其他检测

即在一定压力下，固-液两相之间的变化都是非常敏锐的，初熔至全熔的温度不超过0.5~1℃（熔点范围或称熔距、熔程）。但如混有杂质则其熔点下降，且熔距也较长。因此熔点测定是辨认物质本性的基本手段，也是纯度测定的重要方法之一。

GC-MS 的电离方式中，相对于常用的EI， NCI 电离方式对具有强电负性的物质（如含有卤素、硫、磷、氮、氧的物质）有高选择性和高灵敏度，电负性愈强，灵敏度愈高。由于多溴联苯醚的化学结构中含有溴原子，因此，GC-NCI/MS 可成为该类化合物的特征分析方法。另一方面，使用NCI 时，由于其高选择性，很多杂质没有响应，从而避免了杂质的干扰，降低本底。本方法对15 种化合物采用NCI 模式进行了分析，对几个关键参数进行了优化，建立了GC-NCI-MS 测定多溴联苯醚的方法。

Thermo Scientific™ Q Exactive™ GC 组合型四极杆 Orbitrap 质谱仪是一款全新的台式质谱，致力于将气相色谱（GC）的高分离能力Orbitrap 高分辨精确质量数（HR/AM）能力完美结合。高质量数精度的质谱仪（MS）对于复杂基质下的目标化合物和非目标化合物测量非常关 键，在进行化合物识别和确认时，对于提高测量结果的可靠性也非常关键。对于前者，获得稳定高质量数精度可以使用相对较窄的质量数提取窗口，充分利用该仪器的质量数解析能力优势；对于后者，提供足够准确的测量化合物质量数，允许化学家可靠预测元素组成和同位素比，以识别物质的化学结构。 结果证实，在使用 Q Exactive GC 质谱仪的高分辨率时，即使在很宽的浓度范围和复杂化学背景下，也能获得出色且稳定的质量精度。

随着社会的发展，特种气体不再是只局限于科研单位的研究对象，而是逐渐走向民用化、产业化，人们对特种气体的需求量也越来越大。而高纯的氦气、氖气作为特种气体中少有的几种惰性气体，不仅科研价值极高，而且应用的领域也越来越广泛。涉及到诸如电子、点光源、激光、超导、光导纤维、低温、等离子体显示器、航天及医疗等诸多领域。 在氦气和氖气的提纯工艺中，需要使用到多台仪器设备来对主要的监测点进行监测，然后根据结果适时地调整工艺参数，最终生产出优质的高纯氦气和氖气。 在氦气和氖气提纯时，在四个主要的监测点上选用了多台色谱分析仪来完成此项工作，此套设备中所采用的分析仪器均来自于爱尔兰AGC公司。 1、粗He/Ne除氮后的N2含量分析 2、粗He/Ne除氮系统后的He/Ne/H2/N2含量的分析 3、产品He的纯度分析 4、产品Ne的纯度分析，包括氖中氦分析

Cyclodextrin-enhanced room-temperature phosphorescence (CD-RTP) shows promise as a sensitive analytical technique. Sample preparation is simple, data-acquisition and processing are easily automated with a Fluorolog® spectrometer, and the result is an intense, well-structured RTP signal. CD-RTP offers the advantages of increased selectivity based on molecular geometry, and partial immunity to quenching by dissolved O2 molecules.

传统的聚乙二醇(PEG)色谱柱存在一些不足，尤其在分析水样中较强的化学活性组分时，这种不足尤为明显。醛类、醇类和有机酸类的分析常受到色谱柱惰性不足的影响，这会导致峰拖尾以及不一致、不准确的结果。一些传统的聚乙二醇(PEG)固定相对水溶液样品不稳定，这会导致色谱柱性能下降、重现性差以及寿命缩短。为了满足用户的需求,我们提出了新型耐水聚乙二醇 (PEG)色谱柱GsBP-Wax-AQ。 在此方法中，我们对低浓度游离脂肪酸和水中乙二醇,乙酸,甲醇和乙醇等常见溶剂样品进行了测试。由于这些化合物含有活性官能团羟基(-OH)和羧基(-COOH)，用传统的聚乙二醇 (PEG)气相色谱柱分析时，通常存在响应低和保留时间重现性差以及峰形不理想等问题，GsBP-Wax-AQ改善了这些问题得到尖锐对称的峰形，而且对该气相色谱柱分析水样的稳定性做了测试,结果表明该色谱柱具有更长的使用寿命，可以提供更可靠一致的结果。

