电感耦合等离子体质谱法测定生活饮用水中钡的不确定度评定

评定电感耦合等离子体质谱（ICP-MS）法测定生活饮用水中钡含量的不确定度。根据JJF 1059.1—2012《测量不确定度评定与表示》对各个不确定度来源（包括采样、样品保存、系列标准溶液的配制、校准曲线拟合和测量重复性）进行分析和量化，获得扩展不确定度。生活饮用水中钡的扩展不确定度为2.9μg/L，钡的测量结果为（50.3±2.9）μg/L。结果表明，方法的不确定度主要来源于系列标准溶液配制过程。     

火焰原子吸收光谱法测定汽油中锰的不确定度评价

分析与讨论了汽油中锰含量测定过程中的不确定度来源,并对各个不确定度分量进行量化与合成,计算出火焰原子吸收光谱法测定汽油中锰含量的相对合成不确定度为0.083（锰含量约为10 mg/L）,扩展不确定度U为1.8 mg/L（置信水平为95%,k=2）. 比较各个不确定度分量可知,测定结果的不确定度主要源自标准工作溶液的最小二乘法拟合.     

原子吸收法测定蔬菜罐头中铜含量的测量不确定度评定

对GB／T 5009．13－1996《食品中铜的测定方法》中火争原子吸收法测定蔬菜罐头中铜含量的测量不确定度进行评定，根据JJF1059－1999《测量不确定度评定与表示》技术规范的要求，分析了该测量过程的测量不确定度来源，建立了数学模型，并利用标准样品对测量不确定度的各个分量进行计算，计算得该测定水平下铜含量测定结果的扩展不确定度为0．2mg/kg.     

石墨炉原子吸收法测定酱卤肉中铬的不确定度评定

对石墨炉原子吸收光谱法测定酱卤肉中铬的不确定度进行评定。参照GB 5009.123–2014,采用微波消解–石墨炉原子吸收法测定酱卤肉制品中铬含量,分析不确定度来源,包括测量重复性、标准工作溶液浓度、定容体积、称样质量、样品处理等,对各类不确定度分量进行评定,最终合成得到标准不确定度和扩展不确定度。当酱卤肉制品中铬含量为0.23 mg/kg时,测定结果在95%置信水平时的扩展不确定度为0.017 mg/kg(k=2)。石墨炉原子吸收光谱法测定酱卤肉中铬的不确定度主要来源于测量重复性、铬标准溶液浓度和样品消解处理过程。评定结果可为提高原子吸收法测定肉制品中铬含量的准确性提供参考。     

微波消解-石墨炉原子吸收测定化妆品中微量砷的不确定度评定

建立对微波消解-石墨炉原子吸收法测定化妆品中微量砷的不确定度评定方法.建立有效的数学模型,对影响因素进行全面分析,并评定各因素的不确定度.扩展不确定度为0.25mg/kg,测量结果表示为2.00±0.25 mg/kg(k=2).测量不确定度的来源主要为样品检测的回收率产生的不确定度和重复性引起的不确定度.     

原子吸收光谱法测量不确定度的评定与应用

介绍了测量不确定度的一般评定方法。并以火焰原子吸收光谱法测定奶粉中铜含量为例,研究了原子吸收光谱法不确定度的评定步骤和计算过程。     

ICP—AES测定水样中金属含量的不确定度评定

以ICP-AES法测定水样中铜元素为例,分析来自标准溶液配制过程和仪器测定过程的各种不确定度影响因素,建立了测量不确定度评定数学模型,对各不确定度分量进行了评定与计算,当铜的质量浓度为4.1852 mg/L时,测量结果的扩展不确定度为0.0361 mg/L(k=2).     

燃烧氧化-非分散红外吸收法测定水中总有机碳的不确定度评定

评定燃烧氧化-非分散红外吸收法测定水中总有机碳的测量不确定度。根据JJF1059.1—2012《测量不确定度评定与表示》、CNAS-GL006—2019《化学分析中不确定度的评估指南》,该测量方法的不确定度来源主要有标准物质、溶液配制、校准曲线拟合、测量重复性。对各不确定度分量进行评定,最终合成得到测量结果的相对标准不确定度为1.34%,水样总有机碳质量浓度测定结果表示为(48.28±1.30)mg/L(k=2)。测量重复性是影响测量不确定度的主要因素,校准曲线拟合、标准物质的影响较小。     

