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1.
电感耦合等离子体原子发射光谱法间接测定盐酸苯海索 总被引:12,自引:0,他引:12
研究了等离子发射光谱法间接测定片剂中盐酸苯海索含量的方法。详细讨论了ICP AES测定硼的“记忆效应”及最佳测定条件。实验表明在pH 2 .0~ 6 .0范围内 ,当四苯硼钠过量时可完全沉淀盐酸苯海索 ,硝酸铝可以使沉淀迅速絮凝而易于过滤 ,测定滤液中的四苯硼钠可以计算得到盐酸苯海索的含量。该法简单快速 ,相对标准偏差为 2 1%。实验测得盐酸苯海索 四苯硼沉淀的溶度积Ksp在 2 0℃时为8 84× 10 -12 相似文献
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ICP-AES法同时测定石英砂中的痕量元素 总被引:3,自引:0,他引:3
采用微波溶样,并通过条件试验,建立了微波溶样ICP-AES法同时测定石英砂中13种痕量元素的分析方法并已应用于实际样品的分析,方法的相对标准偏差≤10%,加标回收率为90%-107%。 相似文献
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大体积进样离子色谱法测定环境水样中高氯酸根 总被引:5,自引:0,他引:5
采用大体积500μL进样离子色谱法,电导检测测定了几种水体中高氯酸盐的含量。分析柱为容量高、亲水性强的以脂肪族碳骨架为基质的阴离子交换柱IonPac AS20,淋洗液在线发生器自动产生35 mmol/LKOH淋洗液,0.25 mL/m in等浓度淋洗。这种新型的以脂肪族碳骨架为基质的阴离子交换柱的采用,极大的削弱了该色谱柱对对氯苯磺酸的保留,完全消除了现行美国EPA高氯酸盐分析方法中高氯酸根与对氯苯磺酸共淋洗的问题。方法对高氯酸根的检出限(S/N=3)为0.5μg/L,高氯酸根浓度在1~1000μg/L范围内具有良好的线性(r=0.9991)。将本方法应用于自来水、河水和雪水样品中高氯酸盐的检测,实际样品的加标回收率在87%~114%之间;1μg/L高氯酸根连续进样9次,色谱峰面积相对标准偏差(RSD)为6.9%。 相似文献
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利用硒与4-硝基邻苯二胺在硫酸和高氯酸溶液中生成5-硝基-2,1,3-苯并硒二唑,且可被萃取至甲苯中的性质,用气相色谱法配合电子捕获检测器测定了甲苯中的5-硝基-2,1,3-苯并硒二唑,从而测定了硒的含量,数据处理采用自行研制的CWS1.0色谱工作站进行,可对样品采集文件进行多种处理,操作快速,简便,处理结果精密,准确,该法用于人发中微量硒的含量测定,获得了满意的结果。 相似文献
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铬天青S分光光度法测定食物中铝时高氯酸根的干扰及其消除 总被引:1,自引:0,他引:1
研究了铬天青S分光光度法测定铝时,样品消化液中残留高氯酸根的干扰及其消除方法,用阴离子交换树脂将样品消化液中残留的高氯酸根交换去除。结果表明,样品经过阴离子交换树脂柱后,高氯酸根基本去除,不再产生混浊,且铝的回收率达90%。该法简便可行,提高了铝测定的准确度。 相似文献
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纳米TiO2分离富集和ICP-AES测定地质样品中的钼和钨 总被引:14,自引:0,他引:14
本文以ICP-AES为检测手段,系统地研究了纳米TiO2材料对钼酸根和钨酸根离的分离/富集行为及影响其吸附和解脱的主要因素,并考察了共存离子的干扰影响,在优化的实验条件下,本法测定Mo(Ⅵ)和W(Ⅵ)的检出限分别为0.017μg/mL和0.044μg/mL,相对标准偏差(RSD)为1.8%(对Mo)和2.3%(对W)(n=9,c=5.0μg/mL)。本法已应用于水系沉积物和岩矿标准样品中Mo或W的测定,测定值与标准值基本吻合。 相似文献
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玫瑰桃红R褪色光度法测定水中铬(Ⅵ) 总被引:6,自引:0,他引:6
铬属于第一类污染物,是水质污染控制的一项重要指标。目前测定铬的方法主要有二苯碳酰二肼光度法、原子吸收光谱法、电感耦合等离子发射光谱法(ICP-AES)和滴定法。二苯碳酰二肼光度法显色剂不稳定,并且使用有机试剂;原子吸收光谱法和ICP—AES法只能测定总铬;滴定法灵敏度低,不适合微量铬的测定。 相似文献
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Cyclical bifurcated hydrogen bonded structures are proposed for aqueous solutions of hydrofluoric acid and for the bifluoride ion which are consistent with the spectral data. The structure proposed for HF is also applicable to solutions in organic solvents. Raman spectra of tetramethylguanidinium perchlorate suggest that the corresponding Raman spectra of perchloric acid solutions may not be interpreted in terms of a completely dissociated acid. Other evidence including activity coefficient, heat capacity and partial molal volume data suggest that there is some association in relatively dilute perchloric acid solutions between the perchlorate ion and the hydrated proton. This association decreases in concentrated aqueous solutions. 相似文献
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R. Sh. Erkasov R. M. Nesmeyanova S. R. Massakbayeva L. A. Kusepova 《Russian Journal of Inorganic Chemistry》2017,62(5):619-624
Heterogeneous equilibria in the zinc perchlorate–urea–perchloric acid–water quaternary system at 25°С were studied by investigating solubility. The crystallization regions were found for the initial solid components, eutonic compositions of the ternary systems constituting the quaternary system, binary compounds of urea with zinc perchlorate and perchloric acid, and also two new coordination compounds containing simultaneously zinc perchlorate, urea, and perchloric acid: ZnClO4 · 4CO(NH2)2 · HClO4 and ZnClO4 · 2CO(NH2)2 · HClO4. 相似文献
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R. Sh. Erkasov R. S. Orazbaeva R. M. Nesmeyanova S. R. Masakbaeva 《Russian Journal of Inorganic Chemistry》2016,61(3):370-376