仲钨酸铵（APT）是其他钨化合物和钨合金制备的原料， 作为添加剂常用于石油化工行业，其杂质元素含量直接影响产品的质量。APT中杂质元素含量极低（<0.001%），不同APT牌号对杂质含量要求不同（GB10116-2007），其中Bi、Pb等元素要求处于痕量级，因此，在高钨的基体下杂质元素的检测存在很大的困难。 目前，国标GB/T 4324中已经使用ICP-OES测量仲钨酸铵中Co、Ni、Cr、Al、Ca、V、Cd、Mn等杂质元素的含量。ICP-5000垂直观测模式，具有检出限低、灵敏度高、抗基体干扰的优点，本文采用氨水和双氧水溶解样品，并用盐酸除去基体中钨，随后用ICP-5000检测仲钨酸铵中Al、Ca、Cd等15种杂志元素含量。

The torch configuration (vertical torch, radial observation, sheath gas) allows easy analysis of the incineration solvents mixture. There is no requirement for dilution, cooled spray chamber or additional gases. The optimization was done on the plasma conditions and the sample uptake. The plasma and acquisition parameters are fixed in the analytical method and automatically controlled by computer for an optimum reproducibility from one operator to the other.

This Application Note shows that it is possible to determine trace elements with good sensitivity and low LODs in difficult matrices such as Glycerin and GBL. The only precaution taken was reducing the sample uptake and the nebulizer flow-rate to ensure a stable plasma.

HORIBA Scientific ICPs have the ability to analyze very difficult samples, such as those with high salt content, in part due to the large 3 mm ID injector. In addition, the use of the sheath gas device, originally patented by HORIBA Scientific, enables analysis without clogging of the injector tube and provides the capability of running samples up to 300 g/L salt content. The flexibility of the ULTIMA configuration enables you to choose the gratings depending on the applications, such as the dual grating (4320 and 2400 gr/mm), which provides high resolution and low LOD, in the 200 - 400 nm region. This is particularly useful for the analysis of impurities in rare earths and precious metals.

氮含量的测定首先经硫酸和硫酸钾分解，分解时间往往较长，且长时间电炉加热存在一定危险性。利用海能石墨消解炉消解氮化硼样品，保证实验的安全性，且大大缩短时间。

To achieve the lowest detection limits, dilution is undesirable. The results show the HORIBA spectrometers are able to perform an excellent analysis, even with high dissolved solids. This enables the analysis to be performed to the best detection limits possible.

The structure of many common types of polymer may be modified by either postpolymerization reaction or by the use of modified monomers, producing materials with new and novel properties. Understanding and assessing the effect of these modified structures on the behavior of polymers in various applications is crucial to developing novel uses for such materials. Polystyrene is one of the most commonly seen polymers, used primarily for the manufacture of packing materials. Modified forms of polystyrene may be produced by the use of novel styrene monomers. Gel permeation chromatography (GPC) is a well-known technique for assessing the molecular weight distribution of polymers, a property that influences many physical characteristics. Importantly, increasing the sophistication of the GPC experiment by the use of additional detectors allows the structure and solution properties of polymers to be assessed, of interest when studying the affect of structural modifications on a polymer. Triple detection employing a light scattering detector and a viscometer in combination with a refractive index detector may be used to determine accurate molecular weights for polymers for which narrow standards are not available, and to assess their solvation properties. This application note describes the analysis of a sample of polystyrene and a modified polybromostyrene material by triple detection.

