安捷伦科技变革性的原子光谱仪开创使用空气运行的时代

2011年9月9日,北京—安捷伦科技公司(纽约证交所:A)隆重推出4100微波等离子体原子发射光谱仪(MP-AES),该仪器创造性地使用空气运行进行元素分析。4100MP-AES从根本上改变了科研人员进行元素分析的方式。该光谱仪使用空气即可运行,利用氮气产生等离子体,摒弃了实验室配置危险可燃气体和使用昂贵的气体。     

用国产单道扫描电感耦合等离子体发射光谱仪分析海绵铂

铂族元素具有相似的电子层结构和化学性质,使很多试剂能同时与多种铂族元素发生相似反应并产生相互干扰,很难找到特效的试剂,因此分离和测定十分困难.我国贵金属行业测定海绵铂纯度用直流电弧发射光谱法或进口电感耦合等离子体原子发射光谱仪.     

一种用来可同时测定氮及其它金属元素的新型延长炬管的设计

本文介绍了一种新型延长炬管的设计。该炬管使在电感耦合等离子体原子发射光谱仪(ICP-AES）上同时测定氮及其它金属元素成为可能，并且在不同程度上改善了一些金属元素的检测限。本文利用该炬管．在ARL 3520光谱仪上同时测定了生物标准样品中的氮及Fe，Mn、Cu、Zn等四种金属元素。结果与定值吻合，相对标准偏差均小于5%。     

ICP-AES法测定太阳能级硅中磷等12种痕量杂质元素

用电感耦合等离子体原子发射光谱仪(ICP-AES)测定太阳能级硅(SOG-Si)中磷等12种杂质元素。实验发现,在150℃时,用HF和HNO3的混合溶液,试样在PFA烧杯中能较快溶解。在1000级洁净室中,用金属氧化物半导体(MOS)级试剂溶解电子级硅(EG-Si,纯度大于9N)可控制样品空白中各元素的含量均小于1μg/L,并能较好的补偿基体效应。在选定仪器工作条件下,被测元素检出限为5~50 ng/mL,回收率在93%~105%,相对标准偏差RSD≤9.8%(n=11)。测定结果与电感耦合等离子体原子发射质谱(ICP-MS)法及辉光放电质谱(GDMS)法进行了比对,结果吻合。     

电感耦合等离子体原子发射光谱法测定陶瓷色釉料中稀土元素

为了防止稀土的低附加值滥用,控制陶瓷色釉料中的稀土含量尤为重要,本方法为制订出入境检验检疫行业标准《陶瓷色釉料中稀土总量的测定电感耦合等离子体原子发射光谱法》提供可靠依据。由于陶瓷色釉料极其稳定的化学性质,因此不能采用传统的消解方法进行样品前处理,本文提出了用改进后的氢氧化钠和过氧化钠体系高温碱熔陶瓷色釉料,再用电感耦合等离子体原子发射光谱仪测定La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y 15种稀土元素总量的方法。在陶瓷色釉料的消解方法、待测元素波长的选择和基体干扰校正方面进行重点研究。选取具有代表性的陶瓷色釉料样品进行回收率、精密度及重现性试验,测得方法的回收率在94.7%~102.7%,精密度小于2.7%,重现性小于4.3%。计算了15种稀土元素的检出限均小于0.51 mg·kg-1。     

菠萝蜜微量元素含量的分析

应用电感耦合等离子体发射光谱仪(ICP—AES)，对菠萝蜜各个部位进行了微量元素成分的测定分析，其结果为菠萝蜜的综合开发利用提供依据。     

ICP-AES法测定聚酯切片中的二氧化钛、灰分含量

采用紫外可见光分光光度仪(UV法)和电感耦合等离子体原子发射光谱仪(ICP-AES法)测定聚酯切片中的二氧化钛含量和灰分含量.通过比较分析两种测定方法发现,UV法测定结果的准确度、精密度和可靠性较差;ICP-AES法的准确度、精密度和可靠性较优,二氧化钛的加标回收率为98%～102%,相对标准偏差为0.62(n=8).     

Thermo IRIS IntrepidⅡ型电感耦合等离子体发射光谱仪故障快速判断方法

针对Thermo IRIS IntrepidⅡ型电感耦合等离子体发射光谱仪（ICP-OES）在测定含金基体溶液中的杂质元素时,仪器出现灵敏度下降、稳定性变差等现象,通过故障现象分析和排查,给出相应的解决方案,确保仪器恢复到正常使用状态.     

