偶氮胭脂红B动力学光度法测定Fe(III)

动力学光度法测定铁[1,2]多用2,4 二氯苯酚+4 氨基安替比林[3]、苄橙[4]、次甲基蓝[5]、酸性铬蓝Ｋ[6]和二溴对甲基偶氮羧[7]等为监测组分,以Ｈ2Ｏ2为氧化剂,α,α 联吡啶为活化剂。本文用催化光度法确定铁(ＩＩＩ)催化高碘酸钾氧化偶氮胭脂红Ｂ褪色反应的动力学条件及有关参数,仅以高碘酸钾为氧化剂,不使用活化剂,操作简单、快速,用于水样及生物样中铁的测定,结果满意。1　实验部分移取0 20ｍｌＦｅ(ＩＩＩ)标准工作溶液(1 0μｇ/ｍｌ)于25ｍｌ比色管中,依次加入2 0ｍｌ0 02ｍｏｌ/Ｌ硫酸溶液,1 5ｍｌ0 010ｍｏｌ/Ｌ高碘酸钾溶液,1 5ｍ…     

用碘离子选择性电极测定砷(Ⅲ)

砷是自然界中普遍存在而且对人体有毒的化学元素之一 ,目前分析砷的方法很多[1,2 ] ,本文用碘离子选择性电极间接测定砷 (Ⅲ )的含量 ,方法操作简单 ,结果可靠 ,检出限可达到 6.2 5× 1 0 -7ｍｏｌ·Ｌ-1。1　试验部分1 .1　主要仪器与试剂ｐＸＳ 2 1 5离子活度计(上海精科雷磁公司 )79 1型磁力加热搅拌器碘离子选择性电极 (江苏电分析仪器厂 )离子强度调节剂 :0 .5ｍｏｌ·Ｌ-1ＫＮＯ3 +0 1ｍｏｌ·Ｌ-1氯乙酸水为二次蒸馏水1 .2　试验方法取 5 0ｍｌ容量瓶若干个 ,分别加入 0 .5ｍｏｌ·Ｌ-1ＫＮＯ3 溶液 5ｍｌ,0 .1ｍｏｌ·Ｌ-1氯乙酸 2…     

催化动力学法测定人发中痕量硒

催化动力学褪色法测定痕量硒已有报道[1 ,2 ] ,但大都存在Ｆｅ3+、Ｃｕ2 +等共存离子的干扰。在实际分析中常需对样品进行繁琐的预处理。实验研究了在盐酸溶液中 ,以ＥＤＴＡ作掩蔽剂 ,痕量硒催化氯酸钾氧化 5 Ｂｒ ＰＡＤＡＰ褪色反应及其动力学条件 ,以加硒催化反应与不加硒非催化反应的吸光度之差△Ａ对温度 1 /Ｔ作图得一直线 ,由Ａｒｒｈｅｎｉｕｓ式求得该反应的活化能Ｅａ=94ｋＪ/ｍｏｌ,建立了测定硒的新方法。方法检测限为 5.7× 1 0 - 5μｇ/ｍｌ,Ｓｅ(Ⅳ)的测定范围为 0～ 0 .4μｇ/ 2 5ｍｌ,用此法测定人发中痕量硒 ,结果令人满…     

硅钼蓝光度法测定五氧化二钒中微量硅

采用氢氧化钠对试样进行前处理 ,在硝酸 0 .0 8～ 0 .4 0ｍｏｌ·Ｌ- 1酸度下 ,硅与钼酸铵形成硅钼酸络离子 ,在硫酸 0 .8～ 1.6ｍｏｌ·Ｌ- 1酸度下 ,被还原生成硅钼蓝 ,借此进行光度测定[1] ,硅量在 10～ 10 0 μｇ/5 0ｍｌ范围内遵守比耳定律。1　试验部分1.1　仪器与试剂72 2光栅分光光度计硅标准溶液 :10 μｇ·ｍｌ- 1五氧化二钒标准溶液 :2 .5ｍｇ·ｍｌ- 1,称取五氧化二钒 (99.99%) 0 .2 5 0 0 ｇ置于 30 0ｍｌ聚四氟乙烯烧杯中 ,加入 10 0ｇ·Ｌ- 1ＮａＯＨ溶液 10ｍｌ,低温加热溶解 ,取下 ,加入数滴酚酞 ,用ＨＮＯ3 (1+ 1)调至无…     

催化动力学褪色光度法测定痕量间苯二胺

1　引　　言间苯二胺是一种重要的化工原料 ,同时也是一种致癌的芳香胺类物质。目前未见用催化动力学光度法测定间苯二胺的报道。本文系统地研究了间苯二胺对Ｈ2 Ｏ2 氧化结晶紫褪色反应的催化动力学行为 ,建立了具有高灵敏度的简便、快速、选择性高的测定间苯二胺的新方法。2　实验部分2 1　主要仪器与试剂　ＵＶ 2 4 0型紫外可见分光光度计 (日本岛津公司 ) ;ＴＢ 85恒温器 ;72 1分光光度计 (上海第三分析仪器厂 )。结晶紫 2 4 5× 1 0 - 4 ｍｏｌ Ｌ;ＫＩＯ3 0 .0 0 3ｍｏｌ Ｌ ;Ｈ2 Ｏ2 3% ;间苯二胺储备液 1 0 0 0ｇ Ｌ储备液。然后…     

