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1.
甲基异丁基甲酮萃取－石墨炉平台原子吸收法测定地质样品中痕量硒和碲 总被引：1，自引：1，他引：1
样品经ＨＮＯ＿３－ＨＦ－ＨＣｌＯ＿４分解，在５．４ｍｏｌ／Ｌ的ＨＣｌ介质中，以抗坏血酸为还原剂用甲基异丁基甲酮同时萃取样品中的Ｓｅ、Ｔｅ。以Ｐｄ和Ｎｉ作混合基体改进剂，使用自制的涂锆石墨平台直接测定有机相中的Ｓｅ、Ｔｅ。方法的检出限分别为０．２１×１０￣（－９）ｇＳｅ，０．１３×１０￣（－９）ｇＴｅ；测定０．０６ｇＳｅ、０．０３ｇＴｅ的ＲＳＤ（ｎ＝１１）分别为７．０％和８．９％。 相似文献
2.
氢化物—原子荧光法测定岩石中痕量硒的干扰及消除 总被引：12，自引：10，他引：12
用ＨＦ－ＨＣｌＯ４－ＨＮＯ３混合酸分解样品，采用Ｆｅ＾３＋作释放剂，研究了不同量的Ｆｅ＾３＋与ＨＣｌ酸度对Ｓｅ荧光强度的影响和干扰离子消除的效果，以及Ｆｅ＾３＋存在Ｔｅ存在下对Ｓｅ测定的影响。方法的检出限为０．０１μｇ／ｇ．样品中Ｓｅ量为０．１μｇ／ｇ的相对标准偏差（ｎ＝１１）是５．４％。用于岩石标样中痕量Ｓｅ的测定，结果较好。 相似文献
3.
样品经ＨＮＯ３－ＨＦ－ＨＣＬＯ４分解发，在５．４ｍｏｌ／Ｌ的ＨＣｌ介质中，以抗坏血酸为还原剂用甲基异丁基甲酮同时萃取样品中的Ｓｅ，Ｔｅ．ｃ Ｐｄ和Ｎｉ作混合基体改进剂，使用自制的涂锆石墨平台直接测定有机相中的Ｓｅ，Ｔｅ。方法的检出限分别为０．２１×１０＾－９ｇＳｅ，０．１３×１０＾－９ｇＴｅ；测定０．０６μｇＳＥ、０．０３μｇＴｅ的ＲＳＤ（ｎ＝１１）分别为７．０％和８．９％。 相似文献
4.
流动注射—原子荧光法测定岩矿中痕量硒和碲 总被引：9，自引：2，他引：9
讨论了题示方法中的干扰，指出在一般岩石中多数共存元素不干扰Ｓｅ和Ｔ有的测定；Ｃｕ的干扰可在含Ｆｅ＾３＋，ＨＣｌＯ４的介质中加入邻菲罗啉沉淀预先消除；Ｐｂ的干扰可在Ｈ２ＳＯ４分解试样时形成ＰｂＳＯ４消除；试液保存在塑料容器中可免除残留Ｆ＾－的影响。 相似文献
5.
基性岩超基性岩中痕量铂的催化极谱测定 总被引：1，自引：0，他引：1
本文针对基性岩超基性岩中ＳｉＯ＿２，Ａｌ＿２Ｏ＿３，Ｆｅ＿２Ｏ＿３，ＭｇＯ，ＣａＯ等含量高的特点，确定了１ｍｏｌ／Ｌ盐酸—０．１ｇ／Ｌ硫酸肼—３×１０￣（－３）ｍｏｌ／Ｌ甲醛底液测定痕量铂的体系，通过控制温度与改进熔矿方法，增强了体系稳定性，消除了ＳｉＯ＿２等的干扰。用于铜镍矿、铬铁矿和硅酸盐管理样的测定，结果符合要求。 相似文献
6.
