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《化學試劑》2019年第5期中英文摘要

發布時間: 2019-05-08 16:37:46   試劑信息網

一種鈾酰配合物的合成、結構分析及對染料吸附性能的研究

王超

(寧波大學 材料科學與化學工程學院,浙江 寧波 315211)

 

摘要:在常溫下,采用UO2(Ac)2·2H2O與間甲氧基苯甲酸(HL)反應得到一例鈾酰配合物 ([(UO2)(DMSO)(L)2]2) (DMSO:二甲亞砜)。通過X射線單晶衍射分析配合物屬于三斜晶系,P-1空間群,a 10.744(2) ?,b 14.467(3) ?,c 14.632(3) ?,α 91.04(3) °,β 107.87(3) °,γ 94.59(3) °,V 2155.5(8) ?3,Dc 2.004 g/cm3,Z 2。U(VI)離子均為七配位的UO7五角雙錐構型。此外,研究了配合物對染料的吸附性能。結果表明,配合物對陽離子染料具有較好的吸附性能,其中對羅丹明B的最大吸附量達到249.87 mg/g,對陰離子染料的吸附幾乎可以忽略,說明配合物具有選擇性吸附陽離子染料的性能。

關鍵詞:鈾酰配合物;選擇性染料吸附;間甲氧基苯甲酸;陽離子染料

 

Synthesis, Structural Analysis and Adsorption Properties of the Uranyl Complex WANG Chao (School of Material Science and Chemical Engineering, Ningbo University, Ningbo 315211, China)

Abstract: UO2(Ac)2·2H2O Reacted with m-methoxybenzoic acid (HL) at room temperature to obtain the uranyl complex ([(UO2)(DMSO)(L)2]2). The crystal structure of the complex was characterized by single-crystal X-ray diffraction analysis. The crystallographic data are as follows: ([(UO2)(DMSO)(L)2]2) belongs to the triclinic with space group P-1, a 10.744(2) ?, b 14.467(3) ?, c 14.632(3) ?, α 91.04(3)°, β 107.87(3)°, γ 94.59(3)°, V 2155.5(8) ?3, Dc 2.004 g/cm3, Z 2, in which U(VI) ions show 7-fold coordination environment, demonstrating UO7 pentagonal bipyramidal geometries. In addition, the adsorption properties of ([(UO2)(DMSO)(L)2]2) towards organic dyes are investigated. The results show that ([(UO2)(DMSO)(L)2]2) has good adsorption performance for cationic dyes, and the maximum adsorption amount of rhodamine B (RhB+) is up to 249.87 mg/g, but the adsorption capacity to anionic dyes is negligible. These findings indicate that this uranyl complex possesses the excellent absorbing property towards cationic dyes.

Key words: uranyl complex; selective dye adsorption; m-methoxybenzoic acid; cationic dye

 

稀土-對苯二甲酸金屬有機骨架材料對剛果紅的高效吸附

付秋平*,王洋,田茂文,郭燕菊,劉芳,劉淵

(貴陽學院 化學與材料工程學院,貴州 貴陽  550005

 

摘要:以對苯二甲酸和硝酸鈰為原料,采用溶劑熱法合成Ce2(BDC)3(H2O)4。采用X-射線粉末衍射儀和紫外-可見分光光度計對樣品的物相及其對剛果紅的吸附性能進行了表征。探討了剛果紅初始濃度、吸附時間和背景離子對吸附量的影響。結果表明,Ce2(BDC)3(H2O)4對剛果紅的吸附量隨剛果紅初始濃度的增加而增大。在5 min內,吸附基本達到平衡。Li+、Na+、K+等背景離子均會嚴重影響吸附效果,Ce2(BDC)3(H2O)4對剛果紅的吸附符合Freundlich等溫吸附模型,吸附動力學符合二級動力學模型。

關鍵詞:金屬有機骨架;剛果紅;吸附

中圖分類號:O614.6   文獻標識碼:文章編號:0258-32832019


Highly Efficient Adsorption Capacity of Rare-earth 1,4-Benzenedicarboxylat Metal Organic Framework Material for Congo Red FU Qiu-ping, WANG Yang, TIAN Mao-wen, GUO Yan-ju, LIU Fang, LIU Yuan (College of Chemical and Material Engineering, Guiyang University, Guiyang 550005, China),Huaxue Shiji, 2019, 41(4),

Abstract: Terephthalic acid and cerium nitrate were used to synthesize Ce2(BDC)3(H2O)4 by using solvent heat method. The phase of the sample and the adsorption property of samples on Congo red were measured by X-ray powder diffraction and UV-visible spectrophotometer. The effects of initial concentration of Congo red, adsorption time and background ions on the adsorption capacity were investigated. The results show that, the adsorption capacity of Congo red onto Ce2(BDC)3(H2O)4 increased with increasing of initial concentration of Congo red. The adsorption basically reached the adsorption equilibrium within 5 min. The adsorption effect was seriously affected by the background ions, such as Li+, Na+, K+. The adsorption model of Ce2(BDC)3(H2O)4 for Congo red complies with Freundlich isotherm model and the adsorption kinetics complies with second-order kinetics.

Key words: metal organic frameworks; Congo red; adsorption

 

4-苯氨基喹啉化合物的合成及其與EGFRT790M分子對接研究

劉丹*,張昕旸,袁瑩,薛艾奇

(沈陽化工大學 制藥與生物工程學院,遼寧 沈陽  110142

 

摘要:6-(7-)-4--喹啉為原料與二苯胺經親核取代反應,得到4-(4’-氨基苯氨基)喹啉化合物,再與不同的?;噭┌l生?;磻?,得到12個未見文獻報道的化合物,結構經過ESI-MS確認。用Molegro Virtual Docker軟件完成與EGFRT790M的分子對接,并用Discovery Studio 2016 Client軟件分析化合物與EGFRT790M的作用模式。分子對接研究表明6--4-{4’-[4’’-甲氧基)-苯酰氨基]-苯氨基}-喹啉 1位的氮和4’位甲氧基上的氧分別與ARG A776HIS A850殘基形成兩個氫鍵。為開發EGFRT790M抑制劑提供基礎。

