笔者想在JRC-从卡尔斯鲁厄设计室和车间感谢安德烈亚斯·赫塞尔什未特和乔尼·拉奥的设计和拉曼分析放射性样品架的制造。帕特里克Lajarge，丹尼尔·弗莱斯（JRC-卡尔斯鲁厄），和马克·萨斯菲尔德（NNL，UK）被确认用于提供与所述本发明的技术研究了AMO 2个样本。作者也想感谢鲍里斯·伯拉科弗（Khlopin镭研究所）提供样品制备切尔诺贝利熔岩和菲利普Pöml和罗尔夫·格雷特（无论是在JRC-ITU）的样品。

1.实验计划<ol><li>确保拉曼光谱仪中使用配备有滑动架下方的XY载物台，具有中心孔的至少直径60mm。 </li><li>确保有自由室下方的级的至少150mm至引入囊和，这个房间是方便（从顶部或底部）。 </li><li>确保拉曼光谱仪装备有一个客观的具有至少10毫米的工作距离。 </li><li>确保分析样本被存储，并移植到在适当的气氛中的胶囊（参照本地过程从手套箱转移样品）。 </li><li>确保样品能够与镊子，小化工匙，或将样品装入胶囊所需的刮刀进行处理。 </li><li>高压（HP）选项:确保限制系统配备了系统泵和填充高压胶囊。 </li><li>问当地的RadioProtection官辐射防护措施落实的完整过程。 </li></ol> 2.样品架的制备<ol><li>收集所有构成胶囊或，可选地，高压胶囊中的零件。 </li><li> 固定窗口上的胶囊体 <ol><li>均匀地施加环氧树脂的少量直接与在槽装配窗口的外部部分的涂胶器。需要注意的是不同类型的环氧树脂都试过了。在材料清单中指示的胶水，是因为它比粘度的这种应用最适合的。 </li><li>要确保安装的窗口是光学干净，戴上干净的手套，并解开其原包装的窗口。将其放置在所述丙烯酸类玻璃胶囊的槽，用手指以分散所述窗口和所述槽之间的胶移动它。 </li><li>透过车窗仔细检查，看是否胶水均匀AP窗口和丙烯酸玻璃之间合股。 </li><li>让胶固化，只要在胶说明书指示。 </li><li>再次检查透过玻璃看到窗口和丙烯酸玻璃是否正确粘贴;无气泡应该是可见的。 </li></ol></li><li> HP选项:在高压囊体固定窗口 <ol><li>检查用放大镜与所述胶囊的O形环接触的表面是否清洁和均匀加工，这确保了良好的气密性。 </li><li>放置胶囊的O形环在高压胶囊主体的窗口侧的专用小树林。 </li><li>放置高压胶囊窗口上的高压胶囊主体在胶囊O形环。 </li><li>放置在高压胶囊窗口聚甲醛平环。 </li><li>放置封闭法兰在高压胶囊窗口的窗口一侧的顶部，并与6顶水槽螺钉贴上它。 </li></ol></l我&gt; <li> 固定在袋子上的胶囊 <ol><li>首先插入胶囊，窗，从漏斗形袋的宽侧入漏斗形袋的狭窄部分，结束到在气缸不能进一步滑动，因为突出部分的点。 </li><li>如果需要，调整所述袋位置，以使气缸伸出漏斗形袋的由约1.5cm。 </li><li>放置紧固O形环上的圆筒的槽袋。 </li><li>胶带，以便柔性电胶带到气缸内的袋留下约8mm发现的气缸的上部。这部分将被用于固定在拉曼显微镜气缸。 </li></ol></li><li> 盒装配密封性试验 <ol><li>带来配备有所述胶囊（袋组件）的漏斗形袋，以专用于手套箱手套和囊，通常在核设施可用的气密性试验的安装（在这种情况下，在Ar-H <sub&gt; 2过度加压装置用H 2检测器）。 </li><li>修正了测试法兰袋组件。 </li><li>它带以使用电磁带凸缘。 </li><li>填充至500毫巴用Ar + 5％H 2的气体混合物。 </li><li>移动便携H 2探测器周围的所有胶囊和囊中，并须特别留意周围的地方粘贴在窗口中的区域。 </li><li>如果检测H 2，从步骤2.5.2重复该过程，因为袋组件不够紧密。 </li></ol></li><li> 柱塞的制备 <ol><li>安装在柱塞槽的滑动O形环。 </li><li>安装短轴安装在柱塞上。 </li><li>贴在销存根双面粘合接头片安装，保持在保护层朝向外侧的表面上。 </li><li>螺杆拉螺杆在柱塞的另一侧。 </li><li>如果样品是粉末或具有部分小于1mm，安装外部簧环与在所述柱塞（向着螺钉）的最后槽开口簧环夹钳。对于样品大于1mm，调整在柱塞槽到样品的厚度外部簧环的位置。 </li></ol></li><li> 高压柱塞的制备 <ol><li>请用放大镜在与胶囊O型圈接触两个表面是否清洁，均匀地加工，确保密封性好。 </li><li>在样品上侧的专用柱塞槽安装的胶囊O形环。 </li><li>螺丝样品支架在柱塞的顶部。 </li><li>粘一片双面胶标签，对应于所述样品保持器的尺寸，在样本保持器，保持所述保护层朝向外侧的表面上。 </li><li>检查用放大镜与所述入口的O形环接触两个表面是否清洁且均匀地加工，确保良好的气密性。 </li><li>在在th专用槽安装入口O形环柱塞电子气体入口侧。 </li><li>拧在柱塞适配器。 </li><li>根据安装的安装过程适配器上的球阀。 </li></ol></li></ol>样品架样品3.安装<ol><li>根据本地过程的限制系统上安装所述样品架，并在同一时间，安装在限制系统的柱塞。 （HP选项）:安装6底水槽螺钉为好。 </li><li>从双面粘合片除去保护层。 </li><li>握住推杆，并将粘接标签上的样品。如果样品是单件，请按用镊子或化学勺子，如果可能，样品一点点。如果样品是粉末，轻轻地传播它的样品架。 HP选项:放置样品大于1毫米的高度上的高压样本保持器小。 </li><li>插入柱塞:在胶囊（HP选项柱塞法兰）。推，直至其CAn不是去任何进一步的，同时注意保持胶囊处于垂直位置。从这一点来说，确保胶囊保持尽可能地在垂直位置。 </li><li> HP选项:拧紧6底水槽螺钉在高压胶囊主体组件的底部以固定柱塞凸缘。 </li><li> HP选项:高压囊加压。 <ol><li>球阀连接到在该限制的真空/气体供给管线。 </li><li>打开阀和排空胶囊。 </li><li>加压与所选择的气体的胶囊，注意，它不超过20巴并且该气体是惰性气体相对于所述胶囊材料。 </li><li>关闭阀门。 </li></ol></li><li>从根据本地过程约束分离胶囊，并注意使阀不会损坏塑料袋。通过绑在一起，以适合它下面的显微镜载物台降低袋的容积（见步骤4.4）。注意是t他的过程，可能需要在第一个录音第二袋。 </li></ol> 4.安装下的拉曼显微镜胶囊<ol><li>固定用封闭螺钉金属环滑动件（ 见图3）上的胶囊型的无磁带上部。拧紧螺丝侧阻止它。 </li><li>从顶部或显微镜载物台的底部插入的胶囊。 </li><li>安装在舞台上的滑动架的金属环滑动（参见图3）。与滑动支架弹簧将其固定。 </li><li>检查台下袋可以在任何需要的X，Y内自由移动，和舞台ž运动。如果没有，用胶带包起来，以减小其体积。 </li></ol> 5.拉曼光谱测量<ol><li> 在拉曼光谱仪的频率校准。 <ol><li>将单硅晶体在胶囊的窗口上。 </li><li>选择目标Ťo使用和聚焦显微镜。 </li><li>选择用于测量的激光波长和确定单晶硅，为此，参考频段为520.5厘米-1 26的T-2 克激励。使用该软件，相应地调整频率刻度。 </li></ol></li><li> 在拉曼光谱仪的强度的校准。 <ol><li>调整光路，激光器，入口狭缝，极化配置，共焦空间滤波器，以及为了最大化峰值强度，同时保持作为狭缝而不降低最大强度关闭尽可能使用强Si晶体峰CCD开口。该强度比较后在相同条件下"工厂"对准而得到的值。 </li><li>关闭狭缝和空间滤波器，以达到所要求的光谱和z轴的空间分辨率，分别。 </li></ol></li><li> 样品的测量结果。 <ol&gt; <li>测量以类似的方式为未包封的试样的样品。注意，该步骤在很大程度上取决于所使用的，以及在测量的类型拉曼光谱仪的类型。请参阅拉曼光谱仪的说明书。对于非常小的样品（例如测量激光光斑的尺寸的一种晶时），荧光信号可能出现在喇曼光谱照明双粘合剂标签的主要是因为。在这种情况下确保重新聚焦显微镜以照亮最大的小样品的表面，降低了光谱仪的入射狭缝孔来分析只被照射斑的中心部分。确保以及到不直接与激光照射双面粘合。激光功率可能烧坏粘合剂和释放在测量光谱加入荧光挥发性有机分子。 </li><li>检查，在所测得的光谱中，熔融二氧化硅27的谱线&lt;/窗口不显示的SUP&gt;。使用带有差共焦拉曼光谱仪时，可能发生这种情况。 </li></ol></li></ol>