催化动力学光度法测定痕量铁的研究 总被引：2，自引：0，他引：2
研究了在ｐＨ８．５的Ｎａ２Ｂ４Ｏ７－ＨＣｌ介质中,Ｆｅ＾３＋催化Ｈ２Ｏ２氧化茜素红褪色,建立了动力学光度法测定痕量Ｆｅ＾３＋的方法。方法检出限０．０４３μｇ／ｍｌ,线性范围０￣０．１７μｇ／ｍｌ,除Ｍｎ＾２＋、Ｃｏ＾２＋等离子外,其余共存离子基本无干扰,实测了天然水和化学试剂中痕量Ｆｅ＾３＋,结果满意。 相似文献
7.
本义采用氢化物法分离技术，使样品溶液中的锗转变为气态氢化锗（ＧｅＨ＿４），达到与基体分离的目的，有效地消除了各种离子的干扰。研究并证明了在１５％以上的磷酸介质中，各种酸（ＨＣｌ，Ｈ＿２ＳＯ＿４，ＨＮＯ＿３，ＨＣＩＯ＿４）度在１％－１０％的范围内变化均不影响锗的测定，大大简化了操作手续，方法灵敏度高、使用范围广、准确、简便、快速。Ｇｅ的检出限为０．１μｇ／ｇ，相对标准偏差＜７％。可应用于地质，冶金，生物，环保，卫生，食品中微量锗的测定。 相似文献
8.
对Ｐ５０７萃淋树脂分离稀土元素的条件进行了实验，拟定了以Ｐ５０７萃淋树脂为固定相，ＨＣｌ为流动相分离４Ｎ级荧光材料Ｅｕ＿２Ｏ＿３中１４种稀土杂质元素的流程，使被测杂质与基体Ｅｕ＿２Ｏ＿３达到了较好的分离；再用阳离子交换树脂分离被测液中非稀土杂质元素。选择了端视ＩＣＰ－ＡＥＳ测量稀土杂质元素的最佳条件。称样量５０ｍｇ时各杂质组分的测定下限（ｕｇ／ｇ）为：ＣｅＯ＿２、Ｐｒ＿６Ｏ＿（１１）、Ｎｄ＿２Ｏ＿３、Ｓｍ＿２Ｏ＿３、Ｔｂ＿４Ｏ＿７、Ｈｏ＿２Ｏ＿３、Ｅｒ＿２Ｏ＿３，Ｔｍ＿２Ｏ＿３、Ｌｕ＿２Ｏ＿３０．４，Ｌａ＿２Ｏ＿３、Ｇｄ＿２Ｏ＿３、０．２，Ｄｙ＿２Ｏ＿３、Ｙ＿２Ｏ＿３０．０４，Ｙｂ＿２Ｏ＿３０．０２。６次取样分析，各杂质组分加入量为１０ｕｇ／ｇ（ＣｅＯ＿２为２ｕｇ／ｇ），加入回收率在８４％～１１２％；ＲＳＤ＜１３％。方法可用于纯度在９９．９９％～９９．９９９５％Ｅｕ＿２Ｏ＿３中１４种稀土杂质元素的测定。 相似文献
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10.
铜精矿中铅锌的连续测定 总被引：2，自引：0，他引：2
利用铜铁试剂分离Ｃｕ、Ｆｅ等干扰元素,同时铜铁试剂与Ｐｂ和Ｚｎ产生络合物吸附波,可连续测定铜精矿中的Ｐｂ和Ｚｎ。体系中铅峰在－０．５４Ｖ,锌峰在－０．９９Ｖ,线性范围Ｐｂ为８０～１６００μｇ／ＬＺｎ为１２０～１２００μｇ／Ｌ,检出限Ｐｂ为４０μｇ／Ｌ,Ｚｎ为８０μｇ／Ｌ,测定结果与参考值相符,ＲＳＤ（ｎ＝３）Ｐｂ（ｎ＝３）Ｐｂ〈６％,Ｚｎ〈１０％。 相似文献
11.
