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GC-MS检测萃取剂中内分泌干扰物 总被引:2,自引:0,他引:2
烷基酚作为内分泌干扰物的代表物成为环境毒理学研究的热点,多支链取代也最难生物降解.在湿法冶金工业中壬基酚作为基质改善剂在大量使用[1],而且萃取剂主要品种多含壬基酚结构单元,它们通过降解将释放出壬基酚,为此建立对壬基酚的分析检测十分有必要,尤其是西部开发更应注意新工艺后边有许多新的化学药品还未进行的环境评价,应防止类似农药666的错误再次出现.萃取剂中壬基酚的GC-MS检测方法以国内外3种主产品为对象,其分析样品编号分别为12102,12103,12104,壬基酚对照编号为12101.样品直接溶于甲醇中进样. 相似文献
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Cyanex272-P507浸渍树脂协同萃取色层分离铥镱镥的研究 总被引:1,自引:0,他引:1
以Cyanex272-P507浸渍树脂采用萃取色层法对铥镱镥富集物进行了吸附和淋洗分离研究,考察了淋洗剂浓度、稀土负载量、淋洗液流速等因素对分离铥镱镥富集物的影响。结果表明,在充填的树脂粒度为0.3~0.6 mm的色层柱中,以0.2 ml.cm-2.min-1进料流速时能得到较大的吸附率;在稀土负载量为树脂重量的0.6%,淋洗液流速为1.0 ml.cm-2.min-1,温度为30℃,装柱树脂高度为400 mm(高径比为25∶1)的条件下,用1.0,1.5,2.0 mol.L-1盐酸梯度淋洗Tm,Yb,Lu,可实现铥镱镥富集物三者的完全分离。 相似文献
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Cyanex923对稀土元素硝酸盐的萃取 总被引:2,自引:0,他引:2
研究了Cyanex923在正庚烷溶液中对15种稀土元素硝酸盐的萃取,计算了分离系数,得出了反应机理,考察了温度对萃取平衡的影响以及萃合物的红外光谱,发现yawnex923遥可能应用于从在土中分离镧以及从重稀土中分离钇。 相似文献
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用Cyanex272-Span80-甲苯乳状液膜体系研究了铅的迁移行为,确定了铅迁移的适宜条件。在此条件下,许多常见离子如Cu^2+、Co^2+、Ni^2+、Cd^2+等均不迁移,Hg^2+迁移率很低。因此Pb^2+能与这些离子得到快速且完全的分离。这对分析测定及三废处理等工作具有实际意义。 相似文献
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M. Johansson R. Malmbeck B. Wierczinski G. Skarnemark 《Journal of Radioanalytical and Nuclear Chemistry》2001,250(3):437-443
A study of the extraction of polonium from aqueous solutions containing -hydroxyisobutyric acid (-HIBA) was performed with four different extractants, di-n-octyl sulphide (DOS), Cyanex 272, Cyanex 301 and Cyanex 302, dissolved in toluene. The extracted complex for DOS at low -HIBA concentrations is most likely PoO(-HIB)2·2DOS, while at higher -HIBA concentrations there seems to be a solvating effect implicating an extracted complex of the type PoO(-HIB)2(-HIBA)2·2DOS. For the extraction of polonium with Cyanex 272 the results are inconclusive. The extracted complex is either PoOA2 or PoO(-HIB)2·2HA. For extraction with Cyanex 301 or Cyanex 302 the major extracted species does not contain any -HIBA molecules. The neutral species in both cases is PoOA2, extracted at low extractant concentrations, while at higher extractant concentrations a complex of the type PoOA2·xHA is extracted. The extraction of polonium increases in the order Cyanex 272 < DOS < Cyanex 302 < Cyanex 301. 相似文献
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前言自从发现协同萃取以来,许多作者对协同萃取进行了广泛的研究。Reddy等人应用亚砜等中性萃取剂研究了两种中性萃取剂的协同萃取(以下简称B-B类协萃),认为在第一萃取剂(S~Ⅰ)浓度([S~Ⅰ])固定时,萃取分配比D的对数值对第二萃取剂(S~Ⅱ)的浓度([S~Ⅱ])的对数值作图是直线,其斜率为S~Ⅱ的溶剂化数n,随[S~Ⅰ]的增加直线斜率逐渐下降。似乎难以用斜率分析法来确定溶剂化数目。本文研究了二-正-辛基亚砜(以下简称DOSO),TBP和TOPO从NH_4SCN溶液中萃取Ce(Ⅲ)。分析了实验数据,提出了B-B类协萃分配比D的计算公式。 相似文献
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HBTMPTP与Cyanex925协同萃取Sc(Ⅲ)的研究 总被引:8,自引:0,他引:8
研究了二(2,4,4-三甲基戊基)单硫代膦酸(HBTMPTP,HL)和支链三烷基氧化膦(Cyanex925,B)的正己烷溶液在H2SO4介质中对Sc(Ⅲ)的萃取性能,结果表明,在较低酸度(CH2SO4〈0.25mol/L)时存在协同效应,用斜率法确定了Sc(Ⅲ)的协萃配合物的组成为Sc(HL2)2B3(SO4)1/2,计算了协萃反应的平衡常数,讨论了协萃配合物的IR谱和FAB-MS。 相似文献
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V. V. Belova A. A. Voshkin N. S. Egorova A. I. Khol’kin 《Russian Journal of Inorganic Chemistry》2010,55(4):629-633
Mechanisms for the extraction of rare earth metals with a binary extracting agent based on bis(2,4,4-trimethylpentyl)phosphinic
acid with the formation of various complexes in the organic phase were proposed. The compositions of the extracted compounds
