Determination of Arsenic and Mercury in Soil by Microwave Digestion and Hidride GenerationAtomic Fluorescence Spectrometry

[Objective] The aim was to develop a rapid, simple method for determina- tion of arsenic and mercury in soil samples by atomic fluorescence spectrometry. [Method] The method for determination of As and Hg in soil by combined atomic fluorescence spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-80.0μg/L of As and 0-8.0 μg/L of Hg, and the detection limits of As and Hg was 0.036 μg/L and 0.015 μg/L, respectively. The precision for elevenfold determination of As at 40.0 ug/L level and Hg at 4.0μg/L level were 1.1% and 2.2%（RSD）, respectively. Recoveries of 103.0%-106.6% for As and 90.0%-95.0% for Hg were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of As and Hg in soil samples.

Determination of arsenic in grain and soil by hydride nondispersive atomic fluorescence method

Quantity of trace arsenic in grain and soil was determined by hydride nondispersive atomic fluorescence method.Optimum conditions of measurement were selected in the experiment including the pH of the medium, reductive agent, the concentration and flowing velocity of KBH4, rate of carrier gas and atomized temperature. The reference sample of rice C was determined and the linear relationship of the calibration curve was plotted, indicating that the method was highly precise. In the experiment of recovery rate, the method was quite satisfactory.Based on the determination of hundreds of samples, it is proved that atomic fluorescence method is rapid, sensitive and low in interference. It is very efficient on determination of trace arsenic in soils and grains, especially in grains.

Speciation Analysis of Arsenic Compounds in Seafood by Ion Chromatography-Atomic Fluorescence Spectrometry

Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L^(-1) CH_3COONH_4 and 15 mmol L^(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L^(-1) for As B, 0.4261 μg L^(-1) for As(III), 0.216 μg L^(-1) for DMA, 0.211 μg L^(-1) for MMA, and 0.709 μg L^(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.

Influencing Factors of Determination of Total Arsenic in Soil by Atomic Fluorescence(AFS-9760) Method

In this paper,the atomic fluorescence(AFS-9760)method used for the determination of total arsenic in soil was verified based on three national quality control samples GSS-8,GSS-25,and GSF-3.Under the conditions of negative pressure of 270 V,carrier gas flow of 300 m L/min,and shield flow of 1000 m L/min,the detection limit of the method was 0.0092 mg/kg;the precision of GSS-8,GSS-25,and GSF-3 was 3.96%,1.47%and 1.08%,and the accuracy was 3.07%,2.13%,2.93%respectively.In addition,the matters needing attention during this experiment,such as reagent factor,instrument conditions,calibration curve,etc.,were summarized.It provides certain reference for the determination of total arsenic content in soil by atomic fluorescence spectrometry.

Study on Atomic Fluorescence Spectrometry Excited by Synchrotron Radiation

A novel analysis approach using atomic fluorescence excited by synchrotron radiation is presented. A system for synchrotron radiation-atomic fluorescence spectrometry is developed, and experimental conditions such as flow rate, analyte acidity, concentration of pre-reducing and hydrogenation system are optimized. The proposed method is successfully applied to get an excitation spectrum of arsenic. Seven of ten primary spectral lines, four of which have never been reported by means of atomic fluorescence spectrometry, agree well with the existing reports. The other three are proposed for the first time. Excitation potentials and possible transitions are investigated. Especially for the prominent line at 234.99 nm, the mechanism of generation is discussed and a model of energy transition processes is proposed.

Synthesis of a Novel Imidazole Ionic Liquid Modified Mesoporous Silica SBA15 for Selective Separation and Determination of Inorganic Arsenic in Rice

A novel 1-methylimidazole ionic liquid modified SBA15 mesoporous silica(1-MIIL@SBA15) was synthesized and applied to selective separation of inorganic arsenic(iAs) in rice by dispersive solid phase extraction(DSPE), followed by hydride generation-atomic fluorescence spectrometric(HG-AFS) quantification. The prepared sorbent was characterized by FTIR, FESEM, BET and Zeta potential. Key parameters of adsorption and desorption in DSPE were optimized using standard reference material 1568 b rice flour. Under optimal conditions, the limit of detection was 8.776 ng/kg, relative standard deviation was ≤2.0%, and recoveries of iAs were in the 92.3～94.4% range. This method was successfully applied to the determination of iAs in rice. Under acidic condition, the electrostatic interaction between the positively charged 1-MIIL@SBA15 and anionic iAs played an important role in selective iAs separation, rendering this method suitable for iAs analysis.