關鍵詞:酪氨酸激酶抑制劑;6-(7-)-4--喹啉;分子對接

中圖分類號:R914.5        文獻標識碼:A           文章編號:0258-32832019

 

Synthesis of 4-Phenylamino Quinoline Compounds and Molecular Docking Study with EGFRT790M LIU Dan*, ZHANG Xin-yang, YUAN Ying, XUE Ai-qi (College of Pharmaceutical and Biological Engineering, Shenyang University of Chemical Technology, Shenyang 110142, China), Huaxue Shiji, 2019

Abstract: 6-Fluoro(or 7-fluoro)-4-chloro-quinoline reacted with diphenylamine to give 4-(4'-aminophenylamino) quinoline compounds by nucleophilic substitution reaction. Acylation of 4-(4'-aminophenyl amino) quinoline compounds with different acylation reagents yields twelve novel compounds. The structure of the target compunds was confirmed by ESI-MS. Molecular docking was performed with Molegro Virtual Docker software, The interaction between compounds and EGFRT790M was analyzed by Discovery Studio 2016 Client software. The Molecular docking showed that N of 1 position and O of 4’ position of compound 1.4 give a hydrogen bond with ARG A776 and HIS A850, respectively. This work provides basis for developing EGFR T790M inhibitors.

Key words: Tyrosine Kinase Inhibitor; 6-fluorine(or 7-fluorine)-4-chlorine-quinolines; Molecular docking

 

金包覆的核殼結構納米材料的制備進展

吳睿*a,劉存芳a,張強a,宋娟a,郭鴻b,熊海濤a,田光輝a

(陜西理工大學 a. 化學與環境科學學院 陜西省催化基礎與應用重點實驗室;

b. 土木工程與建筑學院,陜西 漢中  723000 )

摘要: 金、銀等貴金屬納米材料具有獨特的光學、電學和催化性能以及良好的生物兼容性,其在化學、物理、生物和醫學等領域具有廣泛的應用。以貴金屬納米金作為核或者作為殼,制備成核殼結構復合納米材料,這樣的核殼材料同時具有核和殼的性質以及其它優越的性能,因此受到研究者的廣泛青睞。金包覆納米顆粒制備核殼結構的方法眾多,主要對金包覆所形成的核殼型納米材料的制備方法進行綜述。

關鍵詞: 金;核殼結構;包覆;制備

中圖分類號:O654.2        文獻標識碼:A               文章編號:0258-3283(2019)

 

Preparation of Core-shell Structure of Au Coating Nanocomposites WU Rui*a, LIU Cun-fang a, ZHANG Qianga, SONG Juana, GUO Hongb, XIONG Hai-taoa, TIAN Guang-huia (a. Shaanxi key laboratory of catalysis and application, College of Chemical and Environment Science, b. College of Civil Engineering and Architecture, Shaanxi University of Technology, Hanzhong 723000, China ), Huaxue Shiji, 2019

Abstract: Au, Ag and other precious metal nanomaterials(NPs) have been widely used in the fields of chemistry, physics, biology and medicine due to their unique optical, electrical, catalytic properties and good biocompatibility. Au NPs are employed as core or shell to prepare core-shell type of composite NPs, which are widely favored by researchers. Such core-shell NPs endow with both the performance of core and shell, as well as other superior properties, there are many methods for preparing core-shell structure with Au coating NPs. In this work, the methods for preparing core-shell NPs with Au coating was reviewed.

Key words: Au; shell structure; coating; preparation

 

腙參與的環加成反應研究進展

杜佳,閆文靜,馮濤,李興,常宏宏,高文超,魏文瓏*

(太原理工大學 化學化工學院,山西 太原  030024)

 

摘要:環加成是兩個或多個分子通過結合生成環狀化合物的反應,它在有機合成中起著非常重要的作用。腙是一類重要的有機含氮化合物,作為有機合成中間體,它可與含有各種不飽和鍵的化合物發生不同類型的環加成反應來制備多種含氮雜環化合物;這些雜環化合物骨架廣泛存在于醫藥、農藥、材料和天然產物等分子結構中。主要對近幾年腙與含有各種不飽和鍵化合物發生的各種環加成反應進行了綜述,主要包括[3+3]、[3+2]、[3+4]、[4+2][4+3]等環加成反應,并對其發展方向進行了展望。

關鍵詞:腙;環加成;不飽和鍵

中圖分類號: 0626 文獻標識碼:A文章編號:0258-32832019

 

Progress in Cycloaddition Reactions of Hydrazones DU Jia,YAN Wen-jing,FENG Tao,LI Xing,WEN Wen-long* (College of Chemistry Engineering, Taiyuan University of Technology, Taiyuan 030024, China) Huaxue Shiji, 41(5), ~

AbstractCycloaddition is the formation of a cyclic compound via the reaction of two or more molecules, and it plays a very important role in organic synthesis. Hydrazones are very important nitrogen-contain compounds and they could react with various compounds having diverse unsaturated bonds to synthesize different nitrogen-contain heterocyclics. And these heterocyclic skeletons are widely presented in the molecular structure of medicine, pesticides, materials and natural products. The recent progress in the cycloadditions of hydrazones with diverse compounds mainly bearing various unsaturated bonds is summarized, including [3+3], [3+2], [3+5], [4+2] and [2+3] cycloaddition. Moreover, the prospects of future development are also discussed.

Key wordshydrazone; cycloaddition; unsaturated bonds

 

甲醇中克倫特羅、萊克多巴胺和沙丁胺醇3種溶液標準物質的定值及不確定度評估

周劍,齊鑫,楊夢瑞,王彤彤,王敏*

(中國農業科學院農業質量標準與檢測技術研究所,北京  100081)

 

摘要:采用有證標準物質和市售純品為標準物質原料,經過定性和純度核驗的研究,采用重量-容量法配制了甲醇中克倫特羅、萊克多巴胺和沙丁胺醇3種溶液標準物質,經均勻性和穩定性檢驗合格,并進行了定值、均勻性和穩定性的不確定度評估。3種溶液以配制值為發布值,已被批準為國家二級標準物質,標準物質的研制為農產品質量安全相關項目的監測與風險評估提供了溯源保障。

關鍵詞:克倫特羅;萊克多巴胺;沙丁胺醇;溶液標準物質          

中圖分類號:O625      文獻標識碼:A      文章編號:0258-32832019--

 

Determination and Uncertainty Evaluation of Clenbuterol, Ractopamine and Salbutamol in Methanol Solution ZHOU Jian, QI Xin, YANG Meng-rui, WANG Tong-tong, WANG Min* (Institute of Quality Standard and Testing Technology for Agro-Products of CAAS, Beijing 100081, China) Huaxue Shiji, 2019, 41(5), ~

AbstractThe certified reference material and pure products after qualitative and purity verification were used in this study. The clenbuterol, ractopamine and salbutamol in methanol solution were prepared by a gravity-volume method, then were investigated homogeneity study, stability study and uncertainty evaluation. Finally, 100 mg·L-1 clenbuterol, ractopamine and salbutamol in methanol have been approved as the national secondary standard materials, which could provide traceability for the program of monitoring and risk assessment of agricultural product.