ICP-AES测定蜂胶中12种元素

采用全谱直读感耦等离子体发射光谱仪测定了蜂胶及蜂胶制品中的12种元素，分析结果表明蜂胶制品中富含多种微量元素。     

微波消解ICP-OES法快速测定雪莲果中的微量元素

微波消解雪莲果样品后,等离子体发射光谱仪一次进样曝光快速测定了钾、钠、钙、镁、铜、铁、锌、锰、钼、镍10种微量元素。结果表明,雪莲果中富含钾、钙、镁等元素。该法一次消解样品、多元素同时测定,准确、快速、精密度高,符合分析要求。     

PE 2000型等离子发射光谱仪故障排除方法两例

简述PE2000型等离子发射光谱仪的计算机和光栅驱动电路两个典型故障的排除方法。     

Foundrymate真空型光谱仪在铸造不锈钢炉前分析中的应用

ＢａｒｉｄＦｏｕｎｄｒｙｍａｔｅ台式火花直读光谱仪采用了全新的电子系统,提高了分析精密度。在频快速不锈钢的炉前分析中,Ｆｏｕｎｄｒｙｍａｔｅ光谱仪对铸不锈钢中多元素的同时测定快速、准确、克服了化学分析方法存在的问题。并就影响Ｆｏｕｎｄｒｙｍａｔｅ光谱仪对样品分析的准确度与精密度的主要因素进行了分析讨论。     

THE RED EMISSION BANDS OF MOLECULAR OXYGEN

Abstract— The temperature dependence and the absolute emission intensity of the 6340 Å band of molecular oxygen have been measured. The results indicate that the emitting pair of molecules is not bound and possesses a radiative half life of about 25 msec. The implications of these results on some chemiluminescent reactions are discussed.     

EMISSION SPECTRUM OF THE MICROSOMAL CHEMILUMINESCENCE OF A PROXIMATE CARCINOGEN, 7,8-DIOL-BENZO[a]PYRENE, DETERMINED WITH A WEDGE INTERFERENCE FILTER SPECTROMETER*

Abstract— The emission spectrum of the microsome-mediated chemiluminescence of a proximate carcinogenic metabolite of benzo[a]pyrene, 7,8-diol-benzo[a]pyrene. has been measured with a wedge interference filter spectrometer calibrated with known chemiluminescent and bioluminescent reactions. This instrument has a noise equivalent signal at 490 nm (bandpass 24 nm) of 10⁴ photon s-¹ at 20°C. Spectral and kinetic data indicate that the microsomal chemilurninescence of this metabolite is an exiplex chemiluminescence that proceeds through a dioxetane intermediate.     

高聚物声发射的一些观察

对高聚物的声发射做了进一步的实验观察。玻璃态高聚物在拉伸屈服以前的声发射有Kaiser效应,但在高弹态则不然。非晶态高聚物从玻璃态到高弹态的转变,玻璃态拉伸时在屈服附近出现声发射,高弹态时声发射要少而弱得多,只在高弹拉伸的断裂前出现声发射。非晶态、晶态高聚物或共混高聚物在突然升温到100℃时有声发射,但在突然降温到-60℃时却不出现声发射,这可能也说明声发射与高聚物试样内形成空洞有关。一种聚丙烯树脂在不同注射成形工艺条件下所得试件,在拉伸时的声发射行为可反映加工成形的好坏,成形好的声发射少得多。     

ON THE CONSTRUCTION OF NANOSECOND TIME-RESOLVED EMISSION SPECTRA

Abstract Two common methods of obtaining nanosecond time-resolved spectra (TRES) are compared. TRES measured directly are distorted owing to convolution of the fluorescence signal with the exciting pulse but can be obtained with ease. Undistorted TRES, constructed from deconvoluted decay curves, suffer from poor spectral resolution, require much experimental and computation time to produce and may not be completely free from distortions. Nevertheless, they must be used for quantitative calculations. It is recommended that the method of obtaining TRES should be determined by the type of information required.     

