原子荧光光谱法测定铁矿石中砷的研究

试样经过氧化钠熔融,用水和H2SO4浸取.在H2SO4介质中,用硫脲-抗坏血酸将砷酸还原成亚砷酸,再加入KBH4使其还原成砷化氢,于原子荧光光谱仪上测定铁矿石中的微量砷.方法检出限为0.1μg/g,相对标准偏差为2.0%.加标回收率在90%～115%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中药中微量砷

1　引　　言砷是目前公认的对人体有害的微量元素 ,是制定中药质量标准和质量监测中的必测项目。常见的砷的分析方法有原子吸收法、质谱法和分光光度法等。氢化物发生 原子荧光光谱法作为测定砷的国家标准补充方法得到了广泛的应用。该法以其较高的灵敏度、较好的选择性、较小的干扰、较宽的线性范围和较快的分析速度等优点 ,得到了广泛的应用。本文在最佳条件下 ,以 1 2g L碘化钾 +1 0g L硫脲为预还原抗干扰剂 ,建立了断续流动氢化物原子荧光法测定微量砷的方法。2　实验部分2 .1　仪器与试剂　AFS 2 3 0双道原子荧光光度计 (北京海光仪…     

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     

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磷酸中的砷

采用HCl处理H3PO4试样，氢化物发生原于荧光光谱法测定As，对仪器条件、HCl酸度、预还原剂用量、还原剂用量、共存干扰进行了试验，方法的检出限为0．18ng／mL，测定精密度1．9％-3．0％，回收率为96．0％-98．0％。     

氢化物发生-原子荧光光谱法测定黄磷中微量砷

采用氢化物发生-原子荧光光谱法测定黄磷中微量砷,研究了样品消化方法以及仪器工作条件、还原剂等对测定的影响,确定了最佳试验条件.在最佳试验条件下,荧光强度与砷(Ⅲ)的质量浓度在0.06～10μg·L-1范围内呈线性关系,相关系数为0.999 4,检出限为0.03μg·L-1,样品分析结果的相对标准偏差小于3.5 %,加标回收率在93.80～103.6%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%。     

氢化物发生原子荧光光谱法测定污水中的砷

用HNO3-HClO4混合酸消解污水样,采用氢化物发生原子荧光光谱法测定污水中的砷含量。在最佳实验务件下,线性范围为0～40μg/L,检出限为0．4μg/L,测定结果的相对标准偏差小于4％,加标回收率为91．5％～100．9％。     

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。     

Effect of the Mineralization Method on Arsenic Determination in Marine Organisms by Hydride Generation Atomic Fluorescence Spectroscopy

The efficiency of several mineralization methods for As determination in marine organisms has been evaluated. Wet mineralization in closed reactors at 150°C with acids (HNO₃/HClO₄/H₂SO₄) and K₂S₂O₈ and microwave-assisted digestion with HNO₃/H₂O₂ or with HNO₃/H₂O₂/HCl does not quantitatively destroy the organic matter of fish. This was ascertained by comparing the As content obtained by HG-AFS with that obtained by ICP-MS. Dry-ashing destroys organic As species and the resulting As recovery when HG-AFS is applied is similar to that obtained by ICP-MS. Similar arsenic contents were obtained for all the mineralization methods tested when arsenic was analysed by ICP-MS. These results indicate that when HG-AFS is applied for arsenic determination, the organic matter should be completely oxidised (e.g. by UV photo-oxidation and K₂S₂O₈) to transform organic arsenic compounds into those able to generate hydrides. The results have been validated with a fish candidate reference material (CRM) (EU SEAS plaice) with a known content of total arsenic. Arsenic speciation after 1:1 methanol-water extraction (which provides quantitative arsenic recovery after two consecutive extractions) by HPLC-ICP-MS shows that cuttlefish only contains arsenobetaine, which explains the difficulty of mineralization.     

粉煤灰中微量有害元素砷的氢化物-原子荧光光谱法快速测定

采用王水分解试样 -氢化物发生原子荧光光谱法 (HG -AFS)测定粉煤灰中有害微量元素砷。方法回收率为 98 5 %～ 1 0 2 3 % ,相对标准偏差为 1 9%～ 4 8% ,该法具有快速、简便、灵敏、可测范围宽等优点 ,对探讨粉煤灰在农业土壤改良中的应用具有十分重要的意义     

氢化物发生原子荧光光谱法测定临床样品微量砷和硒

研究了氢化物原子荧光法测定临床床样品全血，血清，胎盘，头发，指甲和尿液中微量Ａｓ和Ｓｅ的方法。线性范围为Ａｓ１．３＊１０＾－９－２．５＊１０＾－７ｇ／ｍＬ，Ｓｅ２．８＊１０＾１０－７．５＊１０＾－８ｇ／ｍＬ；相对标准偏差（ｎ＝１３）Ａｓ２．６－３．６％，Ｓｅ２．８－４．２％；Ａｓ、Ｓｅ的标准加入回收率为９６．７－１０４．２％，用于６种临床样品中Ａｓ、Ｓｅ测定，获得满意的结果。     

