关于JJF1159-2006《四极杆电感耦合等离子体质谱仪校准规范》在实际应用中的建议

JJF 1159-2006<四极杆电感耦合等离子体质谱仪校准规范>2007年3月8日正式实施,成为四极杆电感耦合等离子体质谱仪(ICP-MS)校准工作的国家计量技术规范.四极杆电感耦合等离子体质谱仪的工作原理较为复杂,主要用于样品中痕量元素的测定.     

电感耦合等离子体质谱法测定精油中砷、钡、铋、镉、铬、铅、锑、汞含量

研究了采用微波消解-电感耦合等离子体质谱仪测定精油中重金属元素砷、钡、铋、镉、铬、铅、锑、汞含量的方法,确定了实验的最佳条件.方法检出限在0.3～3 μg/kg之间,回收率为84.9%～101.5%,RSD在0.9%～4.7%之间.     

电感耦合等离子体质谱在同位素分析中的研究进展

综述了电感耦合等离子体质谱技术(ICP-MS)在同位素分析方面的应用和最新进展,着重介绍了多接收器电感耦合等离子体质谱(MC-ICP-MS),等离子体飞行时间质谱仪(ICP-TOF-MS),激光烧蚀电感耦合等离子体质谱(LA-ICPMS),扇形磁场电磁双聚焦电感耦合等离子体质谱(ICP-SF-MS).     

全自动消解电感耦合等离子体质谱仪测定环境土壤中铍钡铊银

采用HNO3-HF-HCl O_4消解体系,利用全自动消解仪优化的程序消解土样,电感耦合等离子体质谱仪(ICP-MS)碰撞气流速3.0~4.0 mL/min,以7Li,~(103)Rh,~(209)Bi作为内标,通过编辑干扰元素校正方程校正质谱干扰,建立全自动消解电感耦合等离子体质谱仪测定土壤中铍、钡、铊、银4种元素的新方法。结果表明:铍、钡、铊、银校准曲线r0.999,方法检出限在0.005~0.1μg/g之间,RSD为0.19%~2.0%,加标回收率在100.0%~109.2%,该方法用GSS-13和GSS-10标准样品验证,相对误差-3.8%~1.7%,与标准值吻合。采用实验方法对松花江河岸土壤中4种元素进行测定,并用电感耦合等离子体发射光谱法(ICP-AES)进行仪器比对,结果基本一致。     

微波消解–ICP–MS法测定话梅中的二氧化钛

建立了微波消解–电感耦合等离子体质谱仪(ICP–MS)测定话梅中二氧化钛的方法。话梅样品用硝酸及过氧化氢经微波消解仪消解,将消解液除酸定容后用电感耦合等离子体质谱仪测定,以内标法测得钛的含量,并转换成样品中的二氧化钛含量。钛含量在0~500μg/kg范围内与信号强度呈良好的线性,线性相关系数r=0.999 9,检出限为0.04μg/kg。在0.06,0.15,0.30μg/kg的添加水平下,加标回收率为80%~100%,相对标准偏差为3.2%~3.9%(n=6)。该法稳定性好,测定结果准确、可靠。     

带八极杆碰撞/反应池的电感耦合等离子体质谱测定中药中的微量元素

建立了用带八极杆碰撞/反应池的电感耦合等离子体质谱仪(ICP-MS)测定中药中的多种微量元素的方法.八极杆碰撞/反应池技术的使用,有效地消除了多原子离子对待测元素的干扰,使Se、 As及其它微量元素的测试更为准确.方法对固体中药样品的检出限为0.002～0.085 μg/g,相对标准偏差为0.4%～3.1%,回收率为90%～110%.     

电感耦合等离子体质谱法测定地球化学样品中的银、砷、锑、铋

建立了王水分解样品,电感耦合等离子体质谱法测定地球化学样品中的银、砷、锑、铋的方法,采用王水-水浴分解试样,电感耦合等离子体质谱仪测定新疆和田策勒恰哈地球化学样品中的银、砷、锑、铋,确立了最佳的溶样时间、测定酸度、干扰元素的校正方法,结果令人满意。各元素的方法检出限为0.003 8~0.041g/g;相对标准偏差RSD(n=12)为0.52%~2.8%;方法灵敏度较好、简便、快速,且结果准确,适用于大批量地球化学样品的快速测定。     

电感耦合等离子体质谱法测定高纯氧化钽中28种痕量杂质元素

建立了用电感耦合等离子体质谱仪(ICP-MS)测定高纯氧化钽中28种痕量杂质元素的方法。讨论了质谱干扰及接口效应,采用标准加入法消除基体效应。各元素的方法检出限为0.001~0.1μg/g,回收率为90%~115%,方法适用于纯度为99.999%的高纯氧化钽中痕量杂质元素的测定。     

193nm激光器与电感耦合等离子体质谱仪联用条件优化研究

激光剥蚀电感耦合等离子体质谱仪( LA-ICP-MS)是采用激光剥蚀固体进样方式构建的新型等离子体质谱分析仪器.由于受激光产生原理-“脉冲式激发”的限制,样品的剥蚀进样过程属于间歇模式.因而激光剥蚀系统与电感耦合等离子体质谱仪联机分析结果的相对标准偏差( RSD)通常达10％以上,影响数据的分析精度.本设计在激光剥蚀系...     

电感耦合等离子体质谱法测定无尘产品中痕量氯

研究了利用电感耦合等离子体质谱仪测定无尘产品中的痕量杂质元素氯含量的方法,检测下限0.06 ng/mL,精密度RSD<5%(n=7),回收率93.7%~110.0%。     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。