固相萃取-高效液相色谱法测定水中呋喃丹含量的不确定度评定

采用固相萃取-高效液相色谱法测定水中呋喃丹浓度,对测量结果的不确定度进行了评定。根据《测量不确定度评定与表示(》JJF 1059-1999)中有关规定,建立呋喃丹不确定度分析数学模型。结果表明,该方法测量结果不确定度的主要来源为标准溶液的配制、定容和重复性测试,当水样中呋喃丹的浓度为0.03 mg/L时,扩展不确定度为0.0044 mg/L(k=2)。     

火焰原子吸收光谱法测定镁及镁合金中镉含量不确定度评定

采用火焰原子吸收光谱法测定镁及镁合金中镉含量,对测定结果不确定度进行评定.建立数学模型,分析不确定度来源,计算合成标准不确定度和扩展不确定度.当镁及镁合金中镉含量为0.00418％时,其扩展不确定度为0.00034％(k=2).火焰原子吸收光谱法测定镁及镁合金中镉含量不确定度主要来源于样品称量、样品消解溶液定容、标准工...     

Separation and preconcentration of trace manganese from various samples with Amberlyst 36 column and determination by flame atomic absorption spectrometry

This work assesses the potential of a new adsorptive material, Amberlyst 36, for the separation and preconcentration of trace manganese(II) from various media. It is based on the sorption of manganese(II) ions onto a column filled with Amberlyst 36 cation exchange resin, followed by the elution with 5 mL of 3 mol/L nitric acid and determination by flame atomic absorption spectrometry (FAAS) without interference of the matrix. Different factors including pH of sample solution, sample volume, amount of resin, flow rate of sample solution, volume and concentration of eluent, and matrix effects for preconcentration were investigated. Good relative standard deviation (3%) and high recovery (>95%) at 100 μg/L and high enrichment factor (200) and low analytical detection limit (0.245 μg/L) were obtained. The adsorption equilibrium was described well by the Langmuir isotherm model with maximum adsorption capacity of 88 mg/g of manganese on the resin. The method was applied for the manganese determination by FAAS in tap water, commercial natural drinking water, commercial treated drinking water and commercial tea bag sample. The accuracy of the method is confirmed by analyzing the certified reference material (tea leaves GBW 07605). The results demonstrated good agreement with the certified values.     

火焰原子吸收法测定ZnS：Mn交流电致发光薄膜屏中锰

利用火焰原子吸收光度法，分别测定了ＺｎＳ：Ｍｎ交流电致发光薄膜屏中锰和锌的含量，当样品符合硫化锌的化学量时，可由锌的含量计算出硫化锌的质量和锰在硫化锌薄膜中的浓度。与处理样品的称样量相比较，方法相比误差小于２％，回收率和相对标准偏差分别为１００％－１０２％和０．７％。样品自理容易分析简易，快速。     

浸提法-火焰原子吸收光谱法测化妆品中镉的不确定度分析

对浸提法消化试样和火焰原子吸收光谱法测定化妆品中的镉进行不确定度分析。对各主要不确定度的来源进行分析,为有效控制该法测定化妆品的镉含量提供可靠理论依据。     

塞曼火焰原子吸收法测定黄河水体的总硬度

采用原子吸收分光光度法测定黄河水体的总硬度,钙的浓度在0.100～5.00 mg/L、镁的浓度在0.0500～2.00 mg/L范围内分别与吸光度呈线性关系,线性方程分别为A=0.045 5c+8.354×10~(-5)、A=0.514c+8.354×10~(-5),相关系数均为0.9999。黄河水样6次测定结果的相对标准偏差为1.2％,t检验结果表明,该法与EDTA络合滴定法测定结果无显著性差异。     

Optimization of a new resin, Amberlyst 36, as a solid-phase extractor and determination of copper(II) in drinking water and tea samples by flame atomic absorption spectrometry

A new simple and reliable method has been developed to separate and preconcentrate trace copper ion in drinking water and tea samples for subsequent measurement by flame atomic absorption spectrometry (FAAS). The copper ions are adsorbed quantitatively during passage of aqueous solutions through Amberlyst 36 cation exchange resin. After the separation and preconcentration stage, the analyte was eluted with a potassium cyanide solution and determined by FAAS. Different factors including pH of sample solution, sample volume, amount of resin, flow rate of aqueous solution, volume and concentration of eluent, and matrix effects for preconcentration were examined. The analytical figures of merit for the determination of copper are as follows: analytical detection limit (3 sigma), 0.26 microg/L; precision (RSD), 3.1% for 100 microg/L; enrichment factor, 200 (using 1000 mL of sample solution and 5 mL of eluent); time of analysis, 3.5 h (for obtaining enrichment factor of 200); capacity of resin, 125 mg/g. The method was applied for copper determination by FAAS in tap water, commercial natural spring water, commercial treated drinking water, and commercial tea bag sample. The accuracy of the method is confirmed by analyzing tea leaves (GBW 07605). The results demonstrated good agreement with the certified values.     

