离子色谱法测定硫酸氧钒中的Cl~-和C_2O_4~(2-)

采用离子色谱法测定硫酸氧钒中的Cl-和C2O42-。以水合肼沉淀除去硫酸氧钒溶液中的钒离子,上清液经OnguardⅡH柱过滤后,采用IonPac AS19阴离子分离柱和IonPac AG19阴离子保护柱,以氢氧化钾溶液为淋洗液进行梯度淋洗,电导检测器进行检测。Cl-和C2O42-的线性范围分别为0.01~0.50,0.10~50.0mg·L-1,测定下限分别为0.597,0.594mg·kg-1。加标回收率分别在96.9%~104%和88.2%~92.0%之间,测定值的相对标准偏差均小于5.0%。     

离子色谱法测定不同地区家庭饮用井水中的阴、阳离子

采用离子色谱法测定不同地区家庭饮用井水中氟离子、氯离子、硝酸根、硫酸根、钠离子、钾离子、镁离子和钙离子等8种阴、阳离子的含量。样品经IonPac AS11-HC型分离柱及IonPac AG11-HC型保护柱分离,以30mmol·L-1氢氧化钾溶液为淋洗液(阴离子分析);样品经IonPac CS12A型分离柱及IonPac CG12A型保护柱分离,以20 mmol·L-1甲基磺酸溶液为淋洗液(阳离子分析);采用电导检测器检测。8种离子在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3s)在0.002~0.034mg·L-1之间。对井水样品进行测定,测定值的相对标准偏差(n=6)在0.59%~2.0%之间。用标准加入法做方法的回收试验,计算得回收率在98.3%~109%之间。     

离子色谱法测定水中7种阴离子

建立了离子色谱法同时测定水中7种阴离子的方法。样品过滤后,采用IonPac AS-19阴离子色谱柱分离,KOH溶液梯度淋洗,电导检测器检测水中氟离子、亚氯酸盐、溴酸盐、氯离子、硝酸盐、氯酸盐、硫酸盐的含量。7种阴离子线性关系良好r0.998 8,加标回收率为91.6%~108%,相对标准偏差(RSD)为0.13%~8.8%。样品前处理简便,分离度和加标回收率均较高,适用于水中7种阴离子的测定。     

离子色谱法测定化肥中六种阴离子

提出了离子色谱法同时测定化肥中6种无机阴离子的方法。化肥试样经水超声浸取,采用C18固相萃取柱和Ba固相萃取柱净化,萃取液中氟离子、氯离子、亚硝酸根、溴离子、碘离子、硫氰酸根以IonPac AS18(250 mm×4 mm)为分析柱、IonPac AG18(50 mm×4 mm)为保护柱,氢氧化钾溶液梯度洗脱分离并用电导检测器同时测定了6种阴离子的含量。6种阴离子的检出限(3S/N)在0.001 2~0.013 5 mg.L-1之间。方法的加标回收率在78.9%~103.0%之间,相对标准偏差(n=6)在0.61%~6.5%之间。     

串联电导及紫外检测器-离子色谱法测定土壤中6种有机酸根和无机阴离子

应用离子色谱法测定土壤样品中正丁酸根、草酸根、溴离子、碘离子、氯离子及硫酸根等6种有机酸根和无机阴离子的含量。样品(10.00g)用50mmol·L-1氢氧化钠溶液50mL超声提取60min,离心分离。取上清液,经0.22μm滤膜过滤和OnGuardⅡP柱净化。流出液稀释5倍后通过IonPac AG18柱分离,用不同浓度的氢氧化钾溶液进行梯度淋洗,用串联的电导检测器和紫外检测器(236nm)进行检测。前者用于除碘离子外的5种阴离子的测定,后者用于碘离子的测定。上述6种阴离子的峰面积分别在一定范围与其质量浓度呈线性关系,其检出限(3S/N)在0.013~0.095μg·g-1之间。加标回收率在92.0%~112%之间,测定值的相对标准偏差(n=6)在1.2%~7.2%之间。     

