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本文利用鲁米诺-KIO4-Fe(1,10—phen)32+配合物体系产生化学发光反应,建立了测定痕量铁的新的化学发光分析方法。该法以1,10-phen为配位体,铁的检出限为1.6×10-7g/L,工作曲线响应浓度范围在1×10-5-1×10-3g/L。在测定2×10-4g/L铁的相对标准偏差为3.5%。用于检测工业沉淀BaSO4中痕量铁获得满意结果。 相似文献
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流动注射—化学发光分析测定矿石中痕量铌 总被引:5,自引:0,他引:5
利用铌对鲁米诺-H2O2-K3Fe(CN)6化学发光体系的抑制作用,建立了痕量Nb(Ⅴ)的流动注射-化学发光测定法。方法的检出限是2.3ng/mLNb(V).线性范围为0.01-1μg/mlNb(V),测定的相对标准偏差为3.0%(0.01μg/mLNb(V)(n=11),方法已应用于矿石中Nb的测定。 相似文献
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用偶合反应—流动注射化学发光法测定食品和水中痕量亚硝酸根 总被引:10,自引:0,他引:10
基于在酸性介质下,NO^-2与I^-快速反应产生I2和I2氧化Luminol产生化学发光反应,建立了Luminol-I^--NO ^02偶合发光体系测定痕量NO^-2R YYIUF。用于食品及水中亚硝酸 的测定,结果满意。 相似文献
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几种偶氮胂试剂与高碘酸钾的褪色反应用于动力学光度法测定痕量钌 总被引:22,自引:0,他引:22
本文发现了Ru(Ⅲ)对于KIO4分别与TB-偶氮胂、TC-偶氮胂、DCS-偶氮胂之间的褪色反应有显著的催化作用,研究了用此类褪色反应的动力学光度法测定痕量钌的最佳条件。此法灵敏度极高,其检出限可达0.01μg/10ml,且线性关系良好,反应在水相中直接进行,已用于贵金属精矿中痕量钌的测定。 相似文献
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用2-乙基己基膦酸单2乙基己酯萃取色说分离-原子发射光谱测定超高纯Tm2O3,Yb2O3,Lu2O3中痕量稀土杂质,可用于纯度为99.9999%-99.99999%Tm2O3,Yb2O3,lU2o3的纯分分析,14个稀土杂质的回收率在67%-133%之间;相对标准偏差5.1%-23.2%,分离周期10-13h。 相似文献
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催化光度法测定痕量NO2^—的研究:溴酸钾—酸性络蓝K体系 总被引:9,自引:5,他引:9
研究了在稀硫酸介质中,痕量NO2^-对溴酸钾氧化酸性络蓝K褪色反应的催化作用及其动力学分析,建立了测定痕量NO2^-的一性范围为0 ̄3.4μg/25ml,检出限为2.41×10^-7g·L^-1,用于水及蔬菜中痕量NO2^-的测定,结果满意。究了 相似文献
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对碘偶氮氯膦—高碘酸钾—钌(Ⅲ)的褪色反应用于痕量钌的催化分光 … 总被引:3,自引:0,他引:3
在H2SO4介质中对碘偶氮氯膦与高磺酸钾的褪色反应只有在痕量钌(Ⅲ)的存在下才能定量进行。醒文研究了该褪色瓜伯最佳条件及用于量钌的测定方法,其检出限为0.02μg.10mL^-1,钌含量在0.02~0.30μg.10ml。范围内符合比尔定律。该方法用于贵金属精矿中钌含量的测定,获得满意结果。 相似文献
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研究了钌与α,α‘-联吡啶配位反应。在pH4.6的HAc-NaAc缓冲溶液和NH2OH.HC存在下,在沸水浴中加热近5min,钌与α,α’-联吡啶反应形成了1:3配合物,在456nm表观摩尔吸光系数为1.1×10^4L.mol^-1.cm^-1。钌的比尔定律范围0-70μg/25mL,方法已被用于氯碱厂阳极泥中钌含量的测定。 相似文献
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建立了氢还原重量法测定三氯化钌产品大样中钌含量的新方法,研究并优化了测定条件,结合原子吸收光谱法(AAS)、电感耦合等离子体原子发射光谱法(ICP-AES)和氯化铵纯度考察了杂质元素对了分析结果的误差影响。结果表明,钌含量为0.3~0.6g的三氯化钌与5~7g氯化铵能完全形成(NH4)2RuCl6配合物,于约100℃烘干水分、350℃分解铵盐、750℃氢还原为海绵钌和105℃干燥水气的条件下,测定3.94%,5.88%,7.32%,9.47%,10.84%和12.93%含量的钌,极差、标准偏差(S)、相对标准偏差(RSD,n=22)和重复性限(r)分别为±0.01%,0.0030%~0.0050%,0.0369%~0.0761%和0.008%~0.014%。样品加标回收率99.96%~99.98%。方法的结果准确,精密度好,且与YS/T562—2009标准分析方法的吻合。 相似文献
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Prasad S Naik RM Srivastava A 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2008,70(5):958-965