Key wordsclenbuterol; ractopamine; salbutamol; solution reference material

 

混合磷酸鹽pH溶液標準物質的研制

周瑾艷1,黃彥捷*1,許俊斌1,陳玲1,王世超1,花秀兵1,尹強1,吳朝陽2

1.廣東省計量科學研究院華南國家計量測試中心,廣東 廣州  510405;2.湖南大學 化學化工學院, 湖南 長沙  410000

 

摘要:通過遴選標準物質原材料,優化特性量值測量方法,采用溯源至美國國家標準與技術研究院(NIST)研制的標準物質的定值方法,系統介紹了混合磷酸鹽pH溶液標準物質的研究工作。同時考察了標準物質的均勻性和穩定性,分析了樣品的均勻性、測量的分散性及其他因素對不確定度的貢獻,綜合評定了整個研制體系的不確定度。穩定性考察結果表明,混合磷酸鹽pH溶液標準物質在6個月內量值可靠穩定。其pH值為7.4125 ℃),pH的擴展不確定度為0.03pH。該系列標準物質性能良好,已成功申請國家二級標準物質,編號為GBW(E)130522,可滿足食品、藥品、日化、環境保護及化工產品研究和檢測的需要,可望用于相關儀器(pH計)的校準、分析方法評價,為統一相關量值發揮應有的作用。

關鍵詞:標準物質、pH、混合磷酸鹽、不確定度

中圖分類號:TB99       文獻標識碼:A       文章編號:0258-32832019--

 

Development of Certified Reference Material for Mixed Phosphate pH Solution ZHOU Jin-yan1, HUANG Yan-jie*1, XU Jun-bin1, CHEN Ling1, WANG Shi-chao1, HUA Xiu-bin1, YIN Qiang1, WU Zhao-yang2 (1.Guangdong Provincial Institute of Metrology & South China National Centre of Metrology, Guangzhou 510405;2. College of Chemistry and Chemical Engineering, Hunan University, Changsha, 410000) Huaxue Shiji, 2019, 41(5), ~

AbstractThe research work of the certified reference material of mixed phosphate pH solution was systematically introduced by selecting the raw material, optimizing the measurement method of characteristic quantity value, and adopting the determination method of certified reference material traceable to the reference material from American National Institute of Standards and Technology (NIST). The uniformity and stability of the certified reference materialwere investigated, the uniformity of the sample, the dispersion of the measurement and the contribution of other factors to the uncertainty were analyzed, and the uncertainty of the whole system was comprehensively evaluated.The results show that the certified reference material of the mixed phosphate pH solution was reliable and stable in 6 months.The pH value is 7.41 at 25 ℃ with the expanded uncertainty of 0.02pH.Thesolution reference materialshas been successfullyidentified as the national grade II certified reference materials, which is numbered GBW(E)130522, and is expected to be used in the calibration of instruments(pH meter) and method evaluation in food and cosmetic analysis.

Key wordsreference materials;b pH; mixed phosphate; uncertainty

 

 

質量控制圖在標準物質穩定性評估中的應用

汪斌*,盧曉華,王茜

(中國計量科學研究院,北京  100029

 

摘要:標準物質穩定性評估是標準物質研制的一個重要環節,目的是評估標準物質量值在一定時間內的波動情況,并據此給出標準物質有效期。常用的方法是線性回歸趨勢分析和方差分析法。根據質量控制圖的特點及標準物質穩定性評估的實際需要,探索將質量控制圖應用于標準物質量值的穩定性監測與評估工作中。通過對比發現,質量控制圖具有靈敏直觀的特點,可以作為標準物質穩定性評估的一個有效手段。

關鍵詞:質量控制圖;穩定性評估;標準物質

中圖分類號:TB9x         文獻標識碼:A            文章編號:0258-32832019--

 

The application of control chart for assessment of stability of reference materials WANG Bin*,LU Xiao-hua, WANG Qian (National Institute of Metrology, Beijing 100029, China) huaxue shiji, 2019, 41(5),

Abstract: The assessment of stability of reference materials is an important stage of the development. The aim of assessment of stability is to demonstrate the changes of the values, and give the period of validity for reference materials. The common methods are trend analysis by least squares regression and variance analysis. Control chart will be used in the assessment of stability. By the comparison, it can be found that control chart is very sensitive and intuitive. Control chart can be a useful method for the assessment of stability.

Key words: control chart, assessment of stability, reference materials metrology

 

質量平衡法測定金屬銀純度的不確定度評定

田衎,岳亞萍,楊永*,張覃,郭偉臣,邢書才,房麗萍

(環境保護部標準樣品研究所 國家環境保護污染物計量和標準樣品研究重點實驗室,北京  100029)

 

摘要:采用質量平衡法對金屬銀純度定值。選擇電感耦合等離子體質譜法(ICP-MS)測定了金屬銀中9種痕量金屬雜質含量,按照《CNAS-GL0062018化學分析中不確定度的評估指南》中有關規定分別評定了9種金屬雜質的不確定度,不確定度主要來源于樣品稱量、標準溶液和樣品稀釋制備、工作曲線擬合及測量重復性等,以9種雜質的合成不確定度分量作為金屬銀純度的不確定度。金屬銀純度定值結果為99.637%,擴展不確定度為 0.025% (k 2 )。

關鍵詞:質量平衡法;金屬銀;不確定度評定

中圖分類號:O655.1        文獻標識碼:A            文章編號:0258-3283(2019)