Cloud point extraction preconcentration of manganese(II) from natural water samples using 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone and triton X-100 and determination by flame atomic absorption spectrometry.

The possibility was investigated by using 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) as the chelating reagent for separation and preconcentration of manganese(II) by cloud point extraction (CPE) and subsequent determination by flame atomic absorption spectrometry (FAAS). The effects of experimental conditions such as pH, concentration of chelating agent and surfactant, equilibration temperature and time on cloud point extraction were studied. Under the optimum conditions, preconcentration of 10 ml of sample solution permitted the detection of 1.45 ng mL(-1) of manganese with an enrichment factor of 20. The proposed method was applied to the determination of trace manganese in water samples with satisfactory results.     

测定电解锰中微量铁的 FAAS法——采用 EDTA作释放剂

用盐酸溶解试样,加入EDTA等螯合剂作释放剂,通过改变燃烧器高度调整原子蒸气的温度以消除99．8％以上基体锰的干扰,然后用原子吸收光谱法直接测定电解锰中微量的铁,获得了满意的结果。其标准曲线法、标准加入法的结果相吻合,样品加标回收率99．8％,相对标准偏差为3．1％。方法简便快速,适于工厂的快速分析。     

Preconcentration of cobalt using Amberlyst 36 as a solid-phase extractor and its determination in various environmental samples by flame atomic absorption spectrometry

A new and simple column-solid-phase extraction method has been developed to separate and preconcentrate trace cobalt in water and soil prior to its determination by flame atomic absorption spectrometry (FAAS). Different factors such as pH of sample solution, sample volume, amount of resin, flow rate of aqueous solution, volume and concentration of eluent, and matrix effects for preconcentration were optimized. Under optimized experimentally established conditions, an analytical detection limit of 0.44?µg?L^?1, precision (RSD) of 1.9%, enrichment factor of 200, and capacity of resin of 82?mg?g^?1 were obtained. The method was applied for cobalt determination by FAAS in tap water, natural drinking water, soil, and roadside dust samples. The accuracy of the method is confirmed by analysing standard reference material (Montana Soil, SRM 2711).     

Ultra-trace determination of Pb(II) and Cd(II) in drinking water and alcoholic beverages using homogeneous liquid-liquid extraction followed by flame atomic absorption spectrometry

The determination of Pb(II) and Cd(II) in different sample matrices, including drinking water, distilled spirits and fruit wine, was carried out by flame atomic absorption spectrometry (FAAS) after pre-concentration using homogeneous liquid-liquid extraction (HLLE). First, the HLLE method was optimised with lead diethyldithiocarbamate (Pb-DDTC) complex which was extracted with a perfluorooctanoate anion (PFOA^?) dissolved in lithium hydroxide under acidic conditions. The optimum extraction conditions, using 0.01 M DDTC, 0.05 M PFOA^?, 3 M HCl and 1 mL of 30 vol. % acetone, were obtained. The Pb-DDTC complex in the nitric acid digest of the samples (50–150 mL) was extracted quantitatively into a drop of 100 μL of sediment phase. The sediment phase dissolved in 1 vol. % HNO₃ with at least 3–5 mL of the final volume was then determined by FAAS, affording a pre-concentration factor of 10–50. Hence, the HLLE method afforded an increase in both sensitivity and selectivity for the metal determination by conventional FAAS, resulting in ultra-trace level detection of Pb(II) in all samples analysed (drinking water, 9.2–23 ng mL^?1; distilled spirits, 23–50 ng mL^?1; fruit wine, 24–53 ng mL^?1). In addition, the proposed method could successfully be applied to Cd(II) determination in these samples.     

Separation of Cr(III) and Cr(VI) using melamine-formaldehyde resin and determination of both species in water by FAAS

A method is described for the determination of Cr(VI) and total chromium by FAAS. Cr(VI) is separated from Cr(III) by adsorption on melamine-formaldehyde resin. After elution of Cr(VI) with 0.1 mol/l NaAc solution, it is analysed by FAAS. Total chromium is determined by FAAS after conversion of Cr(III) to Cr(VI) by oxidation with hydrogen peroxide, total Cr(VI) is concentrated as above. If the total concentration of chromium is sufficient, the determination can be directly made by FAAS. Cr(III) can then be calculated by subtracting Cr(VI) from the total Cr. This method was successfully applied to the determination of chromium in lake water.