电感耦合等离子体质谱法同时测定地质样品中锗硒碲 总被引：7，自引：7，他引：0
锗、硒、碲三个元素的分析需要分别采用硝酸-氢氟酸-高氯酸-磷酸、硝酸-氢氟酸-高氯酸两种溶样体系,原子荧光光谱（AFS）、电感耦合等离子体质谱（ICP-MS）两种仪器进行测定,对于大批量地质样品的分析成本高、测试效率低。本文建立了在同一份溶液中用ICP-MS同一种仪器测定锗、硒、碲三元素的方法。样品用硝酸-氢氟酸-硫酸一种体系分解,试液以50%硝酸提取,3%乙醇定容,避免乙醇在复溶时的挥发损失,保证了试样溶液中的乙醇浓度均为最佳增敏作用所需值。试样分解过程中没有使用盐酸,避免了氯离子存在给锗、碲造成的损失。在3%硝酸-3%乙醇介质中硒、碲的灵敏度提高了2.2倍、3.7倍。同时克服了ICP-MS测定硒、碲难电离、灵敏度低的问题,保证了方法稳定性;CCT碰撞池技术消除了氩的多原子离子对硒测定干扰,提高了方法准确度。本方法通过分析国家一级标准物质进行验证,测定值与标准值基本一致,相对标准偏差（RSD,n=4）小于5%,样品前处理过程简单,分析效率高。 相似文献
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13.
铜精矿、镍精矿和锌精矿是金属硫化矿物,且为大宗进口商品,准确分析其中的稀散元素有利于矿物的综合利用。这类矿物中的稀散元素含量极低,各元素性质各异,尤其Ge和Se在湿法消解中由于挥发损失而无法准确定值,很难进行多种元素的同时测定,传统的方法需要通过预先分离富集,采用不同的仪器进行测定。本文以铜精矿、锌精矿和镍精矿为代表性硫化矿,采用微波消解对样品进行密闭前处理,电感耦合等离子体质谱法(ICP-MS)测定稀散元素含量,实现了多种元素的同时测定。条件实验表明在同时检测镓、锗、硒、镉、铟、碲、镧、铊的过程中,总固溶量、内标、质谱干扰消除的条件对三种金属硫化矿均一致,只是前处理过程中用酸的选择有些差异。硝酸-盐酸-氢氟酸-过氧化氢体系适合于测定镍精矿和锌精矿中的Ga、Ge、Se、Cd、In、Te、La、Tl和铜精矿中的Ga、Ge、Se、Cd、In、La、Tl,各元素的回收率在85.5%～116.6%之间;王水溶样法更适合测定铜精矿中的Te。 相似文献
14.
仪器残留物对氢化物发生-原子荧光光谱法测定硒和碲的影响探讨 总被引：1，自引：1，他引：0
用氢化物发生-原子荧光光谱法(HG-AFS)分析地矿样品时,在仪器反应块、传输管路和原子化器上会有残留物生成,这些残留物中的某些成分积累到一定量时就会显著地影响硒和碲的测定.本文在分析HG-AFS法测定硒和碲干扰情况的基础上,用高纯物质配制的标准系列进行试验,避免了共存成分的影响.通过比较在仪器反应块、传输管路和原子化器更换前后标准系列的测定结果,表明仪器残留物会对硒、碲测定产生影响.对一些反应块、传输管路和原子化器的溶出物进行分析,发现钛、铜、砷、锑和铋会影响硒、碲的测定灵敏度和标准系列线性相关系数,这些元素也是文献中提到的共存成分中的干扰元素.通过更换仪器相应配件,克服了仪器残留物的影响,硒、碲的灵敏度有不同程度的提高,标准系列测试结果质量明显改善,线性相关系数均在0.9995以上.本研究认为对仪器残留物成分的分析是控制原子荧光光谱法干扰的一种有效手段. 相似文献
15.