The ruthenium catalyzed oxidation of tris(2-aminoethyl)amine (TREN) by hexacyanoferrate(III) has been utilized for the development of a new and sensitive catalytic kinetic method (CKM) for the determination of ruthenium(III). The reaction was followed spectrophotometrically by the decrease in absorbance at 420nm (lambda(max) of [Fe(CN)(6)](3-)). The CKM developed utilizes fixed time procedure under optimum reaction conditions where the change in absorbance (DeltaA(t)) versus ruthenium(III) concentrations is plotted. The calibration curve recommended for the method is linear in the concentration range 10.11-252.67ngml(-1) with very good accuracy and reproducibility and a maximum error 2.20%. The detection limits of the method for ruthenium(III) corresponding to 10, 15 and 20min are 8.02, 5.03 and 3.15ngml(-1), respectively. The ruthenium(III) has also been determined in the presence of several other interfering and non-interfering cations and anions and no foreign ions interfered in the determination of ruthenium(III) up to five-fold higher concentration of the foreign ions tested. The method is highly sensitive, selective and stable. It has successfully been applied for the determination of trace ruthenium(III) in some synthetic and environmental water samples. A review of most of the published catalytic kinetic and some other important methods for the determination of ruthenium has also been presented. 相似文献
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《Analytical letters》2012,45(9):1799-1805
ABSTRACT A simple spectrophotometric method for the determination of ruthenium in the presence of platinum in Pt-Ru-Ge catalyst applied in fuel cells has been developed. Platinum catalyst (20% Pt) with carbon support containing 0.5% Ru and 5% Ge was digested in the mixture of HCl+HNO3 (6+1). Carbon was separated from the examined sample by filtration after dissolution of the metals. Ruthenium was converted into a complex with thiourea (λmax=640 nm, ε = 2.9·103 1 mol?1 cm?1) in the medium of 5 M in HCl and 1% in thiourea after 15 min heating at 70 °C. Platinum does not interfere with the determination of ruthenium. Germanium is converted into volatile GeCl4 and escapes from the examined sample during the digestion step. The content of ruthenium determined in the examined samples of catalyst amounted to 0.49% (RSD = 0.14%). 相似文献
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毛细管区带电泳法同时测定饲料中西马特罗、盐酸克伦特罗和沙丁胺醇 总被引:2,自引:0,他引:2
建立了同时测定饲料中西马特罗、盐酸克伦特罗与沙丁胺醇的毛细管区带电泳-紫外检测方法。考察了实验参数对
分离和检测结果的影响。在最佳实验条件下,在60 mmol/L的柠檬酸-柠檬酸钠运行缓冲液(pH 6.29)中,上述3种物质在8
min内完全分离。西马特罗、盐酸克伦特罗和沙丁胺醇的线性响应范围为0.1~1.0 mg/L,最低检测限(以信噪比为3计)分
别为0.02,0.03和0.02 mg/L。所建立的方法直接用于饲料中西马特罗、盐酸克伦特罗和沙丁胺醇的测定,结果令人满意
。 相似文献
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Tracer techniques confirmed that a quantitative separation of osmium and ruthenium is possible by distillation from a hydrogen peroxide-sulphuric acid solution. Osmium distils quantitatively as OsO4 at a temperature of 105 ± 5° in about 30 min. The ruthenium contamination is approximately 0.01 %.In the present work a neutron activation analysis is described for the determination of traces of osmium in ruthenium sponge. When quantities of osmium below 30 p.p.m. are determined, the ruthenium contamination of the distillate must be taken into account, when the measurement is made with a 3” x 3” NaI(Tl) crystal. This can easily be achieved by measurement in two energy regions with a γ-spectrometer or with a multichannel pulse-height analyzer. With a NaI(T1) wafer as detector, the correction for ruthenium can be omitted for osmium concentrations above 10 p.p.m.With the addition method of analysis, 10–2000 p.p.m. in 10-mg samples of ruthenium sponge can be determined by neutron activation analysis. Chemical separation is necessary but no carriers are required. The lowest limit of determination is about 3 p.p.m. for a 3” x 3” crystal; for the wafer, about 1 p.p.m. can be determined. 相似文献
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A novel spectrophotometric method for the estimation of carbon monoxide at levels from 2 to 250 ppm is presented. The method is empirical and based on formation of a carbonyl complex of ruthenium(II) octaethylporphyrin and measurement of the difference in absorbance at 393.5 nm between this complex and the porphyrin reagent. Oxygen and nitrogen do not interfere and up to 300 ppm of sulphur dioxide and about 1500 ppm of carbon dioxide can be tolerated in determination of carbon monoxide at the 4 and 10 ppm levels. Hydrogen sulphide interferes and must be removed before the determination. The method has been tested over the range 2-45 ppm of carbon monoxide with 16 synthetic and 2 commercial standard air samples. The average error was +/- 3%. Application to urban-air samples and car-exhaust gases yielded acceptable results. The main disadvantages are the tedious preparation of the initial ruthenium(III)-porphyrin compound and the decomposition of the reagent in the presence of hydrazine. 相似文献
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Rezaei B Majidi N 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2007,66(4-5):869-873
A new simple, selective, high sensitive and rapid method has been developed for spectrophotometric determination of ultra trace amounts of ruthenium based on its catalytic effect on the oxidation of pyronin B by periodate at lambdamax=555 nm. The described method is able to quantify ruthenium in the range of 0.1-100 ng ml-1 (r=0.9973), with a detection limit (S/N=3) of 0.036 ng ml-1. Under optimum conditions, this procedure has been successfully applied to determine the trace levels of ruthenium in the environmental and biological samples. The precision, expressed as relative standard deviation of three measurements, is better than 2.44%. 相似文献
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采用气相分子吸收光谱法测定地下水中的亚硝酸盐氮(NO2^-)、氨氮(NH4^+)、硝酸盐氮(NO3^-)。考察NO2^-,NH4^+和NO3^-测定时的相互干扰,并给出了相应的消除方法。研究结果表明,测定NO2^-时,NH4^+和NO3^-无干扰;NO2^-对测定NH4^+和NO3^-产生干扰,可分别采用分段法和加入2滴10%氨基磺酸溶液的方法消除干扰;对于不含NO2^-或NO2-含量不高的地下水样品,可简化操作步骤直接测定NO3^-。该方法测定结果的相对标准偏差为0.73%~2.74%(n=12),样品加标回收率为97.67%~100.28%。所用检测仪器具有流动注射、自动进样及在线绘制标准曲线的功能,简化了标准方法中的样品前处理过程,减少了样品的损失,实现了自动化分析,大幅提高了检测结果的准确度和工作效率。 相似文献