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Solids. 31 (3), 415-422 (1970).</li><li>Naji, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+original+approach+for+Raman+spectroscopy+analysis+of+radioactive+materials+and+its+application+to+americium-containing+samples.">An original approach for Raman spectroscopy analysis of radioactive materials and its application to americium-containing samples.</a> J. Raman Spectrosc. 46 (9), 750-756 (2015).</li><li>Horlait, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Self-irradiation+and+oxidation+effects+on+americium+sesquioxide+and+Raman+spectroscopy+studies+of+americium+oxides.">Self-irradiation and oxidation effects on americium sesquioxide and Raman spectroscopy studies of americium oxides.</a> J. Solid State Chem. 217, 159-168 (2014).</li><li>Naji, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Raman+Scattering+from+Decoupled+Phonon+and+Electron+States+in+NpO2.">Raman Scattering from Decoupled Phonon and Electron States in NpO2.</a> J Phys Chem C. 120 (9), 4799-4805 (2016).</li></ol>

作者什么都没有透露。

本实验的方法依赖于原本的胶囊，其可被容易地设计和配好的车床一个车间制造。除了外部直径，这应该适合与市售漏斗形袋，胶囊的其它尺寸不是严格必要的。然而，用于高压胶囊，暴露于高压表面应被最小化，尤其是表面垂直于胶囊轴线。这里，例如，最大表面是的5mm半径（r）窗口，这对应于约127平方毫米（A =πr²）的区域A。的暴露于该表面20巴的压力P.开发的254 N的力F中的窗口（P = F * A）上，P以Pa，F在N，和在m 2的。该力，分布在6个螺丝，导致约42 N /螺钉。这应该设计胶囊和活塞侧时加以考虑。第二点应采取的帐户:紧岬柱塞，以及气体的高压体积。当柱塞被放置在封闭内袋，该气体约束袋的内部膨胀在泄漏的情况下，可能损害限制的紧密性。设计应确保，相对于袋容量时，气体中的泄漏的情况下，膨胀的体积是可忽略的。该设计还应当确保在与O形环接触的表面被制造精良，确保密封性的合适的水平。这些表面的质量控制，以及O形环的，应进行。需要注意的是强烈的放射性样品，最终可能随着时间的推移破坏胶囊的材料。因此，胶囊不应该被用来存储放射性样品很长时间。另外请注意，这个系统是一个核材料约束系统，可能需要当地安全部门的批准。 这种技术的优点是很多的在比较部分或补偿勒特拉曼光谱仪禁闭2，3，4，5，6，16，17。没有特别的限制（手套箱和热室）是必需的，因此，不会产生额外的材料必须为核废料在生命的最后处理。没有拉曼光谱仪（坐月子时需要）的定制。有在波长，偏振，测量的模式，或在其中测量完成的气氛的简单设定的条件对测量的可能性没有限制。 与在ORNL所使用的方法比较- USA 12，13，14，15，显微镜可以在适当的光学条件被应用（一个或多个英格尔光学窗口，而不是管），减少了所需的样本数量，以及用于激光功率的要求。 该系统的一些限制，应指出。由于胶囊窗口的存在的样品与显微镜物镜之间的距离施加了使用长焦距物镜的，这可以减少一个宽孔拉曼光谱仪的灵敏度。样品和目标之间的非涂覆的熔融石英窗口的插入也可以降低成像质量。而且，目前的封装系统也不可重复使用，由于这样的事实，漏斗形袋明确固定在胶囊。然而，如果漏斗形袋的小侧配备有一个集成的O形环，从而允许施加转印袋技术的胶囊以及的可能性，这可能得到解决。这将使使用更复杂的胶囊的可能。例如，一种机制，以允许气体流;一德温度测量装置;或机械压力控制阶段固体以及液体的分析，或用于在动力学效应现场测量，将是可能的。要注意的一点是，高放射性样品如镅的拉曼光谱中，应非常快速地测量（有时在不到一周的时间），因为其增加了拉曼光谱随时间的附加荧光信号。后暴露于辐射的几天这种现象可能是由于双面胶粘标签的降解，从而导致生产该样品表面上的冷凝挥发性有机分子。 本系统特别适用于放射性核材料的研究。它也可以应用到任何其他类型的材料，用户应当避免（危险样品），或者必须从保护大气环境样品的研究。