离子色谱法测定聚合物材料中铬(Ⅵ)含量

采用离子色谱法测定聚合物材料中的铬(Ⅵ)含量。取粒径小于250μm的聚合物样品用0.5mol·L-1氢氧化钠溶液提取3h。分取适量提取液经过滤及RP柱净化后,通过IonPac AG19保护柱及DIONEX IonPac AS19阴离子分离柱分离,先后用25mmol·L-1和50mmol·L-1的氢氧化钠溶液淋洗分离柱,采用抑制电导检测器检测。铬(Ⅵ)的质量浓度在0.10~10.0mg·L-1范围内与其峰面积呈线性关系,检出限(3s/k)为7mg·kg-1。对聚氯乙烯(PVC)样品连续测定8次,测定值的相对标准偏差为9.2%。用标准加入法进行方法的回收试验,测得回收率在95.2%~105%之间。     

离子色谱法测定啤酒中6种无机阴离子的含量

取啤酒样品(10.0mL)超声脱气30min,用经活化的固相萃取小柱净化。收集净化液2.0mL,用水稀释至20.0mL。所得样品溶液经0.22μm滤膜过滤后,直接进样进行离子色谱分析。采用阴离子交换柱IonPac AS11作为分离柱,用氢氧化钾淋洗液发生器产生的不同浓度的氢氧化钾溶液作梯度淋洗,流量为1.0 mL·min~(-1),柱温为35℃。6种无机阴离子(Cl~-、NO_2~-、Br~-、NO_3~-、SO_4~(2-)、PO_4~(3-))在一定质量浓度范围内呈线性,检出限(3S/N)在0.005~0.028mg·L~(-1)之间。对同一个啤酒样品进行精密度试验,测定值的相对标准偏差(n=6)在2.1%~3.0%之间。按标准加入法进行回收试验,回收率在89.0%~105%之间。     

离子色谱法分析油气田地层取样样品中的阴、阳离子

探讨使用离子色谱仪分析油气田地层取样样品的可行性。该方法使用ICS900型离子色谱仪(配阴离子色谱柱AS19和阳离子色谱柱CS12A),同时由自动淋洗液发生器RFC30产生20 mmol/L氢氧化钾溶液和20mmol/L甲烷磺酸溶液,流量为1 m L/min。7种离子测定结果的相对标准偏差为0.87%~3.40%,样品加标回收率为98.00%~104.0%。该方法精密度和准确度满足油气田地层取样样品中阴阳离子的分析要求。     

离子色谱法测定食品中氯酸根含量

提出了离子色谱法测定食品中氯酸根含量的方法。食品样品采用水超声萃取15min,取部分萃取液加入亚铁氰化钾和乙酸锌溶液,离心,取上清液调节其酸度至pH 11~12,经IonPac AG19保护柱及Dionex IonPac AS19分离柱分离,以不同浓度的氢氧化钾溶液为淋洗液,采用抑制电导检测器检测。氯酸根的质量浓度在0.01~20.0mg·L-1范围内与其峰面积值之间呈线性关系,检出限(3S/N)为0.04mg·kg-1。方法用于青瓜和虾仁样品的分析,加标回收率在84.7%~93.4%之间,测定值的相对标准偏差(n=6)小于5%。     

离子色谱法测定果汁中乳酸、富马酸、柠檬酸的含量

建立离子色谱测定果汁中的乳酸、富马酸、柠檬酸的分析方法。利用Onguard II RP柱进行预处理除去疏水性物质,使用IonPac AS19(250 mm×4 mm)色谱柱,IonPac AG19(250 mm×4 mm)保护柱,以氢氧化钾溶液梯度淋洗,采用自循环抑制电导检测的方法对苹果汁样品中的乳酸、富马酸、柠檬酸含量进行检测。该方法能够准确地测定果汁中乳酸、富马酸、柠檬酸的含量,线性方程的相关系数在0.999以上,样品的加标回收率为90.7%～102.8%,测定结果的相对标准偏差为0.41%～1.43%(n=6),样品的定量限分别为0.5,0.2,0.3 mg/L。该法操作简单,环境友好,灵敏度高,测定结果准确可靠,能满足果汁中有机酸含量的测定要求。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

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.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

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.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

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%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

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.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

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.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.