were determined, and the distribution of these compounds was adequately described by calculated curves. 相似文献
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Karolina Wieszczycka Joanna Zembrzuska 《Journal of Radioanalytical and Nuclear Chemistry》2014,299(1):709-720
The photodegradation of the organothiophosphorous extractant Cyanex 302 and purified bis(2,4,4-trimethylpentyl)monothiophosphinic acid dissolved in toluene was carried out in photoreactor using UV–Vis light irradiation. Possible degradation products were identified with the assistance of FT-IR, LC/MS/MS and GC/MS. The catalytic influence of zinc(II), copper(II) and cobalt(II) ions and the presence of trace values of water and aqueous solutions of sulphuric acids on the photodecomposition of Cyanex 302 were studied. The results demonstrated that the presence of trace amounts of water causes mainly the degradation of bis(2,4,4-trimethylpentyl)monothiophosphinic acid with the simultaneously fourfold increase in bis(2,4,4-trimethylpentyl)phosphinic acid concentration. The shaking with aqueous solution of sulphuric acids results in the decrease in the photodegradation probably by blocking of OH radical. Metal ions also affect the degradation causing the increase in bis(2,4,4-trimethylpentyl)phosphinic acid concentration. The photodegradation was also carried out in open atmosphere under sunlight and the obtained results were compared with those obtained in a Heraeus photoreactor. 相似文献
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H. Mimura H. Hoshi K. Akiba Y. Onodera 《Journal of Radioanalytical and Nuclear Chemistry》2001,247(2):375-379
Microcapsules enclosing an extractant with strong affinity for Am were prepared by employing a biopolymer gel as an immobilization matrix. A relatively large separation factor between Am and Eu was exhibited by the microcapsule containing of bis(2,4,4-trimethylpentyl)dithiophosphinic acid (Cyanex 301, HA) and alginic acid (HALG). The chromatographic separation of these metal ions was accomplished by gradient elution through the column packed with HA-HALG. 相似文献
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氟乙酰胺分子式为FCH2CONH2,是合成很早的化合物.50年代以后,被用于灭鼠与杀虫,毒力甚强,并容易引起二次中毒[1].虽然,早在1982年我国政府已严禁使用氟乙酰胺和毒鼠强为灭鼠药,但不法分子至今仍在生产和销售,引起误食和投毒.对毒鼠强的GC-MS分析已有一些报道[2,3],但是由于氟乙酰胺对热不稳定(170℃分解),在一般的非极性柱子中的保留时间很短,易与溶剂混合,一般方法很难检定.我们选用GC-MS,通过选择进样方式,色谱条件,溶剂,对氟乙酰胺进行了检定.本法比较简便,定性准确,有较高的灵敏度. 相似文献
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The composition of the commercial reagent Cyanex 302 was investigated by GC-MS. Mass spectrometric studies allowed us to confirm that bis(2,4,4-trimethylpentyl)monothiophosphinic acid is the major compound and that a considerable amount of tris(2,4,4-trimethylpentyl)phosphine oxide is also present. The study also revealed that the extractant has three minor components. These were identified as bis(2,4,4-trimethylpentyl)phosphinic acid, bis(2,4,4-trimethylpentyl)phosphine oxide and bis(2,4,4-trimethylpentyl)dithiophosphinic acid. The mass spectra of these compounds are discussed and some fragmentation processes are postulated. 相似文献
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国外对有机氯农药残留限量要求很严格.目前对残留有机氯农药的常规检验,仍多采用气相色谱-电子俘获检测器(GC-ECD)[1],被认为是检出限最低,定量准确度较高的方法.但GC-ECD定性功能不强,对基底复杂样品常给出假阳性结果.随着近年GC-MS技术的不断发展、完善,仪器的检测灵敏度也随之提高.发达国家已将GC-MS法广泛应用到日常检验中.本实验参照国外限量要求,采用GC-MS的EI-SIR和NCI技术,对应用较多机氯农药进行鉴定,有效地解决了痕量有机氯农药定性问题. 相似文献