 

Uncertainty Evaluating of Metallic Silver by Mass Balance Method TIAN Kan, YUE ya-ping, YANG yong*, ZHANG qin, GUO Wei-chen, XING Shu-cai, FANG Li-ping (Institute for Environmental Reference Materials of Ministry of Environmental Protection, State Key Laboratory of Environmental Pollutant Metrology and Reference Materials of Environmental Protection, Beijing 100029, China) Huaxue Shiji, 41(5),

Abstract: The purities of metallic silver were analysis by mass balance method. The 9 trace impurities in metallic silver were determined by inductively coupled plasma mass spectrometry (ICP-MS) and the uncertainty evaluation for the results were carried out according to CNAS-GL0062018 Guidance on Evaluating the Uncertainty in Chemical Analysis. The main sources of measurement uncertainties were analyzed, including sample weighing,diluting standard solution,standard curve fitting and measurement repeatability, etc. The standard uncertainty of 9 elements and the combined extending uncertainty of silver were evaluated respectively. The certified result with the mass balance method was 99.637% and the expanded uncertainty was 0.025% ( k 2 ).

Key words: mass balance method; metallic silver; uncertainty evaluation

 

12種氯苯類化合物純度定值色譜方法研究

紀潔*,張偉,何雅娟

(中國計量科學研究院 化學所,北京  100029

 

摘要:對用于溶液標準物質制備的12種氯苯類純品原料進行了高效液相色譜法(HPLC-DAD)和氣相色譜法(GC-FID)兩種純度定值方法的研究。在優化的色譜條件下,甲醇基體混合溶液中的12個目標物組分包含一氯代苯、1,2-二氯苯、1,4-二氯苯、1,3-二氯苯、1,2,3-三氯苯、1,2,4-三氯苯、1,3,5-三氯苯、1,2,3,4-四氯苯、1,2,4,5-四氯苯、1,2,3,5-四氯苯、五氯苯、六氯苯均能良好分離。避免了氯苯類原料中存在的同分異構體及同系物雜質與主體成分沒有良好分離而導致的對純度定值結果的影響。

關鍵詞:氯苯類;純度;高效液相色譜;氣相色譜;標準物質

中圖分類號:O625.2    文獻標識碼:A     文章編號:0258-3283 (2019)--

 Purity Measurement for 12 Kinds of Chlorobenzenes via Chromatography JI Jie*, ZHANG Wei, HE Ya-juan (Chemical Metrology & Analytical Science Division, National Institute of Metrology, Beijing 100029, China), Huaxue Shiji, 2019, 41(5), ~

Abstract:The research of purity chromatography measurement method HPLC-DAD and GC-FIDfor 12 kinds of chlorobenzenes raw materials which were used to prepare chlorobenzenes solution reference material was introduced. It contains monochlorobenzene, 1,2-dichlorobenzene, 1,4-dichlorobenzene, 1,3-dichlorobenzene 1,2,3-trichlorobenzene, 1,2,4-trichlorobenzene, 1,3,5-trichlorobenzene, 1,2,3,4-tetrachlorobenzene, 1,2,4, 5-tetrachlorobenzene, 1,2,3,5-tetrachlorobenzene, pentachlorobenzene and hexachlorobenzene. Under optimized chromatographic conditions, good chromatographic separation result was gotten for 12 chlorobenzenes target compounds which were in methanol matrix mixed solution. It avoided the influence of the impurities of isomers and homologues in the raw materials on the results of purity determination due to the poor separation between the impurities and the target compounds.

Key words: chlorobenzenes; purity; high performance liquid chromatography; gas chromatography; reference material

 

模擬汽油餾程標準物質的研制

裴從瑩1,王海峰*2,葉青1,李佳2,宋小平2

(1.北京工業大學 環境與能源工程學院,北京 100022;2.中國計量科學研究院 環境計量中心,北京 100029)

 

摘要:餾程反映了液體的蒸發性能,是有機溶劑、原油及石油產品的重要的技術指標之一。針對國內外對餾程標準物質的迫切需求,研制了模擬汽油餾程標準物質。采用十氫化萘等8種有機物混合物為基體,在劇烈攪拌條件下連續分裝,制備了標準物質?;凇?/span>GB/T 6536 石油產品常壓蒸餾特性測定法》系統研究了方法的影響因素?;诩兾镔|的沸點,采用比較法將自動餾程測定儀的鉑電阻溫度計溯源到了水銀溫度計,實現了溫度的量值溯源。聯合多家權威實驗室,采用國家標準方法為標準物質合作定值。標準物質的蒸發溫度不確定度在1.3 3.4 ℃范圍內。該標準物質可用于餾程測定儀的檢定和校準以及汽油餾程測定方法的驗證。

關鍵詞:餾程;標準物質;不確定度;汽油         

中圖分類號:O657.99       文獻標識碼:A       文章編號:0258-32832019--

 

Development of Certified Reference Material of Synthetic Gasoline for Distillation PEI Cong-Ying1, WANG Hai-Feng*2, YE Qing1, LI Jia2, SONG Xiao-Ping2 (1.college of environmental and energy engineering, Beijing University of Technology 100022, China; 2.centre of environmental metrology, National institute of metrology of China, Beijing 100029) Huaxue Shiji, 2019, 41(5), ~

AbstractDistillation is one of important properties of organic solvent, crude oil and its products which reveals the evaporating performance of samples. The present study developed the certified reference material (CRM) of synthetic gasoline for distillation in order to satisfy the urgent need of CRM. The mixture of 8 organic solvent including naphthene was employed as the matrix of CRM which is dispensed continuously under vigorous stirring for the preparation of CRM. Based on the national standard method for distillation of petroleum products and liquid fuels at atmospheric pressure (GB/T 6536), various effects upon the distillation were investigated. The platinum resistance thermometer of distillation analyzer was calibrated by the mercury thermometer through the boiling point of toluene, which realized the traceability of temperature of distillation to SI unit. The collaborative-study was used to certify the CRM using the national standard method above. The uncertainty of the certified temperature of evaporated volume of CRM ranged from 1.3 ℃ to 3.4 ℃. This CRM can be employed in the verification and calibration of distillation analyzer, and the validation of measurement method of distillation.

