锌-镉还原-分光光度法测定地表水中硝酸盐

提出预先将试样中NO-3用锌-镉还原法还原为NO-2.对还原反应的条件,诸如氯化钠及氯化镉的浓度、溶液的PH值、金属锌(卷状)的加入量以及还原反应所需时间等,进行了研究和优化.还原所得NO-2在酸性溶液中与磺胺进行重氮化后再与萘乙二胺偶合生成红色偶氮化合物.在其吸收峰543 nm波长处测定其吸光度,据此,在校正曲线上间接地查得试样中NO-3的含量.NO-3质量浓度在0～0.400 mg·L-1范围内遵守比耳定律.方法的检出限(S/N=3)为0.008 mg·L-1,在0.1 mg·L-1的浓度水平进行了测定的精密度试验,计算得到相对标准偏差(n=6)为2.1%.在3个浓度水平上作了回收试验,得出回收率在99%～103%之间.     

离子色谱法测定印刷电路板上痕量无机阴离子

将印刷电路板样品置于异丙醇及水(3 1)的混合溶液中浸泡以萃取板上的无机阴离子Cl-、Br-、NO-3及SO2-4,并经在线预处理除去异丙醇对测定的干扰.用离子色谱法测定所得溶液中4种阴离子,对影响上述阴离子分离条件(淋洗液浓度及样品溶液的在线转移时间等)进行了研究.在最优条件下,测得4种阴离子工作曲线的线性范围均为20.0～800.0 μg·L-1,以质量浓度为100.0,800.0μg·L-1的混合标准溶液对方法的精密度作了试验,测得Cl-、Br-、NO-3及SO2-4峰面积值的相对标准偏差(n=6)依次为0.7%,0.8%,0.7%,1.8%和0.1%和0.1%,1%,0.1%,0.7%.     

离子色谱法测定大气降尘中四种阴离子

以流速 1.5ml·min- 1,0 .2 4mol·L- 1Na2 CO3和 0 .30mol·L- 1NaHCO3混合液为淋洗液 ,在YSA 4型阴离子分离柱上分离 ,采用带电导检测器的离子色谱仪对大气降尘中四种阴离子进行分离测定 ,F- 、Cl- 、NO- 3、SO2 - 4的检出限 (3S/N)分别为 0 .0 0 1,0 .0 0 1,0 .0 0 6 ,0 .0 0 4mg·L- 1,相关系数分别为 0 .9991,0 .9986 ,0 .9997,0 .9984 ,RSD分别为 0 .80 % ,0 .76 % ,1.80 % ,1 90 %。     

在线渗析-离子色谱法测定蔬菜中无机阴离子

采用在线渗析技术与离子色谱法联用测定蔬菜等样品中多种阴离子.样品提取后,取上层清液经渗析后进入分离柱,采用Metrosep A Supp 4-250阴离子交换柱,以1.8 mmol·L-1Na2CO3与1.7 mmo·L-1NaHCO3混合溶液为流动相,化学抑制电导检测.方法中各阴离子检出限(3S/N)为1-18ug·L-1.方法用于复杂基质蔬菜样品中F-、Cl-、NO-2、Br-、NO-3、PO3-4和SO2-4等阴离子的测定,加标回收率均大于78%,相对标准偏差(n=6)在1.8%～6.1%之间.     

紫外吸光光度法测定水源水中硝酸盐

氮的化合物 (主要包括氨态氮、亚硝酸盐氮、硝酸盐氮 )是饮用水水质评价的重要卫生指标之一。准确测定水源水中各种氮化合物含量 ,对于水质正确评价和是否适用于饮用有着重要意义。NO- 3 的测定 ,常用二酚磺酸法和镉柱还原法。前法因 Cl-严重干扰需脱氯处理 ,后法也繁琐费时。利用 NO- 3 在紫外区的吸收光谱特性对其进行定量测定 ,已有不少文献报道。本文对水源水中 NO- 3 的测定做了有关条件试验 ,结果较为理想。1　试验部分1 .1　仪器与试剂751 G紫外分光光度计NO- 3 标准溶液 :0 .1 0 0 0 mg.ml- 1 ,称取在 1 0 5～1 1 0°C干燥的硝…     

离子色谱法连续测定乳制品中的NO2-和NO3-

采用AS18,4 mm×250 mm色谱柱,以32 mmol/L的KOH作为淋洗液,建立了一种用具有电导检测器的离子色谱连续测定乳制品中NO-2和NO-3的方法.该法处理简单、快速,定量结果准确. NO-2和NO-3的检出限(3S/N)分别为0.001和0.004 mg/L,标准曲线相关系数分别为0.999 7和0.999 6,添加水平上的回收率均在90.0%～103.4%之间.     