拉曼光谱法被广泛用作在诸如药品，化妆品，地质学，矿物学，纳米技术，环境科学，考古学，法医，和艺术鉴别1字段非破坏性分析方法。它用于在晶体或分子的振动，旋转，和其他低频率模式的分析。此技术是晶体结构，组成，结晶状态，温度，电子状态，应力，压力，晶粒尺寸（特别是在纳米结构的微晶的情况下），夹杂物，和缺陷敏感。对于单分子（气体或基质隔离分子），拉曼是在化学组成，局部协调，和电子结构是敏感的。它可以被用作电子共振或表面增强光谱术的事实使得它非常在非常低的浓度的化合物的检测和测量敏感。 它的便捷性利用，有限的样品制备，以及用于远程测量的可能性的，拉曼光谱是在核领域特别感兴趣的。最近已用于在废核燃料的辐射损伤的应用研究（缺陷）2，3，4，5，以及用于在锕系元素化合物系统6，7，8，9，10，11，12的基础研究， 13，14，15。对核材料的拉曼检测的主要挑战是辐射暴露和结合的固有风险。这些风险是可以管理:辐射被屏蔽，并结合禁闭。通常情况下，像丙烯酸玻璃手套箱内的限制系统是足够的，以限制和屏蔽α发射体。 β和γ，可能需要额外的高密度屏蔽材料，如铅或铅掺杂的玻璃。中子发射器将需要屏蔽组成，其能够容易地捕获中子和富含氢气，例如水或石蜡的材料制成。到现在为止，核材料的最拉曼分光测量已经在屏蔽细胞远程配置， 例如执行与玻璃纤维2，3，4，5，6，16，17连接的远程头的帮助。这种技术甚至适用于废核燃料2的直接分析。不幸的是，这种方法有一定的IMportant限制:第一个是，在小区内的所有远程拉曼光谱仪部分是与放射性材料直接接触迅速损坏它们18，并将它们转换成放射性废物。进一步的限制是固有的远程技术。例如，使用光纤限制使用不同的激发波长，共焦，偏振等的可能性 （ -美国橡树岭国家实验室）12，13，14，15另一种实验方法是在1990年在橡树岭国家实验室开发。放射性样品在双毛细管石英密封，本身放置在由硼硅酸盐玻璃管的第三限制。这使得含有锕物种的第一拉曼测量。然而，测量就一定要通过一些非专业进行弯曲石英和硼硅玻璃的ERS，产生太低信号。以这种方式，这是不可能获得的，例如，AMO 2 12的质量光谱。此外，开始等。 12不得不使用可能已受到局部加热所述样品的相对高的激光功率（几百毫瓦）。 它应该是可以采用，以获得锕系化合物的声音参考拉曼光谱所有拉曼光谱仪的功能（激发波长，光谱仪模式，极化等 ）。鉴于此，我们开发了放射性样品的本地封装的一种新技术。它允许为核材料的测量使用标准的非污染的或定制的微拉曼光谱仪。使用拉曼分析（微拉曼光谱，或μRS）显微镜呈现一个重要优点在于，它仅仅需要样品的一个非常小的量要观察并正确测量。基本上，样品大小为几十微米的数量级就足够了μRS，由于配备有10X 50X或客观显微镜的几微米的空间分辨率。样品的暴露2500微米2（50×50微米大小的）到显微镜的体积，取决于形状，为约0.1mm 3，其对应于重量的约1毫克，考虑到12克的密度/厘米3（典型为锕系氧化物）。高放射性241的AM A 1毫克样品暴露在10厘米0.5微西弗/小时的用户至约50微西弗/小时1米处19。这些级别的法律剂量限值内容易残留，通常在毫希沃特/天的微西弗的手和几十顺序/天的身体20。此外，该系统还隔离大气环境样品，包括高湿度水平或氧气的存在下进行。依赖新生定的测量的需要，从真空中，用户甚至可以选择为20巴，反应性或保护性的最佳气氛。在研究的材料的化学反应性，以他们的大气环境，像锕系氧化物，氟化物盐，金属（氧化，还原，和与水的反应），这是特别重要的。样品，通常需要用于拉曼测量的强烈的激光照射，提高这些反应的动力学，因为样品可以通过激光进行加热。这些反应可以通过选择合适的气氛来补偿。这种类型的过程也可帮助对危险标本，像化学品或感染性生物物质的任何光学测量。 所述α-辐射和大气紧拉曼样品架由丙烯酸类玻璃圆柱体，直径44毫米和60mm长，在其轴线的钻15毫米的深孔（ 图1）的。这一部分，胶囊，用2mm厚的，毫米直径20，一个波光学研磨的熔融石英窗口关闭一侧。甲毫米直径的14.9丙烯酸玻璃棒，柱塞，保持样品被插入在胶囊达到如此地步，所述样品来自右边的窗口的下面。将样品（盘的粉末或小片段）被固定于标准铝销存根一个双面粘合片的帮助下安装直径12.7mm，本身固定在丙烯酸类玻璃棒（柱塞）的端部。柱塞被配备有外部簧环，以避免推压样品和其持有者太远的熔融石英窗口，这可能会导致在实验室中的胶囊和放射性的分散体的破裂的风险。此外，外部簧环可以在不同的位置被设置，在用于在柱塞为此所作的凹槽中的一个，以便调整所述样品和所述窗口之间的距离。柱塞还配备有O形环的平滑滑动的气缸中的杆。为了避免压缩气体或大气中的气缸内，同时插入所述杆，在气缸的内表面中的凹槽允许气体的安装过程中撤离。螺钉可以固定在以拉动杆从缸中的柱塞的底部贯穿设置的螺纹。样品可以因此通常非破坏性拉曼分析之后除去。 第二样品架已经被开发，以便所选择的气氛下进行的拉曼分析高达20巴（ 图2）。这种高耐压的α-辐射和气密拉曼样品架由聚醚醚酮（PEEK）圆筒体的直径44毫米和长65毫米，其中一个16毫米的孔其在轴线钻出。这一部分，胶囊主体，与3mm厚的，毫米直径的12.7，一个波光学研磨的熔融石英未涂覆由金属坯保持窗口关闭在一侧上GE由6个螺丝固定在胶囊主体。为了实现气密性，窗口搁置的O形环放置在所述主体形成的凹槽上。为了防止与金属法兰直接接触的窗口中，含氟聚合物弹性体平坦关节被置于两者之间。胶囊的另一侧由另外的金属凸缘（柱塞凸缘）也固定在车体用螺钉封闭。柱塞凸缘配有一个柱塞，在其一个样品保持器被旋拧（靠近窗户）的端部。刚刚所述样品架的下方，所述柱塞配备有O形环放置在一个槽，从而确保胶囊的高压密封性。柱塞被钻在由只是O形环之后结束的毛细管的整个长度，从而确保密封性。它旨在泵送真空或将样品室的压力下。该样品被固定在样品支架先前相同的方式进行说明。柱塞凸缘配有一个适配器到6毫米的不锈钢气体管道，以便以耦合到用于气体入口或抽真空的阀。 为了对接胶囊和其中样品被存储，而无需破坏该限制的限制系统的外侧部分中，使用公认的传送袋技术。这种技术通常使用的，特别是在核工业，以两个分离的分娩之间安全地传送样品。这里所用的漏斗形袋是专门为使用该技术的设计。在样品架侧，袋子端部是漏斗形，最小的直径与胶囊的外径嵌合。凹槽和一个突出部分，以便安装一个紧O形环围绕所述袋，将其保持在适当位置，并防止汽缸滑动太远入袋，分别在汽缸的外表面上实现的。 本文提供的实验方法的详细信息，以及第t的三个具有代表性的应用实例echnique。其中一个例子是关于高放射性镅二氧化碳拉曼研究。这是在特殊的核燃料瞄准放射性减少在上午嬗变的研究特别感兴趣的长寿命核废料21，22，23，24，而且作为放射性同位素发电机更换238浦为深供电-space探测飞船25。这个高度放射性物质检体的测定证明了开发的技术的强度。第二个例子也涉及计划嬗变的材料。它报告的NPO 2的拉曼特征，包括17 O掺杂的影响的更基本的研究中，使用三种不同的激励波长和各种激光功率电平。将所得的样品温度通过测量估计这里斯托克斯和反斯托克斯谱线强度之间的比例，用三重分光计的配置的帮助。这次成功的测试表明，通过这种技术，还提供帮助，以确定可作为NPO 2指纹电子振动拉曼光谱带的工具的灵活性。在最后一个例子中，使用本方法来拉曼映射从形成在1986反应堆堆芯熔化后切尔诺贝利熔岩取得的样品。这是为了存在于材料中的不同阶段的鉴定。