Key wordsdistillation; reference material; uncertainty; gasoline

 

 

水中3種苯胺類混合標準樣品的研究初探

劉海萍,黃林艷,趙亞嫻,房麗萍*

(環境保護部標準樣品研究所 國家環境保護污染物計量和標準樣品研究重點實驗室,北京  100029)

 

摘要:探索了水中苯胺、對硝基苯胺和間硝基苯胺多組份混合標準樣品的制備技術。本實驗從制備介質、參比波長、流動相、穩定劑、保存條件等方面進行探索,結果表明,采用重組法制備水中3種苯胺類混合標準樣品在SDB-C18型液相色譜柱、甲醇-水混合溶液為流動相的液相色譜儀上分離度良好;分層隨機抽取10瓶樣品進行瓶間均勻性檢驗,經單因素方差分析法統計,證明樣品均勻性良好;將室溫避光和4 ℃冷藏避光保存的樣品進行穩定性檢驗,經趨勢分析法計算,其線性直線的斜率均不顯著,表明在180 d的監測期內,室溫避光和4 ℃冷藏避光保存條件下的樣品穩定性均良好。本方法為后續開展水中有機物標準樣品的研制提供了參考和借鑒價值。

關鍵詞:水;苯胺類;標準樣品;初探

中圖分類號:N023    文獻標識碼:A    文章編號:0258-3283(2019)--

 

Anilines in Water Reference Material LIU Hai-ping1, HUANG Lin-yan1, ZHAO Ya-xian1, FANG Li-ping*1 (State Environmental Protection Key Laboratory of Measurement and Reference Material, Institute for Environmental Reference Materials, Beijing 100029, China), Huaxue Shiji, 2019, 41(5), ~ Abstract: The preparation method of anilines in water reference material was introduced, including aniline, p-nitroaniline and m-nitroaniline. It was prepared by the method of a spiking solution added to water, and factors in the process of preparation were investigated, such as preparation medium, reference wavelength, mobile phase, stabilizer, preservation conditions, et.al. The result showed that anilines in water had a good resolution on the liquid chromatograph with SDB-C18 column, using methanol and water as mobile phase. 10 units selected by random stratified sampling coving the whole batch were obtained for homogeneity, and indicated good homogeneity using one-way analysis of variance. At ambient and 4℃ refrigeration storage conditions, the concentration of anilines did not change during monitoring period of 180 d. At the same time, trend analysis method was used for the stability data, and its linear slope was not significant, indicating good stability. This method provides reference for the subsequent development of organic compounds in water reference material.

Key words: water; Anilines; reference material; preliminary research

 

熒光光譜儀的校準方法研究及不確定度評定

黃彥捷1,李成輝2,周瑾艷1,黃振宇1,陳玲1,王鑫3,關妍*3

(1.廣東省計量科學研究院,廣東 廣州  510405;2.四川大學 分析測試中心,四川 成都  610064;3.北京大學 化學與分子工程學院,北京  100871)

 

摘要:熒光光譜儀是一種常用的分析儀器,適用于食品、衛生、農業、環境等方面的樣品分析,能提供被測樣品的激發光譜、發射光譜、熒光強度、量子產率、熒光壽命及熒光偏振等一種或多種信息。介紹適用于檢測波長范圍為200 1700 nm的熒光光譜儀的校準方法,針對波長示值誤差和重復性、檢出限、測量線性及峰值強度重復性給出了校準實例和不確定度評價方法。其中波長示值誤差的擴展不確定度為0.20 nm (k 2);檢出限為8.09×10-11 g/mL,其擴展不確定度為3.60×10-11 g/mL (k 2);測量線性的相對擴展不確定度為3.1% (k 2);峰值強度重復性的相對擴展不確定度為2.0% (k 2)。熒光光譜儀的校準過程及結果評價的描述將為相關儀器的校準提供一個良好的范例。

關鍵詞:熒光光譜儀;不確定度;波長;檢出限;測量線性;峰值強度;校準

中圖分類號:TB99      文獻標識碼:A      文章編號:0258-32832019--

 

Study on Calibration Method of Fluorescence Spectrometer and Evaluation of Uncertainty HUANG Yan-jie1, LI Cheng-hui2, ZHOU Jin-yan1, HUANG Zhen-yu1, CHEN Ling1, WANG Xin3, GUAN Yan*3 (1.Guangdong Provincial Institute of Metrology, Guangzhou 510405, China; 2.Analytical Instrumentation Center, Sichuan University, Chengdu 610064, China; 3.College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China) Huaxue Shiji, 2019, 41(5), ~

AbstractFluorescence spectrometer is a common analytical instrument, which is suitable for the analysis in food, health, agriculture and environment areas. It can provide one or more information such as excitation spectrum, emission spectrum, fluorescence intensity, quantum yield, fluorescence lifetime, and fluorescence polarization. The calibration methods and uncertainty evaluation methods for fluorescence spectrometer with detection wavelength ranging from 200 nm to 1700 nm are introduced, which containing wavelength indication error and repeatability, detection limit, measurement linearity and peak intensity repeatability. The expanded uncertainty of wavelength indication error is 0.20 nm (k 2); the limit of detection is 8.09×10-11 g·mL-1 with an expanded uncertainty to be 3.60×10-11 g·mL-1 (k 2); the relative expanded uncertainty of measurement linearity is 3.1% (k 2); the relative expanded uncertainty of peak intensity repeatability is 2.0% (k 2). The calibration process and result evaluation of fluorescence spectrometer described in this paper will provide a good example for calibration of related instruments.

