湿法消解/干灰化-氢化物发生-原子荧光光谱法测定基围虾中总砷

建立了一种采用湿法消解/干灰化-氢化物发生-原子荧光光谱法测定基围虾中总砷的方法。样品中加入6mL硝酸,冷消解120min,电热板160℃预消解至澄清,并赶酸至约1mL,加入灰化辅助剂硝酸镁,550℃马弗炉灰化5min。盐酸溶解灰分,采用氢化物发生-原子荧光光谱法测定。通过优化仪器条件,砷含量在0.0～20.0μg/L范围内,标准曲线线性相关系数优于0.999,检出限为0.025μg/L,相对标准偏差(RSD)为2.5%～3.1%,加标回收率为93.6%～103%。方法结果准确,可用于基围虾中总砷测定。     

微波消解-氢化物发生-原子荧光光谱法测定中药材中痕量砷

采用微波消解法用硝酸-过氧化氢(3+1)溶液消解样品,以硫脲及抗坏血酸混合溶液作为预还原剂,利用氢化物发生-原子荧光光谱法测定中药材当归、丹参、甘草、三七和黄芪中痕量砷的含量。在盐酸(3+97)溶液中加入溶于20g.L-1氢氧化钾溶液中的10g.L-1硼氢化钾溶液使与溶液中砷离子反应生成氢化物。分析中采用载气流量为800mL.min-1。砷的质量浓度在12μg.L-1以内与其对应的荧光强度呈线性关系,方法的检出限(3s/k)为0.020μg.L-1。应用此法对国家标准物质人发(GBW 09101)进行分析,测定值与认定值一致。     

氢化物发生-原子荧光光谱法测定海产品中总砷

采用氢化物发生-原子荧光光谱法测定海产品中总砷的含量。样品经硝酸-高氯酸(4+1)混合酸消解,样品溶液中加入硫脲和抗坏血酸混合溶液作为预还原剂。于盐酸(5+95)溶液中加入10g.L-1硼氢化钾-5g.L-1氢氧化钾溶液使与溶液中砷离子反应生成氢化物。分析时采用载气流量为400mL.min-1,屏蔽气流量为800mL.min-1。砷的质量浓度在20μg.L-1以内与荧光强度呈线性关系,方法的检出限(3s/k)为0.015μg.L-1。应用此法对3种海产品进行分析,测定值的相对标准偏差(n=6)在3.4%～4.2%之间,回收率在98.5%～101.0%之间。     

氢化物发生-原子荧光光谱法测定土壤中砷

采用氢化物发生-原子荧光光谱法测定土壤中砷的含量.样品经硝酸-盐酸(1+1)混合酸于沸水浴中加热1 h消解.对测定的影响因素:仪器的负高压、灯电流、载气和屏蔽气流量;硼氢化钾的浓度、酸的种类及其浓度、共存离子的干扰等试验条件作了研究并予以优化.荧光强度与砷的质量浓度在100 μg·L-1以内呈线性关系,方法的检出限(3s/b)为0.6 μg·L-1,方法的相对标准偏差(n=6)小于5%.应用此法对标准物质ESS-1和土壤样品进行分析,测得砷的回收率在93%～105%之间.     

氢化物发生-原子荧光光谱法测定鹿茸中的总砷

研究了氢化物发生-原子荧光光谱法测定鹿茸中总砷的分析方法。采HNO3-HCl O4混合酸(V:V=8:1)消解样品,以2%HCl介质作为载流,样品酸度控制在10%时进行样品分析。方法的线性范围0~10μg/L,相关系数优于0.999,检出限0.04μg/L,相对标准偏差3.2%,加标回收率96.0%~102.0%。     

氢化物发生-原子荧光光谱法测定茶水中砷

采用氢化物发生-原子荧光光谱法测定茶水中砷含量。样品经硝酸-高氯酸(4+1)混合酸消解,在盐酸(6+94)溶液中加入30 g·L-1硼氢化钾-5 g·L-1氢氧化钾溶液使与溶液中砷离子反应生成氢化物。分析中采用载气流量为400 mL·min-1。试样溶液中加入硫脲及抗坏血酸混合溶液作为预还原剂。引入仪器的进取样量为1.2 mL,按选定的工作条件操作。荧光强度与砷的质量浓度在0.20~100μg·L-1范围内呈线性关系,方法的检出限(3s/k)为0.030μg·L-1。应用此法对3种茶叶泡出的茶水进行分析,测得回收率在97.7%~101.5%之间。     

氢化物发生-原子荧光光谱法测定草酸钴中痕量砷

报道了采用氢化物发生-原子荧光光谱(HG-AFS)法测定草酸钴中痕量砷。考察了不同酸介质及其浓度对氢化物发生效率的影响,以及钴基体和其它共存元素的干扰情况。方法的检出限为0.097μg/L,精密度在2.3%~7.9%之间,加标回收率为94.0%~100.9%。     