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			<td>Swagelok, Forst(Germany)</td>
			<td>SS-6P4T-MM</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) 1.4301 stainless steel sample holder</td>
			<td>home made</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) 1.4301 stainless steel high pressure plunger</td>
			<td>home made</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) 1.4301 stainless steel adapter</td>
			<td>home made</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) 1.4301 stainless steel closing flange</td>
			<td>home made</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) 2 x fluoropolymer elastomer capsule O ring 10*1 mm</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) fluoropolymer elastomer inlet O Ring 6*1 mm</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) 6 x DIN 7991 M4 * 25 mm bottom sink screw</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) 6 x DIN 7991 M4 * 18 mm top sink screw</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">(High pressure) Polyoxymethylen flat ring 13/10*1 mm</td>
			<td>home made</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

a novel technique for raman analysis of highly radioactive samples using any standard micro-raman spectrometer

为核材料的拉曼测量的新方法被报道了。它由放射性样品的以紧密胶囊从大气隔离材料机壳。该胶囊可任选地填充有加压至20巴的选择气体。微拉曼测量通过光学级石英窗执行。这种技术允许与不需要分光计被封闭在α-紧容纳准确拉曼测量。因此，它允许使用的拉曼光谱仪的所有选项，例如多波长激光激发，不同的偏振，以及单或三重分光计模式。的测量值的一些例子示出并讨论。首先，高度放射性镅氧化物试样（AMO 2）的一些光谱特征被呈现。然后，我们报告镎氧化物的拉曼光谱（NPO 2）的样品，解释其中大大提高通过使用三个不同的激发波长，17 O掺杂，和三模式配置以测量反斯托克斯拉曼线。这最后一个特征也允许在样品表面温度的估计。最后，在从切尔诺贝利熔岩，其中相通过拉曼作图鉴定的样品进行测量的数据，被示出。