Key wordsfluorescence spectrometer; uncertainty; wavelength; limit of detection; measurement linearity; peak intensity; calibration

 

新型進樣瓶-氣相色譜質譜法測定煙葉中的24種有機酸

劉欣1,梁夢潔2,李銀科1,王燕梅1,米其利1,孔維松1,許永1,李晶*1

(1.云南中煙工業有限責任公司 技術中心,云南 昆明  650106;2.昆明醫科大學 藥學院,云南 昆明 650504)

 

摘要:研發建立了一個新型進樣瓶,結合氣相色譜質譜法(GC-MS)可以測定煙葉中的24種有機酸。結果表明:新型進樣瓶可以集提取、過濾、干燥、衍生化反應和進樣功能為一體,在一定程度上減少操作步驟,縮短前處理時間,可以保障樣品檢測的平行性和穩定性;利用新型進樣瓶,以二氯甲烷為提取劑,N,O-(三甲基硅烷基)三氟乙酰胺(BSTFA)為衍生化試劑,將提取液在40 ℃下反應60 min,衍生化后的樣品利用氣相色譜質譜法,選擇離子模式進行檢測。該方法在0.5 50 mg/L范圍內,線性關系較好(R > 0.99),檢出限為0.1 6.8 μg/g,加標回收率在85% 104%之間,相對標準偏差在1.1% 5.1%之間;利用該方法對不同生長期的煙葉進行檢測,發現有機酸物質具有差異性。該方法操作簡易、重復性好、準確度高,可以滿足煙草及相關樣品中有機酸的檢測要求。

關鍵詞:煙葉;有機酸;氣相色譜質譜法(GC-MS);新型進樣瓶

中圖分類號:O657.61   文獻標識碼:A    文章編號:0258-32832019--

 

Determination of 24 Organic Acids in Tobacco Leaf via Novel Sampling Bottle-gas Chromatography-mass Spectrometer (GC-MS) for the LIU Xin1, LIANG Meng-jie2, LI Yin-ke1, WANG Yan-mei1, MI Qi-li1, KONG Wei-song1, XU Yong1, LI Jing*1 (1. Technology Center, China Tobacco Yunnan Industrial Co., Ltd, Kunming 650106, China; 2. School of Pharmacy, Kunming Medical University, Kunming 650504, China), Huaxue Shiji, 2019, 41(5),

AbstractA novel sampling bottle was developed to couple with gas chromatography-mass spectrometer (GC-MS) for the determination of 24 organic acids in tobacco leaf. The results show that: the pretreatment including extraction, filtering, removing the water, derivation and sampling could be finished in one step by the novel sampling bottle, which can make the procedure simpler, timesaving and having good repeatability; based on the pretreatment device, the tobacco leaf sample was extracted by dichloromethane, then derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide under 40 for 60 min. The separation of 24 organic acids including formic acid, acetic acid, etc., was performed by GC-MS on selected ion mode. In the range of 0.550 mg/L, the linearity was acceptable (correlation coefficients R > 0.99). The spiked recoveries of real sample were 85%104% with the RSD in the range of 1.1%5.1%; With the established test method, different contents of organic acids in different type tobacco leaf were found. With the simplification, good reproducibility, proper accuracy, the developed method can be used for the determination of 24 organic acids in tobacco samples.

Key words: tobacco leaf; organic acids; gas chromatography- mass spectrometer (GC-MS); novel sampling bottle

 

共振光散射光譜法應用于甲氨蝶呤的定量測定

劉小蓮1, 2,張傳林*1

(1.江西醫學高等??茖W校第一附屬醫院 藥劑科,江西 上饒 334000;2.江西醫學高等??茖W校 藥劑科,江西 上饒 334000

摘要:建立測定甲氨蝶呤含量的方法。在pH 12Britton-Robinson緩沖液中,形成n(甲氨蝶呤): nHg(): n(氯化十六烷基吡啶) = 1 : 1 : 4的離子締合物,引起吸收光譜和共振光散射光譜的明顯變化,最大散射峰位于464 nm處。研究表明,體系散射強度的增加與甲氨蝶呤的濃度在一定范圍內有良好的線性關系,其檢出限為11 ng/mL。甲氨蝶呤片和尿液中甲氨蝶呤的平均回收率分別為97.9%88.6%,相對標準偏差分別為3.3%3.6%n = 6)。該方法靈敏、快速,可用于甲氨蝶呤的定量測定。

關鍵詞:甲氨蝶呤;Hg();氯化十六烷基吡啶;共振光散射

中圖分類號:O657.39      文獻標識碼:A      文章編號:0258-3283(2019)--

 

Determination of Methotrexate by Resonance Light Scattering Spectra LIU Xiao-lian1,2, ZHANG Chuan-lin*1(1. Department of Pharmacy, the First Affiliated Hospital of Jiangxi Medical College, Shangrao 334000, China; 2. Department of Pharmacy, Jiangxi Medical College, Shangrao 334000, China), Huaxue Shiji, 2019, 41(4)     

Abstract: To establish a method for determination of methotrexate(MTX), in a Britton-Robinson buffer medium (pH 12.00), methotrexate reacted with Hg() and cetylpyridinium chloride(CPC) to form a 1:1:4 ion-associated complex, which resulted in the change of absorption spectra and resonance light scattering(RLS) spectra. The maximum scattering peak was located at 464 nm. The increment of the enhancement of RLS was linear to the concentration of methotrexate in a certain range. The limit of detection was 11 ng/mL. The average recoveries of methotrexate in tablets and the urine were 97.9% (RSD = 3.3%, n = 6), 88.6% (RSD = 3.6%, n = 6). The method was quick and sensitive, and could be applied in the determination of methotrexate.

Key words: methotrexate; Hg(); cetylpyridinium chloride; resonance light scattering

 

 

重量法測定二乙基次膦酸鋁磷含量的研究

楊麗a,毛祖莉*b

(湖南工學院 a.安全與環境工程學院,b.汽車零部件技術研究院,湖南 衡陽  421002

 

摘要:為了建立二乙基次膦酸鋁(AlPi)中磷含量的分析方法,采用磷鉬酸喹啉沉淀法(重量分析法),分別探討氧化劑過硫酸銨的添加量、喹鉬檸酮試劑添加量、過濾時采用砂芯漏斗規格等檢測條件對磷測定值的影響。結果表明,試樣為0.1 0.2 g,過硫酸銨添加量為2.5 g,喹鉬檸酮體積為30 mL,選擇G4規格的砂芯漏斗過濾時,其結果與理論值更接近,通過精密度試驗,精確度高,準確度好,加標回收率為98.84% 99.34%,較儀器分析更接近理論值,適用于AlPi產品磷含量的檢測。

關鍵詞:二乙基次膦酸鋁;磷含量;磷鉬酸喹啉;過硫酸銨;

中圖分類號:O622.4      文獻標識碼:A      文章編號0258-3283(2019)--

 