Mechanism research on arsenic removal from arsenopyrite ore during a sintering process

The mechanism of arsenic removal during a sintering process was investigated through experiments with a sintering pot and arsenic-bearing iron ore containing arsenopyrite; the corresponding chemical properties of the sinter were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES), X-ray diffraction (XRD), and scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS). The experimental results revealed that the reaction of arsenic removal is mainly related to the oxygen atmosphere and temperature. During the sintering process, arsenic could be removed in the ignition layer, the sinter layer, and the combustion zone. A portion of FeAsS reacted with excess oxygen to generate FeAsO4, and the rest of the FeAsS reacted with oxygen to generate As2O3(g) and SO2(g). A portion of As2O3(g) mixed with Al2O3or CaO, which resulted in the formation of arsenates such as AlAsO4and Ca3(AsO4)2, leading to arsenic residues in sintering products. The FeAsS component in the blending ore was difficult to decompose in the preliminary heating zone, the dry zone, or the bottom layer because of the relatively low temperatures; however, As2O3(g) that originated from the high-temperature zone could react with metal oxides, resulting in the formation of arsenate residues. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.

水浴消解-原子荧光法测定糖厂滤泥中的总砷和总汞

建立了采用水浴消解-原子荧光光度法测定糖厂滤泥中总砷和总汞含量的方法。试验结果表明,在最佳测试条件下,糖厂滤泥样品中总砷、总汞的线性浓度范围分别为0~100μg/L、0~2.00μg/L;总砷、总汞的检出限分别为0.012 mg/kg、0.001 mg/kg;精密度试验(n=9)总砷、总汞的相对标准偏差(RSD)分别为2.4%、3.8%;回收试验总砷、总汞的回收率分别为98.8%~107.9%、98.5%~107.2%。该方法准确度高,其精密度、检出限、回收率均能满足检测的要求,可为广西糖厂滤泥中总砷和总汞的含量测定及安全性评价提供参考。

内部质控样芹菜中总砷含量的不确定度评定

《检验检测机构资质认定能力评价检验检测机构通用要求》(RB/T 214—2017)4.5.15中鼓励检验检测机构在检验检测出现临界值、内部质量控制或客户有要求时,报告测量不确定度。按《食品安全国家标准食品中总砷及无机砷的测定》(GB 5009.11—2014)第二法原子荧光光谱法测定内部质控样芹菜中的总砷,并对其进行测量不确定度评定。结果显示芹菜中总砷的含量为0.516 mg·kg^(-1),其扩展不确定度为0.046 mg·kg^(-1),证书提供的标准差为0.021 mg·kg^(-1),换算成Z比分数,|Z|=0.33,测试结果满意。

西藏羊八井高温地热水砷和氟浓度及来源探析

砷(As)和氟(F)是西藏羊八井高温地热流体中两种典型的高浓度有害元素,通过地热开发可以进一步促进与加速地热源As和F向地表或近地表环境释放,导致地表水和土壤环境污染。如何从As和F浓度分布特征联系水化学特征从而揭示水体As和F的富集规律,对丰富和认识西藏地区水环境中As和F的环境地球化学行为具有重要意义。本文结合野外调查现场测定了水体常规理化指标,包括水温、pH值、电导率(EC)、总溶解固体(TDS)和盐度(SAL),采用原子荧光光谱法和X射线荧光光谱法分别测定水体和土壤样品中的As浓度,离子选择性电极法测定水体和土壤样品中的F浓度,评价As和F超标风险,探析其富集机制。结果表明:水化学类型为Na-HCO_(3)∙Cl型,水体Na+浓度高达445.5mg/L,Ca^(2+)浓度低至3.31mg/L,水体pH在7.87~9.42之间,富钠贫钙高pH是羊八井地热水和温泉水最主要的水化学特征。受水汽蒸发浓缩影响,温泉水As和F浓度高于地热水,两元素浓度最高分别达6.50mg/L和17.89mg/L。地热废水的不当处理存在水体和土壤As和F暴露风险,地热水和温泉水As和F浓度显著高于《地热资源评价方法》(DZ40—85)对有害成分规定的最高允许排放浓度(总砷为0.50mg/L,氟化物为10mg/L)。而土壤中总As浓度为79.50~99.08mg/kg,F浓度为1162.70~1285.10mg/kg,显著高于西藏土壤背景值。地热水体和地表土壤As和F富集主要为水-岩浸溶相互作用,独特的水化学特征为水体As和F浸取溶出提供了有利条件。

