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本文采用8-羟基喹啉-5-磺酸(HQS)为柱前衍生试剂,用含有10mmol·L-1的四丁基溴化铵(TBA+Br-)、7.5×10-5mol·L-1的EDTA和20mmol·L-1的pH5.6乙酸-乙酸钠缓冲溶液的甲醇-水(45:55,V/V)溶液为流动相,以C18硅烷化载体为固定相,16min内分离测定了Co(Ⅲ)、Fe(Ⅲ)、Al(Ⅲ)和Pd(Ⅱ)的HQS的配合物、信噪比为3时,检出限分别为:Co(Ⅲ)0.9ppb、Fe(Ⅲ)1.5ppb和Pd(Ⅱ)5.4ppb,方法灵敏度高,干扰少,用于测定试剂级盐酸,硝酸和中国红茶样品中的这些离子,结果良好。 相似文献
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报道了新荧光试剂3-苯基-5-(4′-硝基-2′-羧基苯偶氮)-2-硫代-4-噻唑啉酮(3P-4NRACP)的合成,通过元素分析、红外光谱、核磁共振谱及质谱确证了其结构。在pH5.6时,它与铜(Ⅱ)形成稳定的荧光螫合物,在γex/λem=305nm/405nm处产生强荧光,其荧光强度与铜(Ⅱ)的浓度在1.57×10-10~1.89×10-8mol/25mL范围内呈线性关系,灵敏度达1.57×10-10mol/g的铜(Ⅱ)。用此方法测定了杂交米、糯米及香米中的痕量铜(Ⅱ),结果满意。 相似文献
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以合成的新试剂5-Br-TAR为往前衍生试剂,首次用阴离子表面活性剂S,D.S.为对离子试剂。以含1×10(-2)mol·L(-1)的pH5.8的乙酸-乙酸钠缓冲溶液和3.5×10(-4)mol·L(-1)的S.D.S.的甲醇-水(68:32,V/V)为流动相,在C(18)柱上,15min内分离测定了Co(Ⅱ)、Rh(Ⅲ)、Cr(Ⅵ)的5-Br-TAR配合物。当SNR=2时,检出限分别为0.49、0.32、0.44ppb。用于废水及电镀液中Co(Ⅱ)、Cr(Ⅵ)的测定,效果较好。 相似文献
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研究了Mo(Ⅵ)与Tiron的反应,发现在pH4.0的HAc-NaAc介质中形成1:1配合物,该配合物在252nm、315nm有两个吸收峰,而在可见光区无吸收峰。测得ε252=6.9×10 ̄3L·mol-1·Cm-1,ε315=3.5×103L·mol-1·Cm-1。据此建立了测定Mo(Ⅵ)的方法,在252nm和315nm处的线性范围分别为1.6×10-6mol·L-1~2.O×10-4mol·L-1和3.2×10-4mol·L-1~2.0×10-4mol·L-1。检出限分别为8.O×10-7mol·L-1和1.6×10-6mol·L-1.PO_4 ̄3+、SiO_3 ̄2-对测定无干扰,而W(Ⅵ)、V(Ⅴ)、Fe(Ⅲ)等有干扰。该法试用于有机磷合钼聚多酸盐样品的测定,结果满意,方法回收率96%~102%,变异系数≤1.l%(n=12)。 相似文献
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Rh(Ⅲ)-TAC-CTMAB体系分光光度法测定Rh的研究 总被引:1,自引:0,他引:1
研究了在阳离子表面活性剂十六烷基三甲基溴化铵(CTMAB)存在下,用2-(2一噻唑偶氮)-对甲酚(TAC),在pH5.0的HAc-NaAc缓冲液中分光光度法测定Rh。Rh(Ⅲ)与TAC的络合比为1:1,表观摩尔吸光系数为ε680nm=1.25×104L·mol-1·cm-1,在1.2~8μg/10mL范围内符合比尔定律。方法的特征灵敏度为0.085μg/mL(1%吸收)。试验了贵金属及常见金属的干扰情况,并研究了干扰消除的方法,EDTA的加入可以消除一定量的Cu、Co、Ni、Zn的干扰。对催化剂试样的分析结果令人满意,变异系数均小于3%。 相似文献
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在PH5.3~7.1的六次甲基四胺缓冲溶液中,Al(Ⅲ)—CAS—CPB—TritonX—100络合物的最大吸收波长为630nm,ε=1.10x10 ̄5L.mol ̄(-1).cm ̄(-1),摩尔组成比Al(Ⅲ):CAS:CPB=1:3:3,铝量在0.2~8μg/25mol范围内符合比尔定律,回收率99~104%。本法以盐酸羟胺和邻菲啉作联合掩蔽剂,常见金属离子干扰少,用本法测定自来水、废水中微量铝,结果令人满意。 相似文献
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(R)-醇腈酶催化法合成(R)-(-)-1-(2-萘基)-2-N-甲基氨基乙醇 总被引:1,自引:0,他引:1
以2-萘甲醛为原料,经酶致转氰化、氰基还原、甲酰化、酰胺还原合成了光学活性(R)-(-)-1-(2-萘基)-2-N-甲基氨基乙醇5.转氰化过程采用来源于苦杏仁、枇杷仁、桃仁、黑布林果仁和苹果籽仁的醇腈酶催化HCN对底物醛的加成获得(R)-氰醇,通过比较反应产率和产物对映体过量值(ee)发现苦杏仁醇腈酶的催化效果最好,相应值分别为68.8%和88.3%;(R)-氰醇的O-保护衍生物2经化学法转化为标题化合物5,总产率达47%,ee值达88.0%, 其结构经IR和1H-NMR确证.实验结果表明,醇腈酶催化合成的手性氰醇光学纯度较高,是合成手性氨基醇化合物的优秀原料,并且在随后的化学转化过程中各步反应产物均很好地保留了光学纯度. 相似文献
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Vijay Kumar Patel Niraj Kumar Vishwakarma Avnish Kumar Mishra Chandra Sekhar Biswas Biswajit Ray 《应用聚合物科学杂志》2012,125(4):2946-2955