Determination of Phosphorus in Aluminum Diethylphosphinate by Gravimetric Method YANG Lia, MAO Zu-li*b (a. School of Safety and Environmental Engineering, b. Research Institute of Automobile Parts Technology, Hunan Institute of Technology, Hengyang 421002, China),Huaxue Shiji, 2019, 41(4)     

Abstact: To establish an analytical method for phosphorus content in aluminum diethylphosphinate (AlPi), the quinolinephosphomolybdate precipitation method (gravimetric analysis) was adopted to investigate and discuss the influence on the measured value of phosphorus by the addition amount of oxidant ammonium persulfate, quinoxalyl ketone reagent, and the specifications of sand core funnel during the filtration. The results suggested: when the sample weighed between 0.1 0.2g, the additional amount of ammonium persulfate added was 2.5 g, and the volume of quimociac was 30 mL, and the result was closer to the theoretical value when the sand core funnel of G4 size was selected for filtration. The precision test suggested that this method had high precision and good accuracy, with the recoveries of the standard addition between 98.84%99.34%, which was closer to the theoretical value than the instrumental analysis, making it suitable for the detection of phosphorus content in AlPi products.

Key words: aluminum diethylphosphinate; phosphorus content; quinolinemolybdophosphoric acid; ammonium persulfate

 

 

硫醇還原α, α, α-三溴甲基酮類化合物的研究

王慧,楊瑩,阿布都熱西提·阿布力克木*

(新疆師范大學 化學系,新疆 烏魯木齊  830000)

 

摘要報道了一種合成α, α-二溴甲基酮類化合物的新方法,該反應以硫醇作為還原劑,高效還原α, α, α-三溴甲基酮類化合物為目標化合物,合成了12α, α-二溴甲基酮類化合物,該方法適用于脂肪族、芳香族和雜環類α, α, α-三溴甲基酮類化合物。最佳的反應條件是nα, α, α-三溴甲基酮):n(還原劑):n(碳酸鉀)=121.2,二氯甲烷中0 ℃反應1 h,α, α-二溴甲基酮類化合物收率達81% 96%。其結構通過1HNMR、13CNMR、HR-MS 進行了表征和確認。該反應條件溫和、操作簡單、效率高,為α,α-二溴甲基酮類化合物的合成提供了新途徑。

關鍵詞 2-苯硫代乙醇;α, α-二溴甲基酮;還原反應;α, α, α-三溴甲基酮

中圖分類號:O622.4       文獻標識碼:A       文章編號:0258-32832019--

 

Reduction of α,α,α-Tribromomethylketones by Mercaptan Wang Hui, YANG Ying, ABULIKEMU Abudu Rexit (Department of Chemistry, Xinjiang Normal University, Urumqi, 830054,China), Huaxue Shiji, 41(5), ~

Abstract A new method for synthesizing α, α-dibromomethylketones is reported. This reaction uses thiol as a reducing agent to efficiently reduce α, α, α-tribromomethylketones as target compounds. 12 Kinds of α, α-dibromomethyl ketone compounds were suitable for aliphatic, aromatic and heterocyclic α, α, α-tribromomethyl ketones. The optimum reaction conditions are n(α, α, α-tribromomethylketone): n (reducing agent): n (potassium carbonate) 1:2: 1.2, and reacted in dichloromethane at 0 ° C for 1 h, The yield of α, α-dibromomethyl ketone compound is 81% 96%. The structure was confirmed by 1H NMR, 13C NMR, HR-MS. The protocol features mild conditions, simple operation and high efficiency, providing a new approach for synthesizing α,α-dibromomethylketones.

Key words: 2-phenylthioethanol; α,α-dibromomethylketones; reduction; α,α,α-tribromomethylketones

 

三氟甲磺酸鉍催化的Beckmann重排反應在酰胺類化合物

合成中的應用研究

陳琦,呂春欣*,呂亞維,朱冰冰,余蕙敏,裘超穎,劉陽

(嘉興學院 生物與化學工程學院,浙江 嘉興  314001)

 

摘要:發展了一種利用三氟甲磺酸鉍(Bi(OTf)3)催化Beckmann重排反應。以三氟甲磺酸鉍為催化劑,通過Beckmann重排反應制備酰胺類化合物??疾炝舜呋瘎?、溶劑、溫度、催化劑用量、反應時間等對Beckmann重排反應的影響。結果表明,結構對稱的酮肟底物相對于不對稱底物更容易發生Beckmann重排反應。結構中含有—OCH3、—CH3等供電子基團的底物,則底物活性更高。對酰胺類化合物進行核磁、紅外表征。

關鍵詞:酮;肟;酰胺;催化;Beckmann重排反應

中圖分類號:O614.53+2    文獻標識碼:A    文章編號:0258-32832019--

 

Application of Beckmann Rearrangement Reaction Using Bi(OTf)3 as the Catalyst in the Synthesis of Amide Compounds CHEN Qi, LV Chun-xin*, LV Ya-wei, ZHU Bing-bing, YU Hui-min, QIU Chao-ying, LIU Yang (College of Biological and Chemical Sciences and Engineering, Jiaxing University, Jiaxing 314001, China), Huaxue Shiji, 2019, 41(5),

Abstract: A Beckmann rearrangement reaction using Bi(OTf)3 as the catalyst was developed. A series of amide compounds were synthesized by Beckmann rearrangement reaction using Bi(OTf)3 as the catalyst. The effects of catalyst, solvent, temperature, catalyst amount and reaction time on the rearrangement of Beckmann were investigated. The results show that the structural symmetric ketoxime substrates are more likely to undergo Beckmann rearrangement reaction than asymmetric substrates. Substrates containing -OCH3, -CH3, etc. groups in the structures have higher activity. The amide compounds were comprehensively confirmed  by NMR and IR.