三个证明了该系统的潜在独特和有代表性的结果报告本节。 这些测量已记录用装有拉曼光谱仪的1800槽每毫米光栅;低噪声，LN 2 -cooled交响乐CCD检测器，一个减色预单色器（在三模式），它允许获得低波数（可达10厘米-1）;和反司托克斯线或边缘滤波器（单模），挡住了弹性激光散射来自样品。入射光被使用长的工作距离（10.6毫米）目标，它提供了一个0.5的数值孔径与5×10 4的放大倍数聚焦。显微镜系统配备有Z-马达，基于压电的定位器提供快速聚焦和长期稳定性。平行和交叉极化配置之间的切换可以利用进行一个λ/ 2板对于入射光束，具有用于反向散射光λ/ 4和90°偏振器的组合。背向散射的光通过一个可调节的空间滤波器，允许它在共焦条件下工作。阶段是机动的在X和Y轴的两个，以允许自动区域映射。激发源是氩离子连续波（CW），在488nm和514.5nm的，或氪+与647纳米和752纳米的波长主要连续激光器主波长的激光器。两个激光器的额定输出功率可被数字从几毫瓦到几瓦，取决于波长调整。单色仪或带通滤波器用于阻断背景等离子体和二次发射线。撞击在样品表面的功率在使用相干功率计的显微镜物镜输出被测量。使用长焦距50X物镜和单个分光计模式允许良好的光谱分辨率（±1 -1），个独立表面形状的吨，具有2微米×2微米的样品表面上的空间分辨率。 AMO 2的拉曼光谱纯二氧化镅的拉曼光谱用较低能量的激发源测量与先前的研究28进行比较。它在大气中的胶囊进行测定。对于AMO 2的无缺陷萤石结构，组理论预测只有一个拉曼活性模式（T 2克 ）28，其对应于一个AM阳离子八根氧阴离子在立方环境所包围的AMO键的振动。虽然Ť2 克的UO 2的位置是精确已知的是约445nm -1（尽管作者之间小的变化），即AMO 2的从未被清楚地识别。 图4 </strong&gt;示出了具有647纳米的激发波长获得的AMO 2的典型拉曼光谱。相同的频谱是由纳吉等人记录。 28和Horlait 等。 29镅的氧化物以往的研究。它是通过在〜380厘米为中心的宽峰，非对称带为主-1和试探性归因于萤石型结构的氧拉伸运动。 为什么在相当低的频率观察到这种模式相对于其他锕系二氧化物的原因仍然是一个有争议的问题。可能的是，这种转变是由于光还原AMO 2至Am 2 O 3 + Z由激发激光声子，最近由纳吉等人提出。 27。这样的效果会与AMO 2的非常高氧势是一致的。为了阐明这一点，进一步拉曼测量被在图2中示出的修改的设置在高氧压下制备。 NPO的拉曼光谱2 当前技术也被用于研究镎氧化钛的使用三种不同的激励源的拉曼特征（NPO 2），具有647纳米，514纳米，且分别为30 488纳米，入射的光子能量。在NPO 2的T 2G频带的不对称的轮廓已经被探测。此外，17 O富集的NPO 2样品（30％富集）已经以区分到的拉曼光谱30振动和电子的贡献进行分析。在样品表面的温度是通过测量斯托克斯和NPO 2的使用玻色-爱因斯坦ST反斯托克斯Ť2 克线强度比来确定atistics（ 图6，顶部和中间）。我们的结果清楚地表明，在第一次，二次模式的在〜431厘米存在- 1（ 图5b，5d和图6，底部），诱导在T2 克峰（ 图5c）的低波数不对称，这是NPO 2晶格的签名。从拉曼强度（ 图6，底部）的同位素移位（ 图5d），激光能源的依赖，以及温度特性，我们表明，该模式从一个频带产生与电子来源。我们建议将它对应于由理论束缚态预测裸，解耦晶体场水平。 切尔诺贝利熔岩的拉曼分析在t他切尔诺贝利事故，高温燃料之间的相互作用（高达2600℃），被毁坏的燃料包壳，和硅酸盐材料（混凝土，砂，和蛇纹岩）滴加到反应器导致一种熔岩的形成称为真皮。液体真皮飞进厂击穿放电走廊地下室。此熔岩的首批样品收集在1987年与AK47机枪的帮助，因为高活性和真皮的强烈力学性能。在1990年，熔岩的热液蚀变和崩解用双氧铀状的第二相的形成观察到。其中一些切尔诺贝利熔岩样本进行多个分析，提供给JRC-卡尔斯鲁厄由Khlopin镭研究所。几个拉曼测量是在切尔诺贝利真皮样品的各种切割和抛光的表面上进行。所有这些测量均加上SEM-EDX数据以识别元素组成和各相呈现上表面。 图7示出了具有使用拉曼光谱进行分析，不同的相"点"的代表性样品的光学图像。 图8示出了从点1，2中得到的拉曼光谱，和图3在图7中。光谱对应于SiO 2个的玻璃:（U，Zr）的的SiO 4，USiO x和（U，锆）O X，分别。这些相无论是从与核燃料包层的直接相互作用而形成的，然后运如在熔体捕虏晶或运输和冷却期间从硅酸盐的熔化物中结晶。 <img alt="图1" class="xfigimg" src="/files/ftp_upload/54889/54889fig1.jpg" /> 图1:示意标准胶囊。该胶囊基本上由闭合丙烯酸GLAS的<html>囊体在一侧上具有熔融石英窗口，并且在相对侧上，所述柱塞保持在销安装存根在其上的样品被固定在粘合剂标签的帮助。 <a href="http://ecsource.jove.com/files/ftp_upload/54889/54889fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" class="xfigimg" src="/files/ftp_upload/54889/54889fig2.jpg" /> 图2:示意高压胶囊。的胶囊基本上由与具有拧凸缘的帮助下熔融石英窗在一侧上封闭的PEEK胶囊主体的。在另一侧，在柱塞凸缘支撑所述样品架，在其上的样品被固定在胶粘带的帮助。此胶囊是为了疏散或填充有气体的囊装有球阀。等="_空白"&gt;点击此处查看该图的放大版本。 <img alt="图3" class="xfigimg" src="/files/ftp_upload/54889/54889fig3.jpg" /> 图3:放置在显微镜载物台上的胶囊的照片。胶囊被固定在与金属环适配器的帮助阶段。在这个例子中，一个647纳米（红色）的激光束被用作激励源通过50X长焦距距离目标的低活性的测量（U，Np个）O 2克的样品（部分片段可通过胶囊中可以看出窗口）。 <a href="http://ecsource.jove.com/files/ftp_upload/54889/54889fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图4" class="xfigimg" src="/files/ftp_upload/54889/54889fig4.jpg" /> 图4:在标准C测量AMO 2的拉曼光谱apsule。 AMO 2的拉曼光谱中在大气压下在N 2下的标准和高压力胶囊和O 2的15巴分别测量。拉曼光谱显示在〜380厘米-1，这是降低AMO 2的签名激烈模式。 <a href="http://ecsource.jove.com/files/ftp_upload/54889/54889fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图5" class="xfigimg" src="/files/ftp_upload/54889/54889fig5.jpg" /> 图5:在不同的能量测量，并且提交给峰反卷积分析NPO 2的拉曼光谱。以不同的能量Np个16 O 2 的 ）拉曼光谱。 B）Np个16 O 2的第t 2G频带在2.41电子伏特测量。峰拟合和去卷积示出一个的存在在441厘米-1 dditional峰。 C）Np个16 O 2的T-2 克比较以不同的能量测量。 D）Np个16 O 2的T-2 克的比较和 NP 17 O 2在2.41电子伏特测量。 <a href="http://ecsource.jove.com/files/ftp_upload/54889/54889fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图6" class="xfigimg" src="/files/ftp_upload/54889/54889fig6.jpg" /> 图6:NPO 2温度测量和结果的总结。顶部:NP 16 O 2的斯托克斯和反斯托克斯光谱的不同的激光照射功率电平测量。中间:通过应用玻色-爱因斯坦统计斯托克斯/反斯托克斯Ť2 克峰比值作为激光IRRAD的函数来确定样本表面温度<html> iation动力。底部:在431nm -1的峰强度-1作为所计算的温度的函数。 <a href="http://ecsource.jove.com/files/ftp_upload/54889/54889fig6large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图7" class="xfigimg" src="/files/ftp_upload/54889/54889fig7.jpg" /> 图7:与拉曼测量点的位置切尔诺贝利熔岩样品的照片。样本包括大约10mm×5mm的切断在一块熔岩的1mm厚的载玻片。不同夹杂在玻璃的暗质量可以看出;他们三人已被选定作为例子。 <a href="http://ecsource.jove.com/files/ftp_upload/54889/54889fig7large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> ES / ftp_upload / 54889 / 54889fig8.jpg" /&gt; 图8: 图7 中所确定的不同相位的拉曼光谱 。拉曼光谱是从点1，2 图7的获得，和3。它们对应于硅酸盐玻璃:（U，Zr）的的SiO 4，USiO x和（U，锆）O X，分别。 <a href="http://ecsource.jove.com/files/ftp_upload/54889/54889fig8large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about A Novel Technique for Raman Analysis of Highly Radioactive Samples Using Any Standard Micro-Raman Spectrometer at JoVE.com