原子荧光光谱法测定硫化钠溶液中的砷

砷元素作为镍电解系统溶液中重要的控制指标之一,其含量的高低影响镍板的品级率。通常在镍系统净化的除铜工序中加入大量硫化钠溶液作为沉淀剂,除去溶液中的铜,为避免硫化钠溶液引入过量的砷,需要对硫化钠溶液中砷含量进行分析。文章以碘单质为氧化剂,氧化硫化钠溶液中的二价硫离子,形成硫单质,过滤除去沉淀,建立了原子荧光法测定硫化钠溶液中砷的分析方法。文章进行了碘离子、碘单质、钠离子对砷测定的影响试验,确定了碘、盐酸、硫脲-抗坏血酸混合溶液的用量,以盐酸作载液、硼氢化钾作还原剂,采用原子荧光光谱法测定样品中砷含量。工作曲线线性范围在0~50μg/L时,相关系数可达到0.9995以上,相对标准偏差在6.55%~8.25%之间,加标回收率在85.0%~109.0%之间,满足分析要求。

氢化物发生-非色散原子荧光光谱法测定粉饼化妆品中Pb,As和Hg含量

建立并优化了氢化物发生-非色散原子荧光光谱法(HG-NDAFS)测定10种粉饼化妆品中铅(Pb),砷(As)和汞(Hg)的含量。确定了较佳载气流速为400 mL/min,屏蔽气流速为800 mL/min。优化了负高压和灯电流,确定了原子化器高度为8 mm。优化还原剂体系时,选择了质量分数1.5%KBH4溶液。载流选择2.4 mol/L HCl。结果显示,Pb,As,Hg的加标回收率分别为83.44%~90.32%,83.22%~86.59%,81.43%~89.94%,加标回收率良好。10种粉饼中共检出2种粉饼中含有Pb(含量0.48和0.27 mg/kg),1种粉饼中含有As(含量0.62 mg/kg),1种粉饼中含有Hg(含量0.11 mg/kg)。10种粉饼中的Pb,As,Hg含量均未超标。本研究建立的HG-NDAFS测定粉饼化妆品中Pb,As和Hg含量的方法准确度高,可用于粉饼化妆品中Pb,As和Hg含量的检测。

原子荧光光谱法测定砷过程中还原反应条件的优化

自然界中砷和砷的化合物一般可通过水、大气和食物等途径进入人体,危害人体健康,原子荧光光谱法测定砷含量被广泛应用。为准确测定样品中砷的含量,以原子荧光光谱法(AFS)测定土壤中总砷含量为例,重点研究高价态砷(Ⅴ)还原为低价态砷(Ⅲ)的实验条件,采用正交实验进行条件优化,建立适合的实验方法。通过设计L_(9)(3^(4))正交实验,高价态砷的还原反应与四个因素有关,即与反应温度、反应时间、盐酸加入量和硫脲的用量呈一定的正相关,结果表明,四个因素中硫脲用量的影响最为显著,其次是盐酸加入量、反应时间和反应温度。通过对四个因素的多水平检验,优化后的实验条件为:硫脲用量2.0 mL、盐酸加入量10%、反应时间20 min、温度20~35℃(即普通室温)。采用土壤标准物质验证优化后条件的可行性,得出砷的测定值在标准值范围内,RSD在2.2%~4.2%,精密度和准确性均满足质控要求。优化后的实验条件使得操作简便易行,提高了工作效率。

4种前处理方法-原子荧光光谱法测定螺旋藻中总砷含量

本文使用原子荧光光谱法,比较了干法、低温湿法、高温湿法和微波消解法4种前处理方法测定螺旋藻中的总砷含量。通过考查正确性、精密度以及回收率3个指标确定了高温湿法为最佳前处理方法,同时通过双人比对和仪器比对验证了该法具有良好的重复性,说明高温湿法-原子荧光光谱法是一种有效的测定螺旋藻总砷含量的方法。

原子荧光光谱法检测食用鱼中汞、砷含量

目的:建立原子荧光光谱法同时测定食用鱼中汞、砷含量的方法。方法:采用微波消解法对样品进行预处理,原子荧光光谱法同时测定食用鱼(淡水鱼、海水鱼)中汞、砷含量,分析其检测结果。结果:汞在0~10.0μg·mL^(-1)时线性关系良好,砷在0~40.0μg·mL^(-1)时线性关系良好,相关系数> 0.999。汞的检出限在2.50~3.83μg·mL^(-1),回收率为94.1%~99.0%,精密度为2.9%;砷的检出限在2.30~3.68μg·mL^(-1),回收率为93.3%~99.2%,精密度为2.0%。对比发现食用海水鱼中汞、砷含量显著高于淡水鱼(P <0.05)。结论:原子荧光光谱法操作简单、检测灵敏度较高,可同时测定食用鱼汞、砷含量。