Heterogeneous equilibria in the manganese perchlorate–urea–perchloric acid–water quaternary system at 25°С were studied by investigating solubility. The crystallization regions were determined for the initial solid components, eutonic compositions of ternary systems constituting the quaternary system, binary compounds of urea with manganese perchlorate and perchloric acid, and also two new coordination compounds containing simultaneously manganese perchlorate, urea, and perchloric acid: Mn(ClO4)2 · 4CO(NH2)2 · HClO4 and Mn(ClO4)2 · 2CO(NH2)2 · HClO4. 相似文献
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R. Sh. Erkasov S. R. Massakbayeva L. A. Kusepova S. M. Bolysbekova 《Russian Journal of Inorganic Chemistry》2017,62(9):1234-1239
Heterogeneous equilibria in the nickel perchlorate–acetamide–perchloric acid–water quaternary system at 25°С were studied by studying solubility. The crystallization regions were determined for the initial solid components, eutonic compositions of the ternary systems constituting the quaternary system, binary compounds of acetamide with nickel perchlorate and perchloric acid, and also two new coordination compounds containing simultaneously nickel perchlorate, acetamide, and perchloric acid: Ni(ClO4)2 · 4CH3CONH2 · HClO4 and Ni(ClO4)2 · 2CH3CONH2 · HClO4. 相似文献
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Potentially useful methods of synthesizing bispyrylium salts are reviewed. It is found that alkaline condensation of aromatic dialdehydes with aliphatic-aromatic ketones gives tetraketones, converted into bispyrylium salts by the action of hydride ion acceptors. Contrary to expectation, condensation of 1, 1, 2, 2-tetraacetylethane with resorcinol in acid solution gives a monopyrylium salt. Acetylation of 2, 4-dimethylpentane-2, 4-diol with acetic anhydride in the presence of perchloric acid led to the isolation of 2, 4, 6-trimethylpyrylium perchlorate, in addition to the expected methylenebispyrylium salt. Reaction of 2, 4-diphenyl-6-methylpyrylium perchlorate with terephthaldehyde gives a low yield of the product formed by condensation at both carbonyl groups. 相似文献
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改进的离子色谱法测定环境水样中的高氯酸盐 总被引:8,自引:0,他引:8
以亲水性阴离子交换柱IonPac AS16为分析柱, 以NaOH、乙腈和水的混合溶液为淋洗液, 采用电导检测法测定了环境水样中的痕量高氯酸盐. 通过添加有机改进剂有效地解决了4-氯苯磺酸和高氯酸盐共淋洗的问题. 实验考察了4种有机溶剂对高氯酸盐和4-氯苯磺酸保留时间的影响, 最终选定乙腈作为有机改进剂. 为了提高方法的灵敏度, 以AG19为浓缩柱对样品进行在线预浓缩. 采用预浓缩技术可使方法的检出限低至0.1 μg/L. 在0.2~200 μg/L线性范围内线性相关系数为0.9989, 将0.5 μg/L 高氯酸盐溶液连续进样测定11次, 所得峰面积的相对标准偏差(RSD)为4.2%. 将该方法应用于环境水样的测定, 加标回收率为93%~113%. 相似文献
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A new volumetric method has been proposed for the determination of beryllium in beryls and associated minerals. The method involves the direct precipitation of beryllium as BeNH4PO4.6H2O in presence of complexone II, dissolving the precipitate in dilute perchloric acid and titrating the liberated phosphate with standard bismuthyl perchlorate. Results for samples agree within ± 0.2% of the standard values. 相似文献
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E. V. Gromachevskaya T. P. Kosulina A. L. Chekhun V. G. Kul'nevich 《Chemistry of Heterocyclic Compounds》1993,29(4):465-468
A new method was developed for obtaining 4,4-diphenyl-4H-3,1-benzoxazinium Perchlorates by acylation of o-aminophenyldiphenylcarbinol with organic acids in the presence of perchloric acid. Weak CH acidity of the exocyclic methyl group of the corresponding perchlorate was observed.For communication 8 see [1].Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 542–546, April, 1993. 相似文献
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Shingo Sato Takeshi Watanabe Hironobu Kumagai Nobuo Kitamura Shigeru Matsuba Toshihiro Kumazawa Jun-Ichi Onodera Masanobu Suzuki 《Journal of heterocyclic chemistry》1999,36(5):1189-1193
Condensation of 2-hydroxyacetophenone with benzaldehyde in the presence of 70% perchloric acid in ethyl orthoformate gave the corresponding 4-ethoxyflavylium perchlorate, which was treated with aqueous ammonia or methylamine solution to afford 1,6,7,8-substituted 2-(3′,4′-substituted-phenyl)-4-quinolone in fair to good yield. 相似文献