A Novel Technique for Raman Analysis of Highly Radioactive Samples Using Any Standard Micro-Raman Spectrometer

我们提出了一个与任何标准微拉曼光谱仪兼容高放射性的样品的拉曼光谱分析的技术，没有仪器的任何放射性污染。我们还表明使用锕系元素化合物和辐照燃料材料的一些应用。

一种新技术用于拉曼分析高放射性样品使用任何标准的微拉曼光谱仪

A novel approach for the Raman measurement of nuclear materials is reported in this paper. It consists of the enclosure of the radioactive sample in a ...

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Analytical Chemistry

Chemistry

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Molecular Vibrational Spectroscopy

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12.6K 次观看.  Joint Research Centre (JRC). 我们提出了一个与任何标准微拉曼光谱仪兼容高放射性的样品的拉曼光谱分析的技术，没有仪器的任何放射性污染。我们还表明使用锕系元素化合物和辐照燃料材料的一些应用。 

视频: A Novel Technique for Raman Analysis of Highly Radioactive Samples Using Any Standard Micro-Raman Spectrometer

Ethylene Polymerizations Using Parallel Pressure Reactors and a Kinetic Analysis of Chain Transfer Polymerization

We demonstrate a method for high-throughput catalyst screening using a parallel pressure reactor starting from the initial synthesis of a nickel &#945;-diimine ethylene polymerization catalyst. Initial polymerizations with the catalyst lead to optimized reaction conditions, including catalyst concentration, ethylene pressure and reaction time. Using gas-uptake data for these reactions, a procedure to calculate the initial rate of propagation (kp) is presented. Using the optimized conditions, the ability of the nickel &#945;-diimine polymerization catalyst to undergo chain transfer with diethylzinc (ZnEt2) during ethylene polymerization was investigated. A procedure to assess the ability of the catalyst to undergo chain transfer (from molecular weight and 13C NMR data), calculate the degree of chain transfer, and calculate chain transfer rates (ke) is presented.

A protocol for the high-throughput analysis of polymerization catalyst, chain transfer polymerizations, polyethylene characterization, and reaction kinetic analysis is presented.

乙烯聚合中使用并联电抗器的压力和链转移聚合的动力学分析

We demonstrate a method for high-throughput catalyst screening using a parallel pressure reactor starting from the initial synthesis of a nickel ...

科研

化学

A Filter-based Surface Enhanced Raman Spectroscopic Assay for Rapid Detection of Chemical Contaminants

We demonstrate a method to fabricate highly sensitive surface-enhanced Raman spectroscopic (SERS) substrates using a filter syringe system that can be applied to the detection of various chemical contaminants. Silver nanoparticles (Ag NPs) are synthesized via reduction of silver nitrate by sodium citrate. Then the NPs are aggregated by sodium chloride to form nanoclusters that could be trapped in the pores of the filter membrane. A syringe is connected to the filter holder, with a filter membrane inside. By loading the nanoclusters into the syringe and passing through the membrane, the liquid goes through the membrane but not the nanoclusters, forming a SERS-active membrane. When testing the analyte, the liquid sample is loaded into the syringe and flowed through the Ag NPs coated membrane. The analyte binds and concentrates on the Ag NPs coated membrane. Then the membrane is detached from the filter holder, air dried and measured by a Raman instrument. Here we present the study of the volume effect of Ag NPs and sample on the detection sensitivity as well as the detection of 10 ppb ferbam and 1 ppm ampicillin using the developed assay.

