钒—钼酸铵比色法测定食品中总磷

食品中的磷具有营养学意义.常用的定量方法有钼蓝比色法和重量法,钼蓝比色法测定食品中的总磷,酸度对测定结果的影响比较大,方法的重现性差;重量法仅适用于磷的含量较高的食品.本文参照文献,用钒-钼酸铵比色法测定食品中总磷,试液酸度对吸光度几乎没有影响,磷含量在0.5～10mg·L~(-1)范围内呈良好的线性关系,相关系数r=0.9998,相对标准偏差<3%,加标回收率在97.6%～103.7%之间.     

微波消解-磷钼蓝分光光度法测定城市污泥中总磷浓度

建立了微波消解-磷钼蓝分光光度法测定城市污泥中总磷的方法。在微波环境中硝酸-过氧化氢能够将城市污泥中无机磷盐和含磷有机物消解为正磷酸盐,在弱酸性条件下,正磷酸盐在铋盐的催化条件下与钼酸铵-抗坏血酸生成磷钼蓝,于分光光度计波长690nm处进行测定总磷浓度。方法的相对标准偏差0.63%～0.95%,加标回收率为101%～102%,能够满足对城市污泥中总磷浓度的测定要求。     

火焰原子吸收法间接测定钢中硼和磷

提出了溶剂萃取-火焰原子吸收光谱法间接测定钢中硼和磷的分析方法.在弱酸性介质中硼酸、苯羟乙酸、铁(Ⅱ)以及邻二氮菲能形成稳定的多元离子缔合物,被1,2-二氯乙烷萃取后再用去离子水反萃取,然后测定水相化合物中的铁;在盐酸介质中,磷酸根与钼酸铵形成磷钼杂多酸,被甲基异丁基甲酮萃取后,测定有机相磷钼杂多酸中的钼.并可分别间接测定硼和磷.在优化的反应条件下,硼和磷的质量浓度分别在0.12～3.24及0.04～1.00mg/L范周内时,吸光度与质量浓度之间具有良好的线性关系,硼和磷的检出限分别为0.036和0.015mg/L.以8份样品空白进行测定,得硼和磷的标准偏差分别为1.2%和0.5%.方法用于钢样中微量硼和磷的测定,拓展了原子吸收分光光度计的应用范围.     

磷钼酸铵分光光度法测定盐酸羟胺

建立了磷钼酸铵分光光度法测定盐酸羟胺的新方法,在酸性条件下,盐酸羟胺可以定量地将磷钼酸铵还原为磷钼蓝,通过测定磷钼蓝的吸光度,从而间接测定盐酸羟胺的含量。显色体系最大吸收波长为720 nm,盐酸羟胺在0.01～0.12 mg/mL浓度范围内与A呈良好的线性关系,其回归方程为A=0.0139+6.1826c(mg/mL),线性相关系数r=0.9994。方法用于实际样品中盐酸羟胺的含量测定,结果与标准方法一致。     

用比色法测定镀镍电极镍磷含量

镍和丁二酮肟在pH=10的缓冲介质中,形成丁二酮肟红色络合物,选择530 nm为测定波长,表观摩尔吸光系数为1.74×105L/mol.cm,稳定时间可达3 h。采用磷钼酸铵比色法测定磷,最大吸收峰位于700 nm,表观摩尔吸光系数为2.70×105L/mol.cm。镍和磷测量的线性范围均为0~100μg/mL。将该方法用于镀镍电极的镍磷含量分析,测定结果的相对标准偏差不大于5.0%。     

磷钼酸铵-孔雀绿-PVA分光光度法测定钽粉中磷

提出了以磷钼酸铵-孔雀绿-PVA三元络合物体系测定金属钽粉中磷的方法,该体系表观摩尔吸光系数ε=8.19×104L.mol-1.cm-1,加标回收率为:99.3%~105%,方法的RSD为:5.9%。有效地解决了目前高纯钽粉中磷的分析难题,方法已应用于实际产品的分析中。     

光度法测定冶金用五氧化二钒中磷

利用光度法测定磷的研究已有报道[1] ,但主要是针对岩石、矿石及污水中的磷 ,对冶金用五氧化二钒中磷的测定很少 ,由于冶金用五氧化二钒产品呈片状 ,采用酸溶方法溶解不完全 ,只能用碱熔方法。冶金用五氧化二钒中磷的测定存在基体效应现象 ,本文采用标准中加入基体的方法予以克服 ,通过对测定波长、酸度、显色剂用量、显色时间等条件的优化选择 ,方法的精密度达到 2 7% ,平均回收率达到10 0 .5 %。能满足冶金用五氧化二钒中磷的测定。1　试验部分1.1　仪器与主要试剂UV75 5B型紫外可见分光光度计过硫酸铵溶液 :30 0g·L- 1钼酸铵溶液 :5 …     

磷钼酸铵分光光度法测定药物中6-巯基嘌呤

建立了磷钼酸铵分光光度法测定6-巯基嘌呤(6-MP)的方法。结果表明,在一定条件下,6-MP可以定量地与磷钼酸铵反应生成磷钼蓝,通过测定磷钼蓝的吸光度,从而间接地测定6-MP的含量。显色体系最大吸收波长为710nm,6-MP质量浓度在0.004～0.06 mg/mL范围内与A呈良好的线性关系,线性回归方程为A=0.0258+10.655ρ(mg/mL),线性相关系数r=0.9986。方法用于实际药品中6-PM的含量测定,结果与药典法一致。     

硒钼杂多酸—罗丹明B离子缔合物显色反应的研究与应用

研究了在聚乙烯醇分散剂存在下 ,硒 钼酸铵 罗丹明B(RDB)三元缔合物的显色反应。建立了测定硒碘盐中微量硒的新方法。离子缔合物的最大吸收波长为 5 70nm ,表观摩尔吸光系数ε570 =5 .6× 10 5L·mol- 1·cm- 1。在测定条件下 ,硒含量在 0～ 6μg/ 2 5ml范围内符合比耳定律。对于硒碘盐样品的测定 ,RSD≤ 2 .5 % ,结果满意     

钼酸铵溶液配制方法的探讨

钼酸铵试剂非常广泛地应用在化工及分析化学方面,而在以钼蓝比色法测定磷时,应用尤为普遍。但是,钼酸铵溶液的配制方法却极不相同。大体有以下四种: 1.配制钼酸铵水溶液,占23％: 2.分别配制钼酸铵水溶液和酸(硫酸或盐酸)溶液,在搅拌下,将前者注入后者,占41％;     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

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.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

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.     

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

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.