柱后衍生离子色谱法测定饮用水中IO3^- ClO2^- BrO3^-和NO2^-的研究

为建立柱后衍生离子色谱法同时测定饮用水中的IO-3、ClO-2、BrO-3和NO-2,采用高容量柱,以8.0 mmol·L-1碳酸钠作淋洗液,0.5 g·L-1邻二甲氧基联苯胺盐酸盐+5 g·L-1溴化钾+25%甲醇+1.0 mol·L-1硝酸作衍生剂,反应温度60℃,450 nm波长处检测.方法的线性范围广、相关性好(r>0.999),相对标准偏差为0.84%～5.4%(n=6),样品加标回收率91.3%～108.0%,检出限0.023～0.97μg·L-1.方法适用性好,可满足上述痕量阴离子试样的测定.     

长链S-烷基双硫腙为载体的碳酸氢根离子电极

以溴化S 十六烷基双硫腙载体制备了碳酸氢根离子选择性电极 ,选择性次序为 :ClO-4 >SCN->I-～HCO-3 >ClO-3 ～NO-3 >Ac->NO-2 >Cl->H2 PO-4 >SO2 -4 。膜配比 (质量百分比 )为溴化S 十六烷基双硫腙 (SHDTZ)·HCO-3 ∶邻苯二甲酸二异辛酯∶PVC =2 .5∶65.0∶32 .5电极性能最佳。 32℃时 ,在pH 8 30 .1mol/L三乙醇胺 硫酸缓冲溶液中 ,HCO-3 离子浓度在 1 .0× 1 0 -2 ～ 1× 1 0 -5mol/L范围与电极电位呈线性响应 ,检测限为 5.0× 1 0 -6mol/L;斜率为 54± 2mV/decade。研究了HCO-3 离子与载体的作用机理。用该法测定了人体血清中HCO-3 ,结果与滴定法一致。     

纤维素水解液厌氧发酵产丁二酸发酵液中有机酸和混合单糖的测定

对于以纤维素类原料(玉米皮)水解糖液作碳源厌氧发酵制备丁二酸的发酵液,利用Aminex HPX-87H(300 mm×7 8 mm i.d., 5 μm)离子排斥色谱柱及折光示差检测器检测,以0 005 mol/L H2SO4溶液(pH 2 0)作流动相,在流速为0 6 mL/min,柱温为55 ℃时对发酵液进行检测,16 min内能将发酵液中甲酸、乙酸、丁二酸、葡萄糖、木糖、阿拉伯糖完全分离定量.6种物质线性相关系数均大于0 999,方法的回收率为99 3%～102 1%;RSD为0 6%～1 6%.本方法能够简便、快速测定丁二酸发酵体系中有机酸及单糖的含量.     

离子色谱法测定茶叶中的无机阴离子

提出了离子交换色谱法分离测定茶叶中F-、Cl-、Br-、NO3-、H2PO4-和SO2-4 6种无机阴离子含量的方法.茶叶样品中6种阴离子用水在95℃超声萃取20 min后,经IonPac ASll-HC阴离子分离柱,AGll-HC阴离子保护柱,以氢氧化钾为淋洗液,浓度从15 mmol·L-1到30 mmol·L-1进行梯度淋洗.F-、Cl-和Soi2-4的峰面积与其质量浓度在0.01～150.0 mg·L-1范围内,H2PO-4、NO-3和Br-在0.05～150.0 mg·L-1范围内呈线性关系.6种离子的检出限(3S/N)均小于0.03 mg·L-1.该方法用于茶叶样品中F-、Cl-、Br-、NO-3、H2PO-4和SOi2-4的测定,加标回收率在90.9%～100.0%之间,测定值的相对标准偏差(n=5)小于3.5%.     

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%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

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.     

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.     

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.     

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.     

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.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.