A procedure for fabrication and performing the filter-based surface enhanced Raman spectroscopic (SERS) assay for the detection of chemical contaminants (i.e., pesticide ferbam and antibiotic ampicillin) is presented.

基于过滤器的表面增强拉曼光谱检测方法的化学污染物快速检测

We demonstrate a method to fabricate highly sensitive surface-enhanced Raman spectroscopic (SERS) substrates using a filter syringe system that can be ...

Preparation of Biopolymer Aerogels Using Green Solvents

Although the first reports on aerogels made by Kistler1 in the 1930s dealt with aerogels from both inorganic oxides (silica and others) and biopolymers (gelatin, agar, cellulose), only recently have biomasses been recognized as an abundant source of chemically diverse macromolecules for functional aerogel materials. Biopolymer aerogels (pectin, alginate, chitosan, cellulose, etc.) exhibit both specific inheritable functions of starting biopolymers and distinctive features of aerogels (80-99% porosity and specific surface up to 800 m2/g). This synergy of properties makes biopolymer aerogels promising candidates for a wide gamut of applications such as thermal insulation, tissue engineering and regenerative medicine, drug delivery systems, functional foods, catalysts, adsorbents and sensors. This work demonstrates the use of pressurized carbon dioxide (5 MPa) for the ionic cross linking of amidated pectin into hydrogels. Initially a biopolymer/salt dispersion is prepared in water. Under pressurized CO2 conditions, the pH of the biopolymer solution is lowered to 3 which releases the crosslinking cations from the salt to bind with the biopolymer yielding hydrogels. Solvent exchange to ethanol and further supercritical CO2 drying (10 - 12 MPa) yield aerogels. Obtained aerogels are ultra-porous with low density (as low as 0.02 g/cm3), high specific surface area (350 - 500 m2/g) and pore volume (3 - 7 cm3/g for pore sizes less than 150 nm).

A new way for the production of biopolymer-based aerogels by carbon dioxide (CO2) induced gelation is shown. The technique utilizes pressurized carbon dioxide (5 MPa) for the production of biopolymer hydrogels and supercritical CO2 (12 MPa) to convert gels into aerogels. The only solvents needed besides CO2 are water and ethanol.

生物聚合物气凝胶制备使用绿色溶剂

Although the first reports on aerogels made by Kistler1 in the 1930s dealt with aerogels from both inorganic oxides (silica and others) and biopolymers ...

Using Capillary Electrophoresis to Quantify Organic Acids from Plant Tissue: A Test Case Examining Coffea arabica Seeds

Carboxylic acids are organic acids containing one or more terminal carboxyl (COOH) functional groups. Short chain carboxylic acids (SCCAs; carboxylic acids containing three to six carbons), such as malate and citrate, are critical to the proper functioning of many biological systems, where they function in cellular respiration and can serve as indicators of cell health. In foods, organic acid content can have significant impact on taste, with increased SCCA levels resulting in a sour or &#34;acid&#34; taste. Because of this, methods for the rapid analysis of organic acid levels are of particular interest to the food and beverage industries. Unfortunately, however, most methods used for SCCA quantification are dependent on time-consuming protocols requiring the derivatization of samples with hazardous reagents, followed by costly chromatographic and/or mass spectrometric analyses. This method details an alternate method for the detection and quantification of organic acids from plant material and food samples using free zonal capillary electrophoresis (CZE), sometimes simply referred to as capillary electrophoresis (CE). CZE provides a cost-effective method for measuring SCCAs with a low limit of detection (0.005 mg/ml). This article details the extraction and quantification of SCCAs from plant samples. While the method provided focuses on measurement of SCCAs from coffee beans, the method provided can be applied to multiple plant-based food materials.

Using Capillary Electrophoresis to Quantify Organic Acids from Plant Tissue: A Test Case Examining Coffea arabica Seeds

This article presents a method for the detection and quantification of organic acids from plant material using free zonal capillary electrophoresis. An example of the potential application of this method, determining the effects of a secondary fermentation on organic acid levels in coffee seeds, is provided.

利用毛细管电泳从植物组织量化有机酸:一个测试用例检查<em&gt;小粒种咖啡</em&gt;种子

Carboxylic acids are organic acids containing one or more terminal carboxyl (COOH) functional groups. Short chain carboxylic acids (SCCAs; carboxylic ...

A Practical Guide on Coupling a Scanning Mobility Sizer and Inductively Coupled Plasma Mass Spectrometer (SMPS-ICPMS)

A large variety of analytical methods are available to characterize particles in aerosols and suspensions. The choice of the appropriate technique depends on the properties to be determined. In many fields information about particle size and chemical composition are of great importance. While in aerosol techniques particle size distributions of gas-borne particles are determined online, their elemental composition is commonly analyzed offline after an appropriate sampling and preparation procedure. To obtain both types of information online and simultaneously, a hyphenated setup was recently developed, including a Scanning Mobility Particle Sizer (SMPS) and an Inductively Coupled Plasma Mass Spectrometer (ICPMS). This allows first to classify the particles with respect to their mobility diameter, and then to determine their number concentration and elemental composition in parallel. A Rotating Disk Diluter (RDD) is used as the introduction system, giving more flexibility regarding the use of different aerosol sources. In this work, a practical guide is provided describing the different steps for establishing this instrumentation, and how to use this analysis tool. The versatility of this hyphenated technique is demonstrated in example measurements on three different aerosols generated out of a) a salt solution, b) a suspension, and c) emitted by a thermal process.

A Practical Guide on Coupling a Scanning Mobility Sizer and Inductively Coupled Plasma Mass Spectrometer SMPS-ICPMS

In this work a practical guide is provided, describing the different steps to establish the coupling of SMPS and ICPMS systems, and how to use them. Three descriptive examples are presented.

耦合扫描流动性测定仪和电感耦合等离子体质谱仪（SMPS-ICPMS）的实用指南

A large variety of analytical methods are available to characterize particles in aerosols and suspensions. The choice of the appropriate technique depends ...