THE CHEMISTRY AND BIOLOGY OF BACTERIAL LIGHT EMISSION

Abstract—Bioluminescent bacteria may be isolated from sea water, and grown on a medium containing fish (or meat or yeast) extract. Cells harvested at the peak of luminescence can be lysed osmotically, releasing into the medium the soluble enzyme bacterial luciferase, which catalyzes the bioluminescent oxidation of reduced riboflavin 5′-phosphate and long chain aldehyde by molecular oxygen. Luciferase is the simplest possible heterpolymeric protein, with an α (catalytic, 42,000 daltons)-β (regulatory, 37,000 daltons) dimeric structure. Luciferase is not constitutive; it is induced by a substance produced by the bacteria themselves and excreted into the medium. Control also involves repression (glucose) and cyclic nucleotides. Recent work has resulted in the characterization of an intermediate in the light emitting reaction postulated to be luciferase-bound 4a-peroxy-dihydro FMN. The final steps in the in vitro light-emitting reaction involve reaction of this peroxy intermediate with aldehyde in a mixed function oxidase-type reaction, yielding an excited luciferase-flavin and long chain acid. The excited state is postulated to be the luciferase-bound 4a-hydroxy-dihydro-FMN. Although the identity of the in vivo aldehyde, its localization and its metabolism is unknown, studies with mutants which fail to synthesize aldehyde suggest that the 14 carbon fatty acid is a precursor. Moreover, although bacterial luciferase is highly soluble (200 mg ml^-1 in aqueous solution) there is recent evidence from our laboratory and others that its function may involve the cytoplasmic membrane. The function of light emission is of particular interest since a considerable amount of energy is involved; assuming a quantum yield of 10%, the cell foregoes the production of about 60 ATP molecules per photon. A fully induced cell emits about 10⁴ quanta/s and about 20% (!) of the oxygen consumption of the cell has been estimated to go via the light emitting pathway. One function is in light organs of higher organisms, where they occur as symbionts. The inducible (and repressible) nature of the luminescent system may be appreciated in terms of ecological options; the bacteria may be biologically very versatile. Induction by an inducer produced by the bacteria themselves would occur only under conditions where it accumulates, as in a luminous organ of a host. In the open ocean such an accumulation does not occur; the luminous system would thus not be synthesized and energy loss via luminescence is averted, allowing the bacteria to compete in an alternate “life style”.     

UPCONVERSION OF THE SINGLET OXYGEN 1269 nm EMISSION TO THE VISIBLE

Abstract— Experiments are described that enable the kinetic behavior of singlet oxygen, O₂(^IΔ_g), to be monitored in the time-resolved mode using a photomultiplier to detect deep orange light (γ_max 660 nm). This orange light is a consequence of the upconversion of the natural emission of O₂(^IΔ_g) at 1269 nm.     

SENSITIZATION BY LUMAZINE PROTEINS OF THE BIOLUMINESCENCE EMISSION FROM THE REACTION OF BACTERIAL LUCIFERASES

Abstract— Lumazine protein from Photobacterium phosphoreurn blue shifts the in vitro bioluminescence spectra in the reactions using each of the 4 main types of bacterial luciferases: P. phosphoreum, P. leiognathi, Vibrio harveyi and V. fischeri . For the reaction initiated with FMNH₂ and tetradecanal at 2°C, this "sensitizing" property of lumazine protein differs quantitatively between the luciferases. An interaction constant characterizing each type of luciferase may be derived from a reciprocal plot of the spectral shift against the lurnazine protein concentration. The weakest interaction constant is in the V. fischeri reaction, 180 μM. For the V. harveyi reaction the interaction is in the range 6–9 μ M , and for both Photobacterium reactions it is 2–3 μM. A concentration of only 0.6 μ M of lumazine protein is sufficient to cause an observable change in the Photobacterium bioluminescence spectra. For the V. harveyi case the interaction constant is near to the equilibrium K _d for the luciferase-lumazine protein complex, observed directly by Visser and Lee. Both constants are decreased markedly by increase in phosphate concentration so that it is concluded that, with V. harveyi luciferase, sensitization occurs within this protein-protein complex. For P. phosphoreum luciferase, however, the equilibrium complex is too weak to correspond to the sensitizing interaction and it is concluded that the rate-limiting process is a protein-protein bimolecular collision. As judged from their molecular weight around 20000, spectral properties, and ability to blue shift the bioluminescence spectra, lumazine proteins are identified in a second strain of P. phosphoreum and in P. leiognathi .     

光谱标样定值的不确定度和标样的不均匀性

分析了目前国内发布的光谱标样的不均匀性，提出了要强调要调不均匀性的概念。为了能检出光谱标样的不均匀性，应该重新设计光谱标样的均匀性检验方案，同时应明确定义不均匀性的概念。