中成药中微量砷和汞的微波消解-氢化物发生-原子荧光光谱法测定

介绍了一种用于测定中成药中微量砷（As)和汞（Ag)元素的方法－微波消解－氢化物发生－原子荧光光谱法。讨论了仪器的工作参数、实验条件、共存元素对分析结果的干扰;同时,通过加标回收试验,对该法进行了验证。实验结果表明,该法具有快速、简便、准确等特点,适用于实验室常规分析。     

氢化物发生-原子荧光光谱法测定低合金钢中微量砷

采用氢化物发生-原子荧光光谱法测定低合金钢中砷的含量。样品经盐酸-硝酸混合酸消解,以盐酸(5+95)溶液为反应介质,15g·L~(-1)硼氢化钾-2g·L~(-1)氢氧化钾的混合溶液为还原剂,采用柠檬酸作为掩蔽剂。砷的质量浓度在60.0μg·L~(-1)以内与荧光强度呈线性关系,方法的检出限(3s/k)为0.023μg·L~(-1)。应用此法对标准钢样进行了分析,测定结果与认定值相符合,可满足钢铁中微量砷(质量分数0.001%～0.04%)的测定要求。     

氢化物发生-原子荧光光谱法测定罐头食品中微量砷

研究了氢化物发生 原子荧光光谱法对微量砷的测定 ,方法灵敏度高 ,准确度好。在最佳条件下 ,荧光强度与砷浓度在 4× 10 - 4～ 0 .2 1μg·ml- 1范围内呈线性关系 ,检出限达 1× 10 - 4μg·ml- 1。用此法测定了罐头食品中微量砷 ,结果满意     

Determination of total arsenic in seawater by hydride generation atomic fluorescence spectrometry

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.     

Determination of arsenic in dinosaur skeleton fossils by hydride generation atomic fluorescence spectrometry

Hydride generation atomic fluorescence spectrometry was for the first time utilized to determine trace toxic element arsenic in the skeleton fossils of four dinosaurs unearthed in Sichuan Province of China. The instrumental limit of detection (LOD) for arsenic was 0.03 μg/L under optimal experimental conditions, which compared favorably to that by ICP-AES and ETAAS. The samples were digested with aqua regia in boiling water bath. The recoveries of standard addition were found to be from 97 to 109%, and the analytical results were found in good agreement with those by ICP-AES. It is a simple, reliable, sensitive yet relatively inexpensive analytical method, compared to ICP-AES, ICP-MS or ETAAS. Interesting analytical results were found that the arsenic concentrations were all abnormally high in the skeleton fossils. The established analytical method and the analytical results may be helpful in revealing the mystery of the mass extinction of the dinosaur fauna. The analytical results, together with other data available to date, supported the argument that the arsenic toxicosis could be a contributing factor for the mass extinction of the dinosaur fauna in Sichuan Province of China.     

氢化物-原子荧光光谱法测定大气沉降物中砷含量

大气沉降物中砷的测定传统方法干扰多,本文针对大气沉降物样品的复杂性,在样品中加入盐酸、硝酸、高氯酸于电热板上加热消解,能有效的消除大量有机质对测量结果的干扰,为大气沉降物研究工作提供更为精准的检测数据。该方法能有效的消除基体干扰,分析成本低,测定的精密度高、准确性好,相对标准偏差(RSD)低于2.0%,样品加标回收率高于90%。     

微波辅助消解-原子荧光法测定玻璃中的镉砷铅

光学玻璃中的各种元素对玻璃的光学性能有不同的影响。如加入镉可以提高玻璃折射率;砷的引入能增加玻璃的透光度,含铅玻璃具有低成本、高折射性等优点。但是镉、砷、铅均为有毒元素,玻璃加工和处理过程以及毒废弃物的处理都可能引起水、土壤、大气的污染并给人体带来一定的危害     

Determination of arsenic and antimony in milk by hydride generation atomic fluorescence spectrometry

A highly sensitive procedure has been developed for total arsenic and antimony determination in milk samples by hydride generation atomic fluorescence spectrometry after microwave-assisted sample digestion. The discrete introduction of 2 ml of digested sample in the automated continuous flow hydride generation system allows us to reduce drastically the sample and HCl consume and to determine several elements from a same sample digestion. The method provides detection limits of 0.006 and 0.003 ng ml⁻¹, a sensitivity of 2390 and 2840 fluorescence units per ng ml⁻¹ for As and Sb respectively, and average relative standard deviation of 2.3% for As and 4.8% for Sb. The analysis of cow milk samples, obtained from the Spanish market evidenced the presence of As at concentration levels from 3.4 to 11.6 ng g⁻¹ and Sb levels from 3.5 to 11.9 ng g⁻¹, thus in a proportion near to 1:1, which is in contrast with the 10:1 natural ratio between As and Sb and could evidence the effect of the introduction of new alloys and polymer materials in the industrial process of milk. The method was validated by the comparison of data found for commercial samples by using the proposed procedure and reference methods based on dry-ashing and AFS, and microwave-assisted digestion and inductively coupled plasma mass spectrometry determination.     