Hydride Generation Atomic Fluorescence Spectrometric Determination of Ultratrace Arsenic in High Purity Indium Oxide

A simple, sensitive, and interference free method was proposed for the determination of total arsenic in high purity indium oxide by hydride generation atomic fluorescence spectrometry (HG-AFS). Preconcentration was carried out by distillation of volatile arsenic trichloride. Hydrazine sulfate was used as a prereductant to reduce As (V) to As (III). The volatile arsenic trichloride generation was based on the reaction between As (III) and hydrochloric acid, and vapors were absorbed with water. The method provides a linear response range of 2 ng/mL–70 ng/mL, a detection limit of 0.1 ng/mL, a recovery of 96%–113%, and an average relative standard deviation of 2.42%. The method was validated by means of interlaboratory comparative analysis with the proposed method HG-AFS, and the comparison of data by using proposed method HG-AFS and reference methods of ICP-OES and spectrophotometry.     

Advances in On-Line Hydride Generation Atomic Spectrometric Determination of Arsenic

Flow analysis has played a major role in many areas of chemical analysis, making operations more robust and precise. It facilitates experimental studies opening new areas of research. In the field of arsenic research, there are various examples of surveys concerning arsenic determination and its species with the use of flow injection analysis (FIA) and sequential injection analysis (SIA). The increasing concern over the human exposure to arsenic and its species has necessitated the development of rapid, highly sensitive, precise, and accurate analytical methods for its determination in trace levels in environmental and biological samples. This review provides a literature survey on the automatic on-line hydride generation methodologies coupled to atomic spectrometry for determination of inorganic and organic arsenic species, during the last decades. All advances in on-line manifolds are categorized and highlighted. There are several reports of manifolds and setup instrumentation concerning hydride generation including continuous flow analysis (CFA), FIA, SIA, lab-on-valve (LOV), multicommutation flow systems, and hyphenated techniques. On-line preconcentration and pretreatment methodologies coupled with hydride generation such as solid phase extraction, co-precipitation and trapping are also discussed, as they are of particular interest in the development of fully automated methods.     

HG-AFS 法测定多金属矿中的痕量锡

研究了酒石酸介质中氢化物发生原子荧光光谱法 ( HG- AFS)测定多金属矿中痕量锡的方法 ,考察了不同酸介质和浓度对氢化物发生效率的影响 ,试验了共存元素的干扰情况。方法的检出限为 1 .4× 1 0 - 10 g/ m L,精密度 ( n=5)为3.71 %～ 5.38%。     

双阳极电化学氢化物发生原子荧光光谱法测定砷

用双阳极电化学氢化物发生原子荧光光谱法测定砷,减少了化学试剂使用给环境带来的污染。在相同条件下,双阳极电化学氢化物发生效率为化学法的99.0%~101.6%。对各种实验参数和干扰情况进行了详细研究。在选定的实验条件下,100μL进样量的As(Ⅲ)线性范围为0~120μg/L;检出限为0.64μg/L(信噪比S/N=3);60μg/L的As(Ⅲ)标准溶液平行进样13次,荧光信号面积的相对标准偏差(RSD)为2.02%。用本法测得GBW07406号标准土壤样品中As含量为(205.2±1.4)μg/g与标准值(220±21)μg/g一致,仔猪饲料样品的加标回收率为97.0%~103.0%。本法灵敏度高、重现性好、结果准确。     

氢化物-原子荧光法测定粮食中的砷

研究了氢化物－原子荧光法测定粮食中砷的适宜条件,试验了酸介质和还原剂的用量对测定砷的影响,选择了仪器的最佳工作条件及氢化物发生条件,试验了生成氢化物元素及粮食中常见元素对测定的干扰情况。在测定条件下,砷的线性范围为０～８０μｇ／Ｌ,检出限为０．３μｇ／Ｌ。用该法测定了标准物质小麦粉及大米,结果与推荐值吻合。方法快速、准确,应用于进口粮食中砷的检测,获得满意结果     

碱式模式氢化物发生原子荧光法测定食用菌中痕量锗

研究了碱式模式氢化物发生原子荧光法测定痕量锗。考察了HG－AFS仪器参数及氢化物发生条件对锗荧光强度的影响以及常见共存元素的干扰。在选定的最佳工作条件下,测定了真菌中的痕量锗。方法检出限（3σ）为0.76μg/L,相对标准偏差(RSD)为0.81％,回收率为94.6％－101.3％。     

氢化物发生－缝管原子捕集－原子吸收法测定钢铁和地质试样中的砷

介绍简易的氢化物发生原子吸收测砷的方法。喷雾器负压将ＫＢＨ_４吸入反应器，并将生成的ＡｓＨ_３吸入乙炔－空气焰原子化。石英缝管使灵敏度提高３．５倍。方法的检测限（３σ）为１．８ｎｇ／ｍＬ（５ｍＬ试样）。２０ｎｇ／ｍＬＡｓ（Ⅲ）标准液１０次测定的ＲＳＤ为３．８％。本法成功地应用于钢铁和地质标样中微量砷的测定。