A method for the determination of Ge, As, Se and Te in silicate samples using isotope dilution-internal standardisation (ID-IS) octopole reaction cell (ORC) ICP-QMS by normal sample nebulisation was developed. The method does not involve either hydride generation or ion exchange. Germanium, Se and Te were determined by isotope dilution (ID), and As was determined by ID-IS. A silicate sample with an added Ge-Se-Te spike was digested with an HF-HNO3 -HBr mixture, dried, re-dissolved with HF and the supernatant liquid was directly aspirated into an ORC-ICP-QMS instrument with He or H2 gas. No matrix effects were observed down to a dilution factor (DF) of ∼ 70 for Ge, Se and Te and DF of ∼ 1000 for As, which resulted in 3s detection limits in silicates of 2, 1, 0.1 and 4 ng g−1 , respectively. Advantages of the method are the simple sample introduction as well as a capability of determining S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by ID-IS-ICP-QMS/SFMS from the same solution. Furthermore, the total sample solution consumption was only 0.253 ml with DF = 2000. Therefore, only a 0.13 mg test portion was required. To demonstrate the applicability of this technique, Ge, As, Se and Te in eight silicate reference materials were determined, as well as S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta in four carbonaceous chondrites. 相似文献
16.
Origin of the difference in the distribution behavior of tellurium and selenium in a soil-water system 总被引：4，自引：0，他引：4
Teppei Harada 《Geochimica et cosmochimica acta》2008,72(5):1281-1294
The distribution behavior of tellurium (Te) between soil and water in a synthetic soil-water system was studied coupled with the speciation of Te both in soil and water phases by using X-ray absorption fine structure (XAFS) spectroscopy and a high-performance liquid chromatography connected to an ICP-MS (HPLC-ICP-MS), respectively. The results were compared with a similar data set for Se, which was simultaneously obtained in this study. The oxidation states and host phases of Te and Se in the soil samples were given by XAFS, while the oxidation states in water were given by HPLC-ICP-MS. It was found that both Te and Se in soil are mainly associated with Fe(III) hydroxides under oxic conditions. From the EXAFS analyses, the outer-sphere complex is important for the Se(VI) sorbed on Fe(III) hydroxides in soils, while Se(IV), Te(IV), and Te(VI) form inner-sphere complexes. Under reducing condition, it was found that Te(0) and Se(0) species were formed and that Se was more readily reduced to Se(0) than Te, as is predicted from their Eh-pH diagrams. The reduction process from hexavalent to zerovalent species was different between Se and Te, that is, the direct reduction from Se(VI) to Se(0) was observed for Se, while Te was reduced stepwise from Te(VI) to Te(0) via Te(IV). In terms of the distribution between soil and water, Se distribution to water was much higher than that of Te under wide redox conditions. For Se, selenate is the predominant species in water even under reducing condition due to the much higher solubility of Se(VI) than Se(IV). Furthermore, a much smaller distribution of Te in water was primarily due to the larger affinities of Te(IV) and Te(VI) to Fe(III) hydroxides than Se(VI), which originates from the formation of the inner-sphere complexes of Te(IV) and Te(VI) to Fe(III) hydroxides. 相似文献
17.
原子荧光光谱法测定铜矿中硒和碲 总被引：11，自引：7，他引：11
介绍了铜矿中Ｓｅ，Ｔｅ的测定方法，样品经ＨＮＯ３－ＨＣｌＯ４分解，以含ＨＣｌＯ４的０．２ｍｏｌ／ＬＨＣｌ溶液通过７４３型阳离子树脂分离Ｃｕ，原子荧光光谱法测定Ｓｅ，Ｔｅ。 相似文献
18.
Allison Forrest Richard Kingsley Jean-Guy Schilling 《Geostandards and Geoanalytical Research》2009,33(2):261-269
Promising methods have been developed recently for the determination of selenium (Se) and tellurium (Te) in geological materials at ng g−1 and lower levels, using hydride generation-inductively coupled plasma-mass spectrometry. Here we report on a new isotope dilution-hydride generation-inductively coupled plasma-mass spectrometry (ID-HG-ICP-MS) method for the simultaneous determination of Se and Te, which is applied to basalts, and modified compared to previous work. The basalts were attacked and dissolved with hydrofluoric and nitric acid, spiked with enriched isotopes, and passed through a cation exchange column (AG 50-X8 100–200 mesh) to separate the major cations that interfere with Se and Te detection (e.g., Fe). The detection limits of this method were 0.010 ng g−1 for Se and 0.0030 ng g−1 for Te, well below the concentrations of Se and Te expected in basalts. The precision of the method for Se was 12.2 to 15.1% and for Te was 4.6 to 7.2% RSD from replicate analyses of basalt reference samples. The accuracy for Se determinations was 61 to 94% and for Te 28 to 100% of values previously reported in the literature for selected USGS reference materials. 相似文献
19.
原子荧光光谱法(AFS)具有灵敏度高、结构简单、容易操作等优点,但目前测定土壤和沉积物中的硒等元素的标准方法所采用的消解过程繁琐,易产生干扰。沸水浴可以把土壤和水系沉积物中硒提取完全,本文根据样品中元素丰度和仪器性能,将AFS测定Se的干扰分为Cu和Pb两大类,根据实验提出在水浴消解液加入浓盐酸(不宜加入硫脲-抗坏血酸),通过增加溶液酸度和Cl~-浓度,即保持样品中盐酸浓度高于23%,可抑制Cu~(2+)还原为Cu~0和Pb~(4+)生成PbH_4,有效降低了Cu的负干扰和Pb的正干扰,提高了AFS测定Se的精密度和准确度。本方法测定Se的检出限为0.008mg/kg,测试标准物质的相对标准偏差为0.5%～11%,相对误差为-16.3%～9.5%;比行业标准HJ 680—2013的检出限(0.01mg/kg)、精密度(0.79%～23.1%)和准确度等技术指标更佳。 相似文献
20.
Mass Fractions of S,Cu, Se,Mo, Ag,Cd, In,Te, Ba,Sm, W,Tl and Bi in Geological Reference Materials and Selected Carbonaceous Chondrites Determined by Isotope Dilution ICP‐MS 
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下载免费PDF全文 Zaicong Wang Harry Becker Frank Wombacher 《Geostandards and Geoanalytical Research》2015,39(2):185-208
Mass fractions of S, Cu, Se, Mo, Ag, Cd, In, Te, Ba, Sm, W and Tl were determined by isotope dilution sector field ICP‐MS in the same sample aliquot of reference materials using HF‐HNO3 digestion in PFA beakers in pressure bombs and glassy carbon vessels in a high‐pressure asher (HPA‐S) for comparison. Additionally, Bi was determined by internal standardisation relative to Tl. Because isobaric and oxide interferences pose problems for many of these elements, efficient chromatographic separation methods in combination with an Aridus desolvator were employed to minimise interference effects. Repeated digestion and measurement of geological reference materials (BHVO‐1, BHVO‐2, SCo‐1, MAG‐1, MRG‐1 and UB‐N) gave results with < 5% relative intermediate precision (1s) for most elements, except Bi. Replicates of NIST SRM 612 glass digested on a hot plate were analysed by the same methods, and the results agree with reference values mostly within 2% relative deviation. Data for the carbonaceous chondrites Allende, Murchison, Orgueil and Ivuna are also reported. Digestion in a HPA‐S was as efficient as in pressure bombs, but some elements displayed higher blank levels following HPA‐S treatment. Pressure bomb digestion yielded precise data for volatile S, Se and Te, but may result in high blanks for W. 相似文献