两种湿消解法消解-原子荧光法测定尿中总砷

目的比较硝酸、硫酸、高氯酸混酸与过硫酸铵两种消解法-原子荧光测定尿中总砷的方法。方法前处理分别用硝酸、高氯酸、硫酸混酸在310℃下对尿样消解1 h后加硫脲-抗坏血酸还原样品和用饱和过硫酸铵溶液在310℃下对尿样消解1 h后加入硫脲-抗坏血酸还原,进入原子荧光仪检测。结果在1.00~20.00μg/L砷含量范围内,标准曲线回归方程:y=106.587 x-11.979,相关系数优于0.9990,混酸消解法的精密度2.06%~3.03%,平均加标回收率101.2%~104.3%,检出限0.012μg/L;饱和过硫酸铵消解法的精密度3.31%~4.05%,平均加标回收率97.9%~101.6%,检出限0.006μg/L。结论两种方法的准确度、精密度均符合卫生标准《尿中砷的测定氢化物发生原子荧光法》(WS/T 474-2015)的要求,适于大批量尿中总砷含量的检测。

原子荧光光谱法测定三苯基膦羰基铑催化剂中的砷含量

采用原子荧光光谱法测定三苯基膦羰基铑催化剂中的砷含量,考察了消解酸的种类和用量、共存元素铑的干扰及消除方法,验证了测定方法的准确度和精密度。实验结果表明,在5.0 mL硝酸+2.0 mL高氯酸的混合酸体系中,催化剂可消解完全,采用共沉淀的方法,pH在9~10时,可完全消除铑对砷含量测定的影响。当砷含量在1.0~10.0μg/L范围内时,砷含量与荧光强度的关系曲线呈线性,相关系数大于0.999。测定结果的相对标准偏差小于5%,加标回收率在92%~106%之间,满足分析测试要求。

84%王铜水分散粒剂中镉、铅、砷分析方法研究

本文采用原子吸收分光光度法和原子荧光光谱法,测定84%王铜水分散粒剂中镉、铅、砷的含量。以空气—乙炔火焰原子吸收分光光度法,于228.8 nm波长处,测定镉含量,于283.3 nm波长处测定铅含量;以氩气—砷空心阴极灯原子荧光光谱法测定砷含量。结果表明,该分析方法的线性相关系数分别为0.99482、0.99986、0.99737,标准偏差为0.039、0.18、0.0052,变异系数为5.3%、5.6%、3.2%,平均回收率分别为98.2%、94.5%、101.9%。该方法简便快捷,灵敏度、精密度和准确度高,适用于镉、铅、砷的定量分析。

原子荧光光谱法测定五氧化二磷中的砷

研究了采用原子荧光光谱法测定五氧化二磷中的砷,确定了酸介质、酸度、还原剂浓度、预还原剂和掩蔽剂。结果表明:方法在1.0~50.0μg/L范围内线性良好,相关系数r>0.999,检出限为0.064μg/L,定量限为0.21μg/L;8次样品分析结果的相对标准偏差(RSD)为1.94%,加标回收率为92.87%~101.30%,检验结果与DDTC银盐法无明显差异。该法操作更便捷,所用试剂少,是一种测定五氧化二磷中砷含量的可靠方法。

水浴密封消解-原子荧光法测定土壤中的汞和砷

建立水浴密封消解-原子荧光法测定土壤中的汞和砷。采用一次性聚丙烯离心管、恒温水浴振荡器为消解设备,取样质量为0.3~0.5 g,以5 mL王水溶液(1∶1)为消解液,消解时间为1 h。汞、砷的质量浓度分别在0~2、0~20μg/L范围内与荧光强度线性关系良好,相关系数分别为0.999 7、0.999 8,汞和砷的检出限分别为0.001、0.01 mg/kg,定量限分别为0.004、0.04 mg/kg。采用该方法对土壤成分分析标准物质GSS-8、GSS-23、GSS-29进行测定,汞和砷测定结果的相对标准偏差分别为3.5%~6.6%、1.8%~3.8%(n=6),相对误差分别为-3.3%~4.9%、-2.1%~2.5%。汞和砷的回收率分别为93.7%~104%、98.6%~102%。该方法采用一次性聚丙烯离心管,无需消清洗解管,消解过程简单,消解液用量少,适用于大批量土壤样品测定。