Real-time Breath Analysis by Using Secondary Nanoelectrospray Ionization Coupled to High Resolution Mass Spectrometry

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental exposure in a non-invasive manner. In this work, we present a protocol to characterize the exhaled VOCs in real time by using secondary nanoelectrospray ionization coupled to high resolution mass spectrometry (Sec-nanoESI-HRMS). The homemade Sec-nanoESI source was readily set up based on a commercial nanoESI source. Hundreds of peaks were observed in the background-subtracted mass spectra of exhaled breath, and the mass accuracy values are -4.0-13.5 ppm and -20.3-1.3 ppm in the positive and negative ion detection modes, respectively. The peaks were assigned with accurate elemental composition according to the accurate mass and isotopic pattern. Less than 30 s is used for one exhalation measurement, and it takes approximately 7 min for six replicated measurements.

A protocol for characterizing chemical composition of exhaled breath in real time by using secondary nanoelectrospray ionization coupled to high resolution mass spectrometry is demonstrated.

利用二次 Nanoelectrospray 电离耦合高分辨质谱的实时呼吸分析

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental ...

Observation and Analysis of Blinking Surface-enhanced Raman Scattering

From a single molecule at a silver nanoaggregate junction, blinking surface-enhanced Raman scattering (SERS) is observed. Here, a protocol is presented on how to prepare the SERS-active silver nanoaggregate, record a video of certain blinking spots in the microscopic image, and analyze the blinking statistics. In this analysis, a power law reproduces the probability distributions for bright events relative to their duration. The probability distributions for dark events are fitted by a power law with an exponential function. The parameters of the power law represent molecular behavior in both bright and dark states. The random walk model and the speed of the molecule across the entire silver surface can be estimated. It is difficult to estimate even when using averages, autocorrelation functions, and super-resolution SERS imaging. In the future, power law analyses should be combined with spectral imaging, because the origins of blinking cannot be confirmed by this analysis method alone.

This protocol describes the analysis of blinking surface-enhanced Raman scattering due to the random walk of a single molecule on a silver surface using power laws.

闪烁表面增强拉曼散射的观测与分析

From a single molecule at a silver nanoaggregate junction, blinking surface-enhanced Raman scattering (SERS) is observed. Here, a protocol is presented on ...

The MPLEx Protocol for Multi-omic Analyses of Soil Samples

Mass spectrometry (MS)-based integrated metaproteomic, metabolomic, and lipidomic (multi-omic) studies are transforming our ability to understand and characterize microbial communities in environmental and biological systems. These measurements are even enabling enhanced analyses of complex soil microbial communities, which are the most complex microbial systems known to date. Multi-omic analyses, however, do have sample preparation challenges, since separate extractions are typically needed for each omic study, thereby greatly amplifying the preparation time and amount of sample required. To address this limitation, a 3-in-1 method for the simultaneous extraction of metabolites, proteins, and lipids (MPLEx) from the same soil sample was created by adapting a solvent-based approach. This MPLEx protocol has proven to be both simple and robust for many sample types, even when utilized for limited quantities of complex soil samples. The MPLEx method also greatly enabled the rapid multi-omic measurements needed to gain a better understanding of the members of each microbial community, while evaluating the changes taking place upon biological and environmental perturbations.

A protocol is presented for simultaneously extracting metabolites, proteins, and lipids from a single soil sample, allowing reduced sample preparation times and enabling multi-omic mass spectrometry analyses of samples with limited quantities.

土壤样品多涨价可能分析的 MPLEx 协议

Mass spectrometry (MS)-based integrated metaproteomic, metabolomic, and lipidomic (multi-omic) studies are transforming our ability to understand and ...

A Facile Synthetic Method to Obtain Bismuth Oxyiodide Microspheres Highly Functional for the Photocatalytic Processes of Water Depuration

Bismuth oxyhalide (BiOI) is a promising material for sunlight-driven-environmental photocatalysis. Given that the physical structure of this kind of materials is highly related to its photocatalytic performance, it is necessary to standardize the synthetic methods in order to obtain the most functional architectures and, thus, the highest photocatalytic efficiency. Here, we report a reliable route to obtain BiOI microspheres via the solvothermal process, using Bi(NO3)3 and potassium iodide (KI) as precursors, and ethylene glycol as a template. The synthesis is standardized in a 150 mL autoclave, at 126 &#176;C for 18 h. This results in 2-3 &#181;m-sized mesoporous microspheres, with a relevant specific surface area (61.3 m2/g). Shortening the reaction times in the synthesis results in amorphous structures, while higher temperatures lead to a slight increase in the porosity of the microspheres, with no effect in the photocatalytic performance. The materials are photo-active under UV-A/visible light irradiation for the degradation of the antibiotic ciprofloxacin in water. This method has demonstrated to be effective in interlaboratory tests, obtaining similar BiOI microspheres in Mexican and Chilean research groups.

This article describes a synthetic method to obtain bismuth oxyiodide microspheres, which are highly functional to perform the photocatalytic removal of organic pollutants, such as ciprofloxacin, in water under UV-A/visible light irradiation.

一种用于水降解光催化过程的高效双氧化二碘微球合成方法

Bismuth oxyhalide (BiOI) is a promising material for sunlight-driven-environmental photocatalysis. Given that the physical structure of this kind of ...

Biological Samples Preparation for Speciation at Cryogenic Temperature using High-Resolution  X-Ray Absorption Spectroscopy

The study of elements with X-ray absorption spectroscopy (XAS) is of particular interest when studying the role of metals in biological systems. Sample preparation is a key and often complex procedure, particularly for biological samples. Although X-ray speciation techniques are widely used, no detailed protocol has been yet disseminated for users of the technique. Further, chemical state modification is of concern, and cryo-based techniques are recommended to analyze the biological samples in their near-native hydrated state to provide the maximum preservation of chemical integrity of the cells or tissues. Here, we propose a cellular preparation protocol based on cryo-preserved samples. It is demonstrated in a high energy resolution fluorescence detected X-ray absorption spectroscopy study of selenium in cancer cells and a study of iron in phytoplankton. This protocol can be used with other biological samples and other X-ray techniques that can be damaged by irradiation.

This protocol presents a detailed procedure to prