Co2+、Zn2+、Cd2+的阴离子交换色谱法分离研究

本文对钴与锌、镉等金属离子的阴离子交换色谱法分离进行了研究．采用201×7型阴离子交换树脂经氧化铵溶液饱和后,在pH＝4．0时,使钴与其它金属离子分离,然后分别用0．02mol／L的盐酸溶液及蒸馏水将锌、镉等金属离子从阴离子交换树脂上洗脱．此法分离效果好,操作简单方便．     

流动注射预富集-液相色谱联机测定痕量镍、铜、汞的研究

萃取－液相色谱用于同时测定痕量金属离子已引起广泛重视［１～３］，但操作方法繁琐，样品易玷污［４］．我们曾用固相萃取的方法使金属离子衍生为二乙基二硫代氨基甲酸盐（ＤＴＣ）配合物富集后，继以ＨＰＬＣ分离测定了钴、铜和汞［５］．本文研究了流动注射固相萃取预...     

碱性条件下的聚合物-盐水-液-固萃取体系应用于钴、锌、镍的分离和测定

1　引　　言水溶性高聚物的水溶液在无机盐的存在下能分成液 固两相 ,称为聚合物 盐水 液 固萃取体系。是近 10年开发的新型萃取体系。该体系在酸性条件下已成功地用于金属离子的定量萃取分离和分离纯化生物活性物质。已报道的聚合物 盐水 液 固萃取体系都是在酸性条件下 ,用调整聚合物和盐的浓度 ,使其分相并进行分离金属离子的。在碱性条件下的研究从未报道。这两种条件的区别在于 ,分相盐浓度与吐温浓度在碱性条件明显低于酸性条件 ,特别是分相用盐更低 ,降低了盐效应。例如 ,使Ｃｏ 萃取率Ｅ %达 10 0 %时 ,在ｐＨ 3.2 0～ 7.0 …     

二癸基次膦酸的合成及其萃取性能

以廉价的工业副产物混合癸烯和次膦酸钠反应,在常压下合成了二癸基次膦酸,分离产率达99.8%,产物纯度98%.萃取实验表明,二癸基次膦酸对镍/钴分离的选择性要好于Cyanex272,对镍和钴的萃取率和反萃率均大于96%;同时,对钴等金属离子,可实现对低pH浸出液的直接萃取.     

用作镍钴分离的P507萃取剂中微量硅的测定

P507是镍钴分离系数很高的新型酸性磷型萃取剂,我所拟用于氧化钴生产工艺中。但是萃取钴时也带入少量硅、钙和镁等金属离子,这将严重影响有机相的分层及氧化钴产品的质量等级。因此工艺试验提出准确测定P507相中金属离子的要求。我们考察了     

5-Br-PADAP光度法连续测定锌(Ⅱ)和钴(Ⅱ)

本文提出用二安替比林甲烷(DAM)连续分离锌、钴。在盐酸介质中加DAM,用二氯乙烷萃取锌,此时钴留在水相中,随后向水相加硫氰酸钾,用氯仿萃取钴,再分别用氨缓冲液,乙酸缓冲液反萃取有机相中的锌     

P_(507)萃取原子吸收法测定微量镍

P_(507)是目前国内外正在研究和使用的一种高效能的酸性磷型萃取剂,在不同pH值的条件下,可用于萃取下列金属Fe~(3+)、Zn~(2+)、Cu~(2+)、Co~(2+)……上述被萃取的金属离子又可在较强酸度下被反萃下来,本文着重探讨了钴、镍萃取分离条件,确定在pH4—5进行萃取,使钴与镍进行分离,又在2N盐酸介质中将Co~(2+)、Ni~(2+)定量地反萃下来,以原子吸收法测定镍,方法简单,快速,重现性好,同时适用于氧化钴、钴渣等冶金物料中微量镍的测定。     

火焰原子吸收法测定猕猴桃根茎叶中微量铜钴镍

试样经高氯酸、硝酸、盐酸分解，在ｐＨ６．８￣８．０的酒石酸铵介质中，利用铁的增敏作用，用乙酸丁酯萃取１－亚硝基－２－萘酚（ＮＮＰ）－铜、钴、镍的配合物，在有机相中用火焰原子吸收光谱法测定。方法简便、快速、灵敏，回收率在９６％￣１０６％，适宜于猕猴桃各部位微量铜、钴、镍的分析。     

酰胺型萃取剂——N,N-二烷基乙酰胺萃取分离钼及其在分析上的应用

酰胺型萃取剂于盐酸、硫酸介质中萃取分离某些金属离子已有报导。但这类萃取剂在磷酸介质中的萃取性能及其在分析上的实际应用尚未见报导。本文研究了磷酸介质中用N,N-二烷基乙酰胺(A_(?))萃取剂分离钼的条件,并用2-(5-溴-2(?)吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)作为显色剂分光光度测定微量钼。实验结果表明,选择酒石酸-磷酸介质,用A_(101)萃取剂可定量萃取钼(Ⅵ),一次萃取率达95%以上,且重现性好;数十毫克的铁、钴、镍、锰、铜、锌和铅等均不影响10微克钼的萃     

吐温80-盐-水体系的液-固萃取光度法测定痕量钴

研究了Ｃｏ（Ⅱ）－ＰＡＲ在吐温８０－硫酸铵体系中的最佳萃取条件,建立了生物样品中测定痕量钴的非有机溶剂液－固萃取光度法。在ｐＨ７．０～１０．５的ＮＨ３．Ｈ２Ｏ－ＮＨ４Ｃｌ缓冲溶液中,１金属配合物Ｃｏ（Ⅱ）－ＰＡＲ可被吐温８０固相富集,最大吸收波长为５１５ｎｍ,钴含量在０～５．０ｕｇ／ｍＬ范围内服从比尔定律,可用于头发、茶叶和维生素Ｂ１２针剂中痕量钴的测定。     

反相高效液相色谱法同时测定镉、铅、铜和锌

 研究了meso-四（对羟基苯基）卟啉为柱前衍生化试剂与Cd2+,Pb2+,Cu2+和Zn2+离子的配合反应条件及配合物在C18色谱柱上的分离条件,建立了反相高效液相色谱快速分离光度检测Cd2+,Pb2+,Cu2+和Zn2+的新方法。配合物和试剂在15 min内出峰完毕。4种离子的检出限为: Cd2+0.02 ng,Pb2+0.02 ng, Cu2+0.02 ng,Zn2+0.12 ng;线性范围为:Cd2+0.8 μg/L～150 μg/L,Pb2+0.8 μg/L～300 μg/L,Cu2+0.8 μg/L～500 μg/L,Zn2+5.0 μg/L～1 000 μg/L;方法的日内相对标准偏差为:2.8%～4.8%,测定低、中、高3个浓度的日间相对标准偏差为3.7%～9.7%。     

A tryptophan-containing fluoroionophore sensor with high sensitivity to and selectivity for lead ion in water

We report herein a fluoroionophore sensor derivated from tryptophan that shows high sensitivity (detection limit up to 0.15 microM) and specific selectivity for lead ion (Pb2+) over Ca2+, Cd2+, Co2+, Cr3+, Cu2+, K+, Mg2+, Na+, Fe2+, Mn2+, Ni2+ and Zn2+ in aqueous solution.     

低压离子分离-化学发光在线检测过渡金属离子

 研究了低压离子 (LPIC)分离 柱后鲁米诺化学发光 (CL)检测方法 ,并分离测定了Cu2 + ,Co2 + ,Cr3 + ,Fe2 + ,Mn2 + 等 5种过渡金属离子。以草酸 柠檬酸混合溶液作为洗脱液 ,Luminol H2 O2 Mn + 作为化学发光检测体系 ,对过渡金属离子进行在线检测。测定的线性范围分别为 (mg·L-1) :Co2 + ,0 0 0 1～ 0 .1;Cu2 + ,0 1～ 6 ;Mn2 + ,0 0 6～ 4 ;Fe2 + ,0 0 3～ 5 ;Cr3 + ,0 0 2 5～ 1。检测限分别为 (μg·L-1) :Co2 + ,0 85 ;Cu2 + ,85 ;Mn2 + ,4 2 ;Fe2 + ,2 1;Cr3 + ,2 0。     

1-乙酰基-3-(2-羟基-4,6-二甲氧基苯基)-5-芳基-2-吡唑啉的合成及Cu2+荧光探针行为

设计合成了6个1-乙酰基-3-(2-羟基-4,6二甲氧基苯基)-5-芳基-2-吡唑啉化合物4a～4f.测试了它们的紫外光谱和荧光光谱,研究了其对铜离子的选择性识别作用.结果表明,化合物4f作为铜离子荧光探针,受常见离子干扰较小,对于铜离子有着较高的选择性和较低的检出限.     

Senio river ecosystem: characterization and distribution of inorganic species in water and sediments

Analytical results are reported for the determination of inorganic species in water and sediments sampled in the Senio river ecosystem. The species determined are Cu, Pb, Cd, Zn, Co, Cr, Ni, Fe, Mn, Hg, F-, Cl-, Br, NO3-, SO4-, Na+, K+, Ca++, Mg++, NH4+ in integrated water, and Cu, Pb, Cd, Zn, Co, Cr, Ni, Fe, Mn, Hg in sediments. For all the elements, in addition to detection limits, precision and accuracy are given: the former, expressed as relative standard deviation (sr), and the latter, expressed as relative error (e), were good, being in all cases lower than 6%. Limitedly to Cu, Pb, Cd and Zn a critical comparison with voltammetric measurements is also discussed.     

Improved scheme of chelation ion chromatography with a mixed eluent for the simultaneous analysis of transition metals at microg l(-1) levels

An improved scheme of chelation ion chromatography (CIC) system and a mixed eluent for the simultaneous determination of transition metals are described. A method based on the improved CIC system and the mixed eluent (PDCA/Na2C2O4/LiOH/NaCl) for the analysis of seven metals (Pb2+, Cu2+, Ni2+, Zn2+, Co2+, Cd2+ and Mn2+) at microg l(-1) levels in a single isocratic elution is developed. The optimize conditions which are different from references for analyte concentration and chromatographic separation are studied in detail. D418 chelation resin is used to further reduce values of the reagent blank. The above seven metals are measured at 565 nm using 2-[(5-Bromo-2-Pyridyl)-Azo]-5-Diethyl-AminoPhenol(5-Br-PADAP) as the post-column derivatizing reagent. Detection limits range from 0.3 to 12 microg l(-1) when 4 ml of sample is pre-concentrated. The results of real sample analysis are satisfactory.     

Inorganic species in water and sediments of the Lamone and Marzeno rivers ecosystem

Analytical results are reported for the determination of inorganic species in water and sediments sampled in the Lamone and Marzeno rivers ecosystem. The species determined are Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn, Hg, F-, Cl- Br-, NO3-, SO4--, Na+, K+, Mg++, Ca++, NH4+ in superficial water, and Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn, Hg in sediments. For all the elements, in addition to detection limits, precision and accuracy are given: the former, expressed as relative standard deviation (s(r)), and the latter, expressed as relative error (e), were good, being in all cases lower than 6%.     

Effects of Ca2+, Zn2+ and Cd2+ on uridine diphosphate-glucuronyltransferase and beta-glucuronidase activities in rat liver microsomes

The effect of various metals on uridine diphosphate (UDP)-glucuronyltransferase and beta-glucuronidase activities in rat liver microsomes was investigated. The presence of Mn2+, Cd2+, Zn2+, V5+, Ni2+, Co2+, Cu+ or Ca2+ (20 microM) in the enzyme reaction mixture did not cause a significant alteration of UDP-glucuronyltransferase activity in hepatic microsomes. Of these metals, Zn2+ and Cd2+ (20 microM) caused a remarkable increase in hepatic microsomal beta-glucuronidase activity. Appreciable effects of Zn2+ and Cd2+ on beta-glucuronidase activity were seen at 5.0 microM, and the effects were saturated at 50 microM. Ca2+ (5.0-50 microM) and/or the Ca2(+)-binding protein regucalcin (2.0 microM) did not have an appreciable effect on UDP-glucuronyltransferase and beta-glucuronidase activities in hepatic microsomes. Thus, Zn2+ and Cd2+ uniquely increased beta-glucuronidase activity. The Zn2(+)- and Cd2(+)-induced increase in beta-glucuronidase activity was completely reversed by the presence of an SH group-protecting reagent (dithiothreitol). The response of the microsomal enzyme to Zn2+ and Cd2+ (20 microM) was no longer seen after treatment with 0.2% Triton X-100 [polyoxyethylene(10)octylphenyl ether], indicating that the stimulation by these metals is dependent on membrane association. The present study suggests that, of various metals tested, Zn2+ and Cd2+ can uniquely increase hepatic microsomal beta-glucuronidase activity and that their effect is based on binding to membranous SH groups, beside the enzyme protein.     

A study of the mechanisms involved in the separation of metal ions with a mixed-bed stationary phase

Summary The optimization of chromatographic methods for the determination of metal species require an understanding of the mechanisms involved. In this work, the separation of Cd, Co, Cu, Fe(II/III), Mn, Pb and Zn using a mixed bed column (IonPac CS5A) and a cation-exchange column (IonPac CS2) is studied as a function of mobile phase composition. The type and concentration of complexing agent and of ionic strength modificators were evaluated. The charge of analytes were calculated using the classical ion exchange approach to highlight the effect of eluent composition on retention. The comparative study enabled us to identify an optimal eluent composition for the separation of the nine metal species.     

Analysis of heavy metals in atmospheric particulate by ion chromatography

Cu, Ni, Zn, Co, Fe+2, Mn, Cd, Fe+3 and Pb are easily separated and detected in isocratic mode by ion chromatography with post-column derivatization using a bifunctional ion-exchange column and an eluent formed by oxalic acid (28 mM) and sodium nitrate (250 mM). The separation is optimised by using a suggested sample solution containing a given concentration of chloride. Detection limits were 10-15 ppb for all the metals except for cadmium and lead, for which detection limits of 30 and 60 ppb were found, respectively. The method was tested on an atmospheric particulate certified sample. The measured values were in good agreement with certified values. Real samples of atmospheric particulate from industrial and urban sites were analysed and the results are discussed.