5-Br-PADAP光度法测定锰矿中微量钴

5 Ｂｒ ＰＡＤＡＰ作为显色剂 ,已被广泛用于测定许多金属元素。本文将其用于锰矿中微量钴的测定 ,获得满意结果。1　试验方法取 0～ 10 μｇ钴标准于 5 0ｍｌ容量瓶 ,加入0 0 5ｍｏｌ·Ｌ-1氨三乙酸 5ｍｌ,10 0ｇ·Ｌ-1ＮＨ4 Ｆ溶液 2ｍｌ,以水稀至约 30ｍｌ ,加入 7.5× 10 -4 ｍｏｌ·Ｌ-15 Ｂｒ ＰＡＤＡＰ溶液 4ｍｌ ,摇匀 ,放置 2 0ｍｉｎ ,在摇动下加入硫酸 (1+2 ) 10ｍｌ,以水稀释至刻度 ,用 2ｃｍ比收稿日期 :2 0 0 1 0 4 2 9色皿 ,5 80ｎｍ波长处 ,在 72 1Ａ分光光度计上测其吸光度。2　样品分析称取样品 0 .2 0 0 0ｇ于 2 0 0…     

催化动力学光度法测定生物样品中的草酸

提出了一种经动力学光度法测定生物样品中草酸的方法。基于在硫酸介质中,草酸能有效地催化重铬酸钾氧化丁基罗丹明Ｂ褪色,当反应温度为６５℃、反应时间１２ｍｉｎ时,非催化反应溶液的吸光度Ａ０和催化反应溶液吸光度Ａ的ｌｎＡ０／Ａ值与草酸浓度在０．２０～１０．０８μｇ／ｍｌ之间存在良好线性关系。反应体系用高浓度ＮａＯＨ终止后室温下可稳定２ｈ以上。催化反应的表观活化能为１３．５３ｋｊ／ｍｏｌ。方法可直接用于菠菜     

Excel在理化检验中的应用

对食用盐中碘和盐业部门的加碘食盐 (根据调查加碘食盐中碘均以碘酸钾形式加入 )中的碘含量进行监测时 ,由于此项工作样本量多 ,为了避免人为误差 ,可运用Ｅｘｃｅｌ电子表格的数据处理功能 ,对测定的大量数据进行统计计算 ,提高其准确度。1　原理碘盐中的碘酸钾在酸性环境中 ,加入过量的碘化钾析出碘 ,以淀粉作指示剂 ,用硫代硫酸钠标准溶液滴定并计算其含量 :ＩＯ- 3+ 5Ｉ- + 6Ｈ+3Ｉ2 + 3Ｈ2 Ｏ　　　2Ｎａ2 Ｓ2 Ｏ3+Ｉ2 2ＮａＩ+Ｎａ2 Ｓ4 Ｏ62　食盐中碘含量检测称取碘盐 10 .0 0 0 0 ｇ置于 2 5 0ｍｌ碘量瓶中 ,加无碘水 5 0ｍｌ使盐…     

吸光光度法测定硝酸银中微量铜

硝酸银制成后测定杂质含量是鉴定纯度的一个重要环节。杂质铜的含量多少直接影响到硝酸银的纯度。本文研究了 0 .1～ 0 .3ｍｏｌ·Ｌ- 1ＫＯＨ介质中 ,用ＫＩＯ4 作为显色剂 ,采用巯基棉分离 ,吸光光度法测定了硝酸银中微量铜 ,结果满意。1　试验部分1.1　主要仪器与试剂756ＭＣ紫外可见分光光度计 (上海第三分析仪器厂 )Ｃｕ2 +标准溶液 :称取ＣｕＳＯ4 ·Ｈ2 Ｏ 1.96 4 4 ｇ于烧杯中 ,加水溶解后 ,再加几滴硫酸 ,移入 50 0ｍｌ容量瓶 ,稀至刻度 ,配成 1ｍｇ·ｍｌ- 1储备液。逐级稀释成10 μｇ·ｍｌ- 1工作液。ＫＩＯ4 溶液 :称取ＫＩＯ4…     

关于配位滴定测定水的总硬度终点返红问题的讨论

ＥＤＴＡ滴定法测定水的总硬度时 ,常以 0 .1ｍｏｌ·Ｌ-1氨 氯化铵缓冲液调节溶液ｐＨ为 1 0 ,以络黑Ｔ为指示剂 ,用 0 .0 1ｍｏｌ·Ｌ-1ＥＤＴＡ滴定。此方法使用过程中经常出现终点返红问题。本文对此进行了试验。1　试验部分1 .1　主要仪器与试剂ＣＯ2 发生器 (自制 )氨 氯化铵缓冲溶液 :0 .1ｍｏｌ·Ｌ-1所用试剂均为分析纯以上1 .2　试验方法取自来水样 1 0 0 .0ｍｌ,以 0 .1ｍｏｌ·Ｌ-1氨 氯化铵缓冲液调节其 ｐＨ为 1 0 ,加络黑Ｔ指示剂 (与ＮａＣｌ配比为 1∶1 0 0 )少许 ,以 0 .0 1 0 0 0ｍｏｌ·Ｌ-1ＥＤＴＡ标准溶液滴定至终点…     

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.     

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.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.