Polyvinyl alcohol (often abbreviated as PVOH) is a water-soluble synthetic material used as an emulsifier and adhesive. PVOH can be modified by reaction of pendant –OH groups with various reagents to form new polymers with novel surfactant properties. Gel permeation chromatography (GPC) is a well-known technique for assessing the molecular weight distribution of polymers, a property that influences many of their physical characteristics. GPC viscometry employing a viscometer in combination with a differential refractive index detector may be used to determine accurate molecular weights for polymers based on the universal calibration approach, useful for materials for which narrow standards are not available. GPC viscometry can also be used to investigate the solution behavior of modified polymers, a useful tool in the analysis of surfactant materials. This application note describes the analysis of two PVOH materials by GPC viscometry – one pure PVOH, and one that had been modified by reaction with imidazole. This second material was insoluble in water so for comparison both materials were analyzed in a polar organic solvent, dimethyl sulfoxide.

Polybutadiene is an elastomer – a polymer that exhibits elasticity. Elasticity is the ability to deform under external stress but return to the original form after removal of the stress. Polybutadiene is a synthetic rubber manufactured from the monomer 1,3-butadiene. Polybutadiene exhibits 80% recovery after stress, one of the highest values of a synthetic material. It is commonly used to coat electronic assemblies due to its extremely high electrical resistivity. Polybutadiene displays a high wear resistance, low heat build-up after repeated flexing and a low rolling resistance, making it suitable for applications such as tires. It is often used in combination with other materials to produce rubber blends with differing properties. The 390-MDS offers triple detection GPC by employing a light scattering detector and a viscometer in combination with a differential refractive index detector, to determine accurate molecular weights for polymers for which narrow standards are not available, such as polybutadiene.

The Agilent J&W CP-Select 624 Hexane GC column, with an optimized G43 stationary phase, separates dichloromethane (DCM) from hexane isomers. This application note shows the separation as applied by pharmaceutical and food processing industries in India. Each column is tested with a special test mix that guarantees good column-to-column reproducibility. As with the specific separation of DCM, the USP <467> specification for the separation of acetonitrile and dichloromethane is in compliance, and tested for in every batch of stationary phase. Column selectivity is compared for two series using a multicomponent mix against two columns from another vendor.

Advanced technology products containing rare earth elements (REEs) continue to evolve at a rapid pace. Consequently, the use of REEs has extended from well-established applications such as glass polishing, to high-performance magnets, high-tech catalysts, electronics, glass, ceramics, and alloys. An alloy of the second most abundant REE, neodymium (Nd), with iron and boron (NIB) is an important material in the super permanent magnets that are used in vehicle components, computer data storage devices, MRI scanners, and loudspeakers. Nd is also used to make glass and safety glasses (didymium) used by glassblowers and welders. As REEs are increasingly used in high-tech products, control of any impurities is important. For example, the presence of other REEs as contaminants in a purified single-element REE material may affect the functionality of the final product, so impurities in the REE oxide raw material must be carefully controlled.

To prevent adsorption of sulfur compounds, deactivation of the stainless steel surface of the sample path is required for the analysis of low ppm levels. This application note shows the separation, low level detection, and analysis perfor- mance of hydrogen sulfide and carbonyl sulfide using the Agilent 490 Micro GC in combination with a fully deactivated sample inlet.

ASTM 2668 and IEC 60666 are the standard test methods, using infrared spectroscopy (IR) technology to monitor the concentrations of DBPC and DBP in electrical insulating oil. These test methods are used to determine if the new electrical insulating oil meets the specification for oxidation inhibitor initial concentration levels. They also monitor the concentration of inhibitors in the used oil. If the inhibitors have been depleted to a critical level, additional inhibitor can be added. Therefore, the standard test methods are essential for manufacturing control, specification acceptance, and to periodically monitor the level of inhibitors in used oils.

