~105%. 相似文献
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Determination of total arsenic in seawater by hydride generation atomic fluorescence spectrometry 总被引:1,自引:0,他引:1
Carolina L.T. Correia Marlo S. Azevedo Reinaldo C. Campos 《Microchemical Journal》2010,96(1):157-3927
In this work, the determination of total As in seawater by hydride generation atomic fluorescence spectrometry was studied. The influence of the chemical, flow and instrumental parameters were investigated and optimized. The pre-reduction of As(V) to As(III) was performed using KI plus ascorbic acid in 3.5 mol L− 1 HCl medium. No multiplicative interference was present and external aqueous calibration could be used. The limit of detection was 36 ng L− 1, while the repeatability was 2% (n = 10), at a 500 ng L− 1 concentration level. The sample throughput was 15 h− 1 if triplicate measurements were made. The accuracy was assessed by the analysis of a seawater certified reference material and excellent agreement between the obtained and certified values was verified. The procedure was used for the analysis of seawater offshore samples collected at the Brazilian coast and results ranging from 860 to 1200 ng L− 1 were found. 相似文献
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The potential of coupling anion-exchange high-performance liquid chromatography, hydride generation and atomic fluorescence spectrometry (HPLC–HG–AFS) for arsenic speciation is considered. The effects of hydrochloric acid and sodium tetrahydroborate concentrations on signal-to-background ratio, as well as argon and hydrogen flow rates, were investigated. Detection limits for arsenite, dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and arsenate were 0.17, 0.45, 0.30 and 0.38 μg l−1, respectively, using a 20-μl loop. Linearity ranges were 0.1–500 ng for As(III) and MMA (as arsenic), and 0.1–800 ng for DMA and As(V) (as arsenic). Arsenobetaine (AsB) was also determined by introducing an on-line photo-oxidation step after the chromatographic separation. In this case the limits of detection and linear ranges for the different species studied were similar to the values obtained previously for As(V). The technique was tested with a human urine reference material and a volunteer's sample. © 1998 John Wiley & Sons, Ltd. 相似文献