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1.
周会 《色谱》2001,19(4):353-355
 利用AS4A SC分离柱 ,AG4A SC保护柱 ,ASRS Ⅱ抑制器 ,TAC 2阴离子富集柱和ATC 1阴离子捕集柱 ,以四硼酸钠 (Na2 B4O7)为淋洗液试剂 ,2 5mmol/LH2 SO4为化学抑制的再生液 ,采用梯度淋洗方式 ,对中国天山乌鲁木齐河源一号冰川雪冰中的生物有机酸和无机酸阴离子进行了测试分析。 2mL雪冰融水样品可在 16min内通过一次进样检测出氟离子、乙酸根离子、甲酸根离子、丙酮酸根离子、一氯乙酸根离子、氯离子、亚硝酸根离子、溴离子、硝酸根离子、磷酸根离子、硫酸根离子和草酸根离子共 10多种有机酸和无机酸阴离子。  相似文献   

2.
有机酸与无机阴离子的梯度离子色谱法分析研究   总被引:17,自引:0,他引:17  
刘  刘克纳  沈冬青  宋强  牟世芬  冯应升 《色谱》1997,15(4):334-337
研究了用离子色谱法梯度洗脱抑制电导检测器分析有机酸与无机阴离子的色谱条件,建立了最佳梯度程序。用阴离子交换分离,选用去离子水、氢氧化钠和甲醇作淋洗液,分别对5种二元有机酸和3种无机阴离子做二元梯度淋洗,对10种多元有机酸和3种无机阴离子做三元梯度淋洗。方法用于果汁饮料与柠檬酸发酵液的测定,结果令人满意。  相似文献   

3.
分析有机酸与无机阴离子的梯度离子色谱法   总被引:5,自引:1,他引:5  
利用梯度离子色谱法和抑制电导检测器对有机酸与无机阴离子的色谱分析条件进行了研究。建立了最佳梯度程序;通过浓缩柱的富集,可使方法的检出限达10^-2μg/L,各离子的相对标准偏差一般在5%以下;该法可用于火电厂水汽系统中的痕量低分子有机酸和无机阴离子的快速、准确分析,结果令人满意。  相似文献   

4.
施超欧  姚宝龙  胡咪  陈爱连 《色谱》2016,34(10):951-955
建立了离子转换色谱与紫外检测器联用检测啤酒中无机阴离子与有机酸的新方法。在传统的离子色谱基础上引入两根离子转换柱,无机阴离子与有机酸经过两步转换,定量转换成有相同紫外响应的碘酸盐,然后用紫外检测器代替电导检测器进行定量分析。在Dionex AS11-HC阴离子色谱柱上,采用KOH梯度淋洗方式实现了12种无机阴离子与有机酸的分离。结果表明,12种无机阴离子和有机酸检出限(S/N=3)与定量限(S/N=10)分别为6.168~29.01 μg/L与20.56~66.30 μg/L;线性关系良好(r在0.9994以上),回收率为89.0%~117.0%,RSD均小于1.0%,该方法与传统的电导检测器检测结果相当。该方法简单快捷,只需采用少数标准曲线,就可以实现啤酒中无机离子与有机酸的定量测定。  相似文献   

5.
饮料中有机酸和无机离子的离子色谱测定法   总被引:4,自引:3,他引:1  
朱岩  杨更生 《色谱》1990,8(1):43-45
离子色谱是一项对水溶液的电离物质色谱分析的技术,从70年代中期以来,这项技术运用愈来愈广泛,特别在食品分析方面有很快的发展。 有机酸和无机酸在碱性条件呈阴离子状态,往往可以用离子色谱法检测,但由于不  相似文献   

6.
离子交换色谱法同时测定啤酒中有机酸和无机阴离子   总被引:15,自引:2,他引:13  
建立了用亲水性阴离子交换分离柱,KOH为淋洗液等浓度泵作梯度淋洗,电导检测,同时分离和检测16种无机阴离子和低分子量有机酸的离子色谱法。方法对所测无机阴离子和有机酸检出限在9.3~32μg/L之间;线性范围均在2个数量级以上;回收率在90.2%~107.2%之间。方法用于啤酒样品的分析,结果满意,样品的RSD小于5.3%(n=7)。  相似文献   

7.
建立了高氯、高钠油田回注水中痕量无机阴、阳离子和有机酸的离子色谱分析方法。对高钠基质中痕量阳离子的测定,选用IonPac CS12A分析柱、H2SO4溶液梯度淋洗、电导检测器检测;对高氯基质中阴离子及有机酸的测定,选用对OH-具有高选择性的高容量的IonPac AS11-HC柱、KOH梯度淋洗、电导检测器检测。在优化的梯度淋洗条件下,高氯或高钠的存在不影响痕量阴离子或阳离子的测定。该方法具有良好的线性(r=0.9926~0.9990)和精密度(测定组分峰面积的相对标准偏差(n=7)在8.0%以下),回收率  相似文献   

8.
为了从用于油漆工业作分散剂或润湿剂的有机酸中,或者从用于塑料工业作缩合反应的H~+离子给予体的有机酸中除去无机酸,可用离子交换法来进行纯化。将阴离子交换剂(特别是带有三甲铵基团的二乙烯苯—苯乙烯树脂)用水溶胀,用将一有机溶剂流经树脂床的办法使有机相替代水相。将含  相似文献   

9.
于泓 《色谱》1998,16(1):18-21
 对单柱离子色谱法测定一价阳离子的流动相进行了系统研究,阐述了一价阳离子的保留行为和电导检测行为与流动相之间的关系,分别对无机酸(硝酸)、有机酸(柠檬酸)和芳香碱(苯胺)为流动相测定一价阳离子进行了讨论,其中有机酸和无机酸是较为适宜的流动相。  相似文献   

10.
有机酸和无机酸是食品中的重要组成之一,对食品的色、香、味有较大的影响;但由于以往没有快速、方便、和准确的测定方法,使研究受到限制。离子色谱是一种新兴的分析技术,由于通用、方便和准确,在食品分析领域正在得到应用。在此,我们用其对五香粉、辣椒粉的有机酸和无机酸进行了测定。  相似文献   

11.
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%.  相似文献   

12.
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   

13.
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   

14.
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   

15.
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.  相似文献   

16.
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   

17.
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.  相似文献   

18.
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   

19.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
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.  相似文献   

20.
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