Key words: ketone; oxime; amide; catalysis; Beckmann rearrangement reaction

 

 

三氯化鋁-氯化鋰體系中5-取代-1-茚酮化合物的合成研究

潘繼剛*,張光輝,姚兵,陶勇凱

(山西大學 化學化工學院,山西 太原  030031

 

摘要:茚酮類化合物不僅廣泛存在于天然產物中,而且在藥物研發、殺蟲劑等方面有廣闊的應用前景。本研究工作以3-氯丙酰氯及取代苯(Cl-、Br-、CH3-CH3O-)為原料,通過路易斯酸催化,先后經過付克?;?、付克烷基化來合成相應的5-取代-1-茚酮化合物(Cl-、Br-、CH3-HO-)。優化了這類化合物的合成條件,選擇新型的AlCl3-LiCl熔鹽體系作為付克烷基化的路易斯酸催化劑和反應溶劑,大大提高了茚酮類化合物的合成產率,總收率可達到77% 82%。目標化合物的結構通過核磁共振分析確定。

關鍵詞5-取代-1-茚酮;付克反應;AlCl3-LiCl熔鹽;路易斯酸催化劑

中圖分類號O621.3        文獻標識碼      文章編號0258-32832019

 

Synthesis of 5-Substituted-1-indanone in AlCl3-LiCl Systems PAN Ji-gang*, ZHANG Guanghui, YAO Bing, TAO Yong-kai (School of Chemistry and Chemical Engineering,Shanxi University,Taiyuan 030031,China), Huaxue Shiji, 2019, 41(5),

Abstract: Indanone compounds not only exist widely in natural products, but also have broad application prospects in drug development, insecticides and so on. With 3-chloroacetic chloride and substituted benzeneCl—, Br—, CH3— and CH3O—as raw materials, 5-substituted-1-indanoneCl—, Br—, CH3— and HO—were synthesized via Friedel-Crafts acylation reaction and alkylation reaction in the presence of Lewis acid catalyst. The reaction conditions were optimized using the new type AlCl3-LiCl molten salt as Lewis acid catalyst and reaction solvent for Friedel-Crafts alkylation reaction, the yield of 5-substituted-1-indanone is up to 77-82%. The compounds were characterized by 1HNMR and 13CNMR.

Key words: 5-substituted-1-indanone; Friedel-Crafts reaction; AlCl3-LiCl molten salt; Lewis acid catalyst

 

 

阿西美辛雜質F和阿西美辛一水合物晶體的制備及表征

姚明*1,張靜靜1, 2,董志強1,楊森1,熊航行1,李立威1

(1.荊楚理工學院 化工與藥學院,湖北 荊門  448000;2.武漢工程大學 化工與制藥學院,湖北 武漢  430205)

 

摘要:為控制阿西美辛的質量,建立阿西美辛雜質F和阿西美辛一水合物晶體的制備和表征方法。以阿西美辛為原料實現了阿西美辛雜質F的制備,并通過1HNMR、13CNMR和高分辨質譜確證結構。以阿西美辛為原料,通過丙酮和水重結晶制備阿西美辛一水合物,利用紅外光譜、粉末X-射線衍射法和X-射線單晶衍射對該晶體晶型進行表征,獲得了阿西美辛一水合物晶型的表征方法。

關鍵詞:阿西美辛一水合物;阿西美辛雜質F;單晶結構;制備;

中圖分類號:TQ46      文獻標識碼:A      文章編號:0258-32832019

 

Preparation and Characterization of Impurity F of Acemetacin and Acematacin Monohydate YAO Ming*1, ZHANG Jing-jing2, DONG Zhi-qiang1, YANG Sen1, XIONG Han-xing1, LI Li-wei1 (1.College of Chemical Engineering and Pharmacy, Jingchu University of Technology, Jingmen 448000, China; 2.School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan 430205, China), Huaxue Shiji, 2019,

AbstractIn order to control the quality of acemetacin, the preparation and characterization of impurity F of acemetacin and acemetacin monohydrate were established. The impurity F of acemetacin was synthesized by the reaction of acemetacin, and its structure was confirmed by 1HNMR, 13CNMR and high resolution mass spectrum. Acemetacin monohydrate was obtained by re-crystallization using water and acetone as the solvent and was confirmed by infrared spectroscopy, powder X-ray diffractometry and X-ray diffraction. The characterization method for the crystal form of acemetacin monohydrate was achieved.

Key wordsacemetacin monohydrate; impurity F of acemetacin; crystal structures; preparation

 

無溶劑研磨法合成二氫三嗪類化合物

甘信燃2,夏強強*1,史作冬1,邊啟龍1,袁江培1,徐元清*1

(1. 河南大學 化學化工學院,河南 開封  475000;2. 鄭州大學 材料科學與工程學院,河南 鄭州  450000)

 

摘要:采用無溶劑研磨法,以醛和苯甲脒為底物,首先,醛與苯甲脒發生親核加成反應形成席夫堿中間體;然后,中間體與另一分子苯甲脒發生共軛加成,最后經氧化得到相應的二氫三嗪類雜環衍生物,收率高達90%。其結構經1HNMR、13CNMR和熔點進行確證,同時探究了研磨介質、物質的量比和放置時間對反應收率的影響。該方法操作簡單、條件溫和、無污染,為二氫三嗪提供了一條綠色的合成方法,并且為以后藥物的開發提供了關鍵的中間體。

關鍵詞:二氫三嗪;脒鹽;無溶劑;研磨法;綠色合成方法

中圖分類號:O626      文獻標識碼:A       文章編號:0258-32832019

 

Synthesis of Dihydrotriazine Derivatives via Solvent-free Grinding Method GAN Xin-ran 2, XIA Qiang-qiang *1, SHI Zuo-dong 1, BIAN Qi-long 1, YUAN Jiang-pei 1, XU Yuan-qing *1, (1. College of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, China; 2. School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450000, China), Huaxue Shiji, 2019, 41(5),

AbstractDihydrotriazine heterocyclic derivatives were synthesized in up-to 90% yields via solvent-free grinding method, using aldehydes and benzamidine as substrates. Initially, aldehyde reacts with benzamidine and forms an intermediate (Schiff base). Then, the intermediate undergoes conjugate addition reaction with another molecule of benzamidine to give which on oxidation offers product. The structures were confirmed by 1HNMR, 13CNMR and melting point. The effects of grinding medium, molar ratio and storage time on the yield of the reaction were also investigated. This method has advantages such as simplicity of operates, mild reaction conditions, and pollution-free, which provides a new green strategy for the synthesis of dihydrotriazine compounds and a key intermediate for future drug development.

Key wordsdihydrotriazine; amidine salt; no solvent; grinding method; green synthetic method


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