在进样前对样品进行浓缩，可以大幅提高安捷伦490 微型色谱的检出限。首先使用带有富集和解吸单元（EDU）的样品浓缩仪将样品吸附到多孔的介质中，然后将被吸附的组分解吸并转移进入到微型气相色谱进行分离和检测。本应用报告介绍了一种使用EDU 样品浓缩仪分析BTEX 的方法，可以将检出限提高140 到200 倍。

表面活性剂在许多生产制造过程中被广泛使用，临界胶束浓度(CMC)对表面活性剂在各个领域的应用具有重要意义。本文采用光学接触角仪对表面活性剂SDS的临界胶束浓度进行了测定。

高纯度异戊烯是一种重要的精细化工中间体，主要用 于生产频哪酮、异戊二烯和叔戊醇，也可作为合成橡胶、 树脂的中间体等。以碳五分离装置的抽余碳五馏分为原 料，碳五馏分中的粗异戊烯与甲醇进行醚化制取甲基叔戊 基醚（TAME）后再分解为高纯度异戊烯是制备异戊烯的 主要方法。采取醚化法生产的异戊烯产品中通常含有甲 醇、二甲醚、TAME等含氧化合物杂质，这类杂质对产品 质量影响很大，因此在生产过程中要控制它们的含量。 本实验采用Trace 1310气相色谱仪，配合AS 1310自 动进样器，参考石油化工行业标准送审稿《工业用异戊 烯中含氧化合物的测定（气相色谱法）》，测定工业用 异戊烯中浓度不低于0.001%（质量分数）的甲醇、甲基 叔戊基醚、叔戊醇等含氧化合物，以外标法计算各组分 的含量。

物质的熔点，即在一定压力下，纯物质的固态和液态呈平衡时的温度，在有机化学领域中，对于纯粹的有机化合物，一般都有固定熔点。即在一定压力下，固-液两相之间的变化都是非常敏锐的，初熔至全熔的温度不超过0.5~1℃（熔点范围或称熔距、熔程）。但如混有杂质则其熔点下降，且熔距也较长。因此熔点测定是辨认物质本性的基本手段，也是纯度测定的重要方法之一。

Ris? DTU，即丹麦科技大学国家可持续能源实验室，位于丹麦罗斯基勒峡湾(Roskilde Fjord)。Ris? DTU的研究领域与能源供给、能源消耗和与健康相关的技术息息相关。 Ris? DTU拥有数个研究分部开展研究（生物系统、燃料电池、材料、辐射、系统分析、风能、等离子体物理和太阳能）。 目前正在开展的研究主题中，约11年来生物质能燃烧研究一直都在充分利用红外热成像技术。

气态反应产物从反应器上部排出后进入ecom-J2KN多功能烟气分析仪利用计算机在线检测分析反应管上端排出的烟气成分．

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本文介绍滑石粉中钙、镁、铁、铝含量的测定方法及石英砂中钙、钾、铁、铝含量的测定方法。包括样品溶液制备等内容。

SPEX —— 是闻名遐迩的三维∞形运动球磨机的发明者， 60 年球磨机生产经验，享誉全球，技术卓越领先。唯一成 功实现机械合金化和纳米研磨的高能球磨技术。SPEX 能 效高，速度快，研磨效果好，是当之无愧以性能杰出的世 界顶级球磨机，其超强性能处于世界第一水平。

活性炭在显微镜下观察有长条状，并且粒径较大，样品不易团聚。用winner2000ZDE测试数据准确，重复测试稳定，效果理想

环氧丙烷，又称氧化丙烯、甲基环氧乙烷，是非常重要的有机化合物原料，是仅次于聚丙烯和丙烯腈的第三大丙烯类衍生物。我国目前对于环氧丙烷的分析标准为GB/T 14491-2001，该标准采用气相色谱法仅仅环氧丙烷中的环氧乙烷，对于国外标准中分析的丙酮等均不做检测。 本实验采用Thermo Scientific 最新型的Trace 1310气相色谱仪，配合AS1310自动进样器，一次进样分析环氧丙烷中甲醇、乙醛、甲酸甲酯、环氧乙烷等多种杂质，扩展了国标中气相色谱检测的杂质范围。