原子荧光光谱法测定以磷块岩为原料制备磷酸中的砷

本文利用以水作载流的氢化物发生-原子荧光光谱仪测定了以磷块岩为原料自制的磷酸中的砷（As）。利用硫酸法溶融磷块岩自制出磷酸,优化仪器的工作条件,通过条件实验选择出适用于测定砷所需的盐酸和5% L（+）-抗坏血酸-5% 硫脲的用量。原子荧光光谱法测定结果如下：在0.5 ng·mL-1 ~ 8.0 ng·mL-1浓度范围内线性相关系数R2=0.99996;检出限为0.0018 ng·mL-1,样品的相对标准偏差（RSD）为0.82 %,样品的加标回收率在92.4 % ~ 103.4 %。通过与电感耦合等离子体发射光谱法（ICP-OES）比对,结果一致。     

Open digestion under reflux for the determination of total arsenic in seafood by inductively coupled plasma atomic emission spectrometry with hydride generation

A method for the determination of arsenic (As) in seafood by inductively coupled plasma atomic emission spectrometry with continuous hydride generation is described. Several analytical parameters have been investigated and optimised. The analytical features of the method (recovery, precision, accuracy and limit of detection) were calculated. Practical detection limit of 3.6 μg/kg fresh weight for As has been reached. The precision of the method expressed as relative standard deviation (R.S.D.) was in the range of 2.7-3.7% and the recovery percentage ranged from 98.4 to 101.8%. The reliability of the developed method was checked by analysing several certified reference materials. A complete mineralization was obtained for arsenobetaine (AsB) containing reference material with a mixture of nitric and sulphuric acids followed by adding hydrogen peroxide in an open digestion system. This method can be applied to routine analysis without any risks of interferences.     

石墨消解-原子荧光光谱法测定土壤中的总硒

为准确定量土壤硒总量,提出以逆王水(1+1)-石墨消解法消解土壤,氢化物原子荧光光谱法(HG-AFS)测定土壤总硒含量的方法.其中,对消解方式、消解时间和仪器条件进行了探讨,确定最优检测条件.称取0.2 g土壤样品加入5 mL逆王水(1+1),于石墨消解仪120℃消解1.5 h,冷却至室温后用超纯水定容至25 m L,...     

Non-chromatographic speciation analysis of arsenic and antimony in milk hydride generation atomic fluorescence spectrometry

A rapid, high sensitivity method has been developed for the determination of As(III), As(V), Sb(III) and Sb(V) in milk samples by using hydride generation atomic fluorescence spectrometry. The method is based on the leaching of As and Sb from milk through the sonication of samples with aqua regia followed by direct determination of the corresponding hydrides both before and after reduction with KI. It was confirmed by recovery experiments on spiked commercially available samples that neither the reduced nor the oxidized forms of the elements under study or mixtures of the two oxidation states were modified by the room temperature sample treatment with aqua regia. The methodologies developed provided 3σ limit of detection values of 8.1, 10.3, 5.4 and 7.7 ng l⁻¹ for As(III), As(V), Sb(III) and Sb(V) in the diluted samples. Average relative standard deviation values of 5.7, 5.5, 8.2 and 4.7% were found for determination of As(III), As(V), Sb(III) and Sb(V) in commercially available samples of different composition and origin containing from 3.5 to 13.6 ng g⁻¹ total As and from 4.9 to 11.8 ng g⁻¹ total Sb, it being confirmed that As(V) and Sb(V) are the main species present in the samples analyzed (62±5 and 73±5%, respectively). The time required to determine As and Sb species in milk involves 10 min sonication and 30 min prereduction but these steps can be carried out for several sample simultaneously. Additionally the fluorescence measurement step involves less than 20 min for three replicates of all the four measurements required. So, in less than 2 h it is possible to determine the content of As(III), As(V), Sb(III) and Sb(V) in four samples.     

断续流动-氢化物发生-原子荧光光谱法测定木材中砷含量

采用断续流动进样氢化物发生，原子荧光光谱法测定木材中砷含量，确定了仪器的最佳工作条件，考察了酸度、预还原剂和还原剂用量和栽流流速的影响以及共存元素的干扰情况。在选定的测定条件下，砷的检出限为0．5μg／L，相对标准偏差为1．7％，回收率为95．8％～102．0％。