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1.
原子荧光光谱法测定食品中的镉   总被引:7,自引:0,他引:7  
袁爱萍 《分析化学》1997,25(10):1199-1201
研究了在水溶液中,Cd与KBH4反应生成挥发性物种,以原子荧光光谱法测定食品中的痕量Cd的分析方法,方法的检出限为0.12μg/L,线性范围0~50μg/L,回收率为86%~112%。  相似文献   

2.
氢化物—无色散原子荧光法测定螺旋藻胶囊中的微量硒   总被引:18,自引:2,他引:18  
邹菁  张平 《分析试验室》1998,17(5):84-86
研究了氢化物原子荧光法测定螺旋藻胶囊中的微量硒,系统地考察了消解体系;确定了最佳测定条件,共存元素的影响及干扰的消除,硒的检出限为1.3×10^-3mg/L,线性范围为0-0.25mg/L,回收率在97.5%-102.3%之间,RSD小于5%。  相似文献   

3.
本文描述了用2,3-二氨基萘荧光分光光度法测定水样中亚硝酸盐的最佳测定条件,并测定了井水和湖水中的亚硝酸盐。测定样品的检出限为0.4μg/L,线性范围是1.0~1500μg/L,相对标准偏差为1.6%,加标回收率为95%~106%。本法简便、快速,准确度高,共存离子干扰小,样品无须萃取步骤。  相似文献   

4.
用离子色谱法测定环境样品中甲酸、乙酸、草酸   总被引:12,自引:0,他引:12  
用离子色谱法分析环境样品中甲酸、乙酸、草酸,操作简便,灵敏度较好,线性范围宽。甲酸、乙酸、草酸的检出限分别为0.02mg/L、0.10mg/L、0.04mg/L;样品加标回收率分别为93%~106%、94%~108%、92%~108%;相对标准偏差分别为1.2%、2.4%、2.7%;工作曲线的线性范围分别为0.00~30mg/L、0.00~30mg/L、0.00~50mg/L。该法可用于酸雨、大气  相似文献   

5.
建立了用荧光分光光度计作为流动注射分析的检测器,用自动研制的流通池测定垃圾渗出液中苯胺的新方法。方法的线性范围为0.07~0.5mg/L,检出限为0.05mg/L。用于垃圾渗出液的测定,结果与HPLC法无显著性差异,回收率在96%~104%之间,该法具有选择性好、灵敏度高、重现性好的特点。  相似文献   

6.
对微波消解-氢化物发生原子荧光光谱法测定头发样品中微量汞的方法进行了研究。采用HNO3和H2O2作消解剂,在最佳微波消解条件和测定条件下,线性回归线方程为Y=259.7c 155.4,相关系数r=0.9996,检出限为0.01ng/mL,线性范围为0-20ng/mL。测定结果的相对标准偏差为0,4%~2.8%,回收率为94,0%-102.0%。  相似文献   

7.
协同催化光度法测定血清中唾液酸   总被引:5,自引:0,他引:5  
本文利用Cu^2+和Cr^3+的协同催化作用及Brij35的增溶作用建立了测定唾液酸的光度分析新方法,该方法的线性范围为0~980mg/L,检出限为1.5mg/L,相对标准偏差为1.83%~2.66%,回收率为94.7%~102.0%,用于测定人血清中的唾液酸,获得满意结果。  相似文献   

8.
采用酶联反应荧光法测定样品烯醇化酶的总活性。方法最低检出限为0.2IU/L,在0.20~35IU/L范围标准曲线呈线性,γ〉0.997,回收率达90%,相对标准偏差〈10%,对临床确诊的视网膜母细胞瘤进行了初步探讨,检验结果垢特异性较高。  相似文献   

9.
采用微波消解进行样品前处理,以硫脲为预还原剂,用氢化物发生原子荧光法测定塑料原料及其制品中的砷、汞。测定砷和汞的线性范围均为0~8μg/L,砷、汞的检出限分别为0.005、0.076μg/L,测定结果的相对标准偏差分别为4.96%~7.38%、2.94%~7.20%(n=6),回收率分别为92.0%~103.2%、92.0%~98.0%。  相似文献   

10.
建立在硝酸介质中用氢化物发生-原子荧光光谱法同时测定水中砷和锑的方法。优化了仪器工作条件、酸度、硼氢化钾及还原剂浓度。砷、锑的线性范围为0~10.0μg/L;检出限分别为0.02,0.01μg/L;测定结果的相对标准偏差分别为1.77%~3.72%,2.95%~4.87%(n=6);加标回收率分别为98%106%,96%105%。该法操作简便,灵敏度高,快速,便于推广,适用于水中砷和锑的同时测定。  相似文献   

11.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

12.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

13.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

14.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

15.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

16.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

17.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

18.
N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).  相似文献   

19.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

20.
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.  相似文献   

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