(S)-2-(Ethyl propionate)-(O-ethyl xanthate) (X1) and (S)-2-(Ethyl isobutyrate)-(O-ethyl xanthate) (X2) were used as the reversible addition-fragmentation chain transfer (RAFT) agents for the radical polymerization of vinyl acetate (VAc). The former showed the better chain transfer ability in the polymerization at 60°C. Kinetic study with both RAFT agents showed pseudo-first order kinetics up to around 85% monomer conversion. Molecular weight of the resulting polymer increased linearly with increase in the monomer conversion up to around 85%. The observed molecular weights calculated from 1H-NMR spectrum [Mn(NMR)] are close to the corresponding theoretical molecular weights [Mn(theor)]. The corresponding polydispersity index (PDI) of the resulting polymers remained almost constant at around 1.2 up to ∼ 65% monomer conversion and then increased gradually with the further increase in the monomer conversion. Chain-end analysis of the resulting polymers by 1H-NMR showed clearly that polymerization started with the radical forming out of the xanthate mediator. The negligible homo-chain extension and the hetero-chain extension involving synthesis of poly(VAc)-b-poly(NVP) diblock copolymer were occurred. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012 相似文献
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Vijay Kumar Patel Avnish Kumar Mishra Niraj Kumar Vishwakarma Chandra Sekhar Biswas Biswajit Ray 《Polymer Bulletin》2010,65(2):97-110
(S)-2-(Ethyl propionate)-(O-ethyl xanthate) (X1) and the newly synthesized (S)-2-(ethyl isobutyrate)-(O-ethyl xanthate) (X2) were used as the reversible addition-fragmentation chain transfer (RAFT) agents for the radical polymerization
of N-vinylpyrrolidone (NVP). The former showed the better chain transfer ability in the polymerization at 60 °C. Kinetics study
with X1 shows the psuedo-first order kinetics upto 45% monomer conversion. Molecular weight (M
n) of the resulted polymer increases linearly with increase in the monomer conversion upto around 45%. Polydispersity of the
corresponding poly(NVP)s increase gradually from 1.2 to 1.9 with increase in the monomer conversion. Chain-end analysis of
the resulted polymer by 1H NMR shows clearly that polymerization started with radical forming out of xanthate mediator. Living nature of the polymerization
was confirmed from the successful homo chain extension experiment and also the hetero-chain extension experiment involving
synthesis of poly(NVP)-b-polystyrene amphiphilic diblock copolymer. 相似文献
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以吲哚-4-甲醛、对甲基苯肼和对氯苯胺为原料,合成了1-(4-甲苯基)-3-(4-吲哚基)-5-(4-氯苯基)甲臢。经红外、核磁和质谱等波谱鉴定了目标分子的结构,并测定了它的氧化还原电位值。 相似文献
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