一种机器人采制样系统在选煤厂的应用

目前选煤厂煤质检测过程自动化程度低,采样与制样技术需要大量的人工参与。检测技术的落后直接影响数据的准确性从而对整个选煤厂生产过程控制与产品质量控制产生重要影响,直接关系选煤厂的经济效益。面对产业升级的需要,将先进的自动采制样技术引进煤炭生产经营企业是当务之急。机器人采制样系统包含:机械化采样与初制样技术、机器人精细化制样技术、煤炭快速检测技术、自动快速浮沉技术,为选煤厂提供了一种全自动采制检的新技术方案。     

一种机器人采制样系统在选煤厂的应用

目前选煤厂煤质检测过程自动化程度低,采样与制样技术需要大量的人工参与。检测技术的落后直接影响数据的准确性从而对整个选煤厂生产过程控制与产品质量控制产生重要影响,直接关系选煤厂的经济效益。面对产业升级的需要,将先进的自动采制样技术引进煤炭生产经营企业是当务之急。机器人采制样系统包含:机械化采样与初制样技术、机器人精细化制样技术、煤炭快速检测技术、自动快速浮沉技术,为选煤厂提供了一种全自动采制检的新技术方案。     

废弃线路板化学分析采样、制样及检测方法

介绍废弃线路板中有回收价值元素和有害物质分析的采样、制样及检测技术。样品经过分类采样、剪切破碎和高温灰化制样,采用样品全分析或副批混合样分析。通过提高称样量、多次测定求平均值的办法,火试金富集-重量法测定贵金属金、银。湿法王水溶解样品,碘量法测定主体元素铜。电感耦合等离子体发射光谱(ICP-AES)法测定其它杂质元素,被测元素质量浓度在0~10μg/mL范围内与光谱强度呈良好线性关系,相关系数均大于0.9998。测定结果的相对标准偏差小于10%(n=5),加标回收率为97.0%~102.5%。该方法简单、快速,有效地解决了线路板样品不均匀而难采样,以及硬度、韧性强制样难,金属易包裹难分解的技术瓶颈,测定结果准确,具有代表性。该方法适用于废弃线路板化学成分分析,其它废弃电子产品检测可参考此方法。     

世界采样大会的由来与Pierre Gy采样理论的发展

简单介绍了世界采样大会的由来与Pierre Gy采样理论的产生与发展。重点阐述了Pierre Gy公式和采样理论的涵义与应用,以及化学计量学对采样理论发展的推动和促进作用。同时,采样理论的发展也推动了过程分析技术的应用以及各类先进采样、制样和混样设备的研制和应用。中国作为全球最大的大宗商品进口国和消费国,对采样理论和实践应用有着迫切的需求,将第九届世界采样与混样大会引入中国,必将促进和提升我国采样理论的研究和实践水平,使其更好地为我国大宗商品交易和检验检测市场服务。     

世界采样大会的由来与Pierre Gy采样理论的发展

简单介绍了世界采样大会的由来与Pierre Gy采样理论的产生与发展。重点阐述了Pierre Gy公式和采样理论的涵义与应用,以及化学计量学对采样理论发展的推动和促进作用。同时,采样理论的发展也推动了过程分析技术的应用以及各类先进采样、制样和混样设备的研制和应用。中国作为全球最大的大宗商品进口国和消费国,对采样理论和实践应用有着迫切的需求,将第九届世界采样与混样大会引入中国,必将促进和提升我国采样理论的研究和实践水平,使其更好地为我国大宗商品交易和检验检测市场服务。     

光谱法快速测定半钢发热剂中Si、P、S的方法研究

目前,国内没有关于半钢发热剂的国家标准检测方法,只能根据组分范围分别检测各个组分,不仅耗时而且大量化学试剂对环境造成污染。故研究半钢发热剂全组分快速测定方法。文章采用粉末压片制样,研究其制样条件,包括磨样时间、压样时间和压力对测定结果的影响。采用其他方法定值提供的检测样品,作为X-射线荧光光谱法内控标样,文章中基体校正采用经验系数法,通过解谱拟合建立校准曲线,校准曲线建立后仪器建立漂移校正程序。实验结果精密度好,各元素的相对标准偏差在0.15%-1.3%。准确度满足生产需求,实验方法可用于公司快速检测半钢发热剂化学组分。     

X-射线荧光光谱法快速测定半钢发热剂中Si,P,S

目前,国内没有关于半钢发热剂的国家标准检测方法,只能根据组分范围分别检测各个组分,不仅耗时而且使用的大量化学试剂对环境造成污染。故研究了X-射线荧光光谱法快速测定半钢发热剂中Si,P,S的方法。采用粉末压片制样,研究其制样条件,包括磨样时间、压样时间和压力对测定结果的影响。采用其它方法定值提供的检测样品,作为X-射线荧光光谱法内控标准样品,采用经验系数法进行基体校正,通过解谱拟合建立校准曲线,校准曲线建立后仪器建立漂移校正程序。实验结果精密度好,各元素的相对标准偏差在0.15%~1.3%。准确度满足生产需求,实验方法可用于快速检测半钢发热剂化学组分。     

X-射线荧光光谱法快速测定半钢发热剂中Si,P,S

目前,国内没有关于半钢发热剂的国家标准检测方法,只能根据组分范围分别检测各个组分,不仅耗时而且使用的大量化学试剂对环境造成污染。故研究了X-射线荧光光谱法快速测定半钢发热剂中Si,P,S的方法。采用粉末压片制样,研究其制样条件,包括磨样时间、压样时间和压力对测定结果的影响。采用其它方法定值提供的检测样品,作为X-射线荧光光谱法内控标准样品,采用经验系数法进行基体校正,通过解谱拟合建立校准曲线,校准曲线建立后仪器建立漂移校正程序。实验结果精密度好,各元素的相对标准偏差在0.15%¹.3%。准确度满足生产需求,实验方法可用于快速检测半钢发热剂化学组分。     

XRF分析铁矿粉的标准选择判据研究和应用

本文对ＸＲＦ法分析铁矿的基体校正元素进行了研究，并建立了标准选择判据，编制的计算软件可以自动地从大量标样中选择适合该样品分析的标准。该法可用于粉末压片制样的分析，方法快速，准确度和精密度均符合生产要求。     

环炉法检测大气中氯化氢的研究

用环炉法检测大气中氯化氢,不仅仪器价廉,适合现场快速检测,而且在0.01—6微克范围内定量分析误差在10％以内。本法着重对盐雾和氯气的干扰消除进行了研究。本法一次采样还可进行氯气的检测。 1.纸上采样:将经过处理的(色层定量中速)滤纸,装入三孔采样头内,前面加一张浸渍过20％胆碱碘化物的测尘滤膜。用大针筒往复拉推采样,在检测范围内采样效率为100％。 2.检测步骤:控制三孔环炉仪温度为105±2℃。将载样滤纸置于22毫米辅环上,用33毫米轴环压住。加0.05M硝酸银10微升于样品上,立即以自动充盈管用8×10微升的0.025M硝酸-0.025M醋酸混合冲洗液冲洗。取下上述滤纸,另置于16毫     

激光诱导击穿光谱在煤质检测中的应用现状

我国当前主要能源仍是煤炭资源,煤质快速检测有利于其清洁高效利用。激光诱导击穿光谱（Laser-Induced Breakdown Spectroscopy,LIBS）作为一种快速光谱检测技术,具有样品需求量小、制样简便、可多元素同时测量等优点,其在煤质快速检测中的应用潜力已得到广泛认可。本文从激光诱导击穿光谱仪器（实验室台式、在线式和便携式）的研发现状、激光诱导击穿光谱对煤质（金属元素、非金属元素和工业指标）的检测现状、煤质分析性能提升方法,以及激光诱导击穿光谱定量分析模型研究等方面介绍了近几年来LIBS技术在煤质检测中的应用现状及未来展望。     

干果类食品的样品前处理与分析检测方法研究进展

坚果、果脯等干果类食品含有丰富的营养成分,深受国内外广大消费者的喜爱。但这些食品在果实生产、加工、储运时会使用农药或产生霉变等,造成干果中农药、重金属、霉菌毒素或添加剂等有害成分残留,甚至超过国家限量要求,带来严重的食品安全问题。因此,加强干果类食品的质量监督具有重要的经济和社会意义。但干果类食品基质复杂,有害物质种类多,结构和性质差异大,含量低,其分析检测需要快速高效的样品前处理技术和准确灵敏的分析检测方法。该文主要综述了近十年来干果类食品中有害物质的样品前处理及分析检测方法研究进展。其中样品前处理方法主要包括各种场辅助萃取法、相分离法和衍生化萃取方法等。场辅助萃取法主要是借助超声波和微波场等外场(协同)作用加快干果中有害物质的溶出速度,提高其萃取效率。相分离法,包括固相(微)萃取、分散固相萃取和液相(微)萃取法等,具有溶剂消耗少、分离富集效率高的优势,是干果样品分析中较常使用的前处理方法。该文还重点介绍了干果中各类有害成分分析检测技术,主要包括色谱、原子光谱、无机质谱、电化学分析等常规实验室方法,以及一些适用于现场分析的快速检测技术,并以此为基础,展望了干果类食品中有害物质分析检测技术的发展趋势。     

铁矿石、锰矿石和铬矿石取样和样品制备技术概况

我国钢铁工业的主要原料铁矿石、锰矿石和铬矿石进口量大,对外依存度分别在80%,55%,95%以上,贸易中经常发生质量纠纷,有些质量纠纷的焦点为取样和样品制备技术。从影响样品代表性的角度概述了铁矿石(包括直接还原铁和热压块)、锰矿石和铬矿石取样和样品制备所涉及的方法标准、品质波动、样品部位、最小份样数、最小份样量、缩分方法、最小留样量和设备的技术要求,分析了取样和样品制备中存在的问题,提出了确保取样和样品制备人员能正确执行方法标准、采取有代表性样品应采取的措施。     

Lithium-fusion sample preparation method for radio frequency glow discharge optical emission spectroscopy (rf-GD-OES): analysis of coal ash specimens

The use of lithium-fusion sample preparation methods for the analysis of powder-form specimens by radio frequency glow discharge optical emission spectroscopy (rf-GD-OES) has been evaluated for the test case of coal ash samples. The development of an elemental analysis technique for chemically complex coal ashes presents a challenge in terms of having simple sample preparation, providing accurate results, and minimizing analysis time. The adopted sample preparation procedure for the coal specimens involved a standard lithium fusion methodology. This procedure circumvents many problems associated with the common compaction methods employed for GD analysis of inorganic powders. It was found that coal ashes prepared as glass disks using a mixture of lithium compounds as the host matrix and analyzed by rf-GD-OES provide good plasma stabilization, with analyte optical emission signals stabilizing in ∼1 min and exhibiting ∼2% RSD variations for sputtering times of up to 10 min thereafter. The evaluation of discharge operating parameters and the assessment of approaches to quantitative analysis were also investigated. Discharge parameters of an rf power of 30 W and an Ar discharge gas pressure of 4 Torr yielded rapid signal stabilization and optimized S/B ratios. Sample-to-sample precision of better than 7% RSD was achieved for repetitive samplings (in the same sample locations) for species present at the parts-per-million level in the sample. Limits of quantification could not be adequately evaluated as the levels of the target analytes in the fusion components (i.e. lithium compounds) were above the method detection limit. It is believed that the general methodology holds promise for rf-GD analysis of a range of inorganic solids in powder form.     

Determination of cyclosporin A in blood and plasma by column switching-HPLC after rapid sample preparation

A method for the determination of cyclosporin A in human whole blood and plasma is described which uses liquid chromatography with step gradient elution and a column switching technique. The chromatographic conditions chosen allow simple and rapid sample preparation, so that a result can be obtained within one hour. Blood and plasma are deproteinized with diluted methanol and an aliquot of the clear supernatant is directly injected. The detection limit for cyclosporin A is about 20 ng/ml starting from a 0.5 ml sample. The method is sensitive enough for monitoring the drug in the therapeutic range.     

植物激素样品前处理方法的研究进展

植物激素是植物中一类含量很低,却对植物生长发育等生命过程起重要调控作用的有机化合物。近年色谱/质谱联用技术不断发展,已成为植物激素分析的常用方法,而样品前处理则是色谱分析过程中的一个关键环节,所以高选择性和高回收率的前处理方法对于植物激素的分析至关重要。根据植物激素的化学性质,本文将其分为酸碱性植物激素、油菜素甾醇、植物多肽3类,并对相应的前处理方法加以综述,特别是近年来发展起来的新方法。内容包括前处理方法的原理、装置、萃取材料以及衍生试剂等,相关内容主要围绕本研究组的痕量植物激素研究工作展开,最后对研究趋势做了简短展望。     

Solid-phase microextraction: a powerful sample preparation tool prior to mass spectrometric analysis

Sample preparation is an essential step in analysis, greatly influencing the reliability and accuracy of resulted the time and cost of analysis. Solid-Phase Microextraction (SPME) is a very simple and efficient, solventless sample preparation method, invented by Pawliszyn in 1989. SPME has been widely used in different fields of analytical chemistry since its first applications to environmental and food analysis and is ideally suited for coupling with mass spectrometry (MS). All steps of the conventional liquid-liquid extraction (LLE) such as extraction, concentration, (derivatization) and transfer to the chromatograph are integrated into one step and one device, considerably simplifying the sample preparation procedure. It uses a fused-silica fibre that is coated on the outside with an appropriate stationary phase. The analytes in the sample are directly extracted to the fibre coating. The SPME technique can be routinely used in combination with gas chromatography, high-performance liquid chromatography and capillary electrophoresis and places no restriction on MS. SPME reduces the time necessary for sample preparation, decreases purchase and disposal costs of solvents and can improve detection limits. The SPME technique is ideally suited for MS applications, combining a simple and efficient sample preparation with versatile and sensitive detection. This review summarizes analytical characteristics and variants of the SPME technique and its applications in combination with MS.     

Recent advances in application and progress of advanced materials as adsorbents in sample preparation for plant growth regulators

Plant growth regulators are a class of physiologically active substances that could modify or regulate basic physiological processes in the plant and defense against abiotic and biotic stresses, including natural plant growth regulators and synthetic ones. Different from natural plant growth regulators with low content and high cost of extraction in plants, synthetic ones can be produced in large-scale production and widely used in agriculture for increasing and securing yield and quality of the harvested produce. However, like pesticides, the abuse of plant growth regulators will have negative impacts on human beings. Therefore, it is important to monitor plant growth regulators residues. Due to the low concentration of plant growth regulators and complex matrices of food, it is necessary to isolate and extract plant growth regulators by appropriate adsorbents in sample preparation for obtaining satisfactory results. In the last decade, several advanced materials as adsorbents have shown superiority in sample preparation. This review briefly introduces the recent application and progress of advanced materials as adsorbents in sample preparation for extraction of plant growth regulators from the complex matrix. In the end, the challenge and outlook about the extraction of plant growth regulators of these advanced adsorbents in sample preparation are presented.     

Chemical microanalytical systems: objectives and latest developments

Chemical microanalysis systems are at a very early state of development. At the present time a modular approach with subsystems carrying out the various functions such as sampling, preparation and measurement seems to be favored by the developers. The marketpotential of the systems can be seen primarily in the area of inexpensive monitoring equipment for environmental and process control. Reduction of size leads also to smaller sample volumes, less waste and shorter analysis time: Miniaturization is in many cases an essential feature for biological and in-vivo medical investigations, while some properties inherently associated with miniaturization can also lead to substantial improvements in the technical performance of the microsystem as compared to its macro version. This will be demonstrated by discussing some microsystems which include spectroscopic detection systems:- Miniature separation instruments coupled with advanced miniaturized detection device based on photothermal spectroscopy- Integrated-optical NIR evanescent wave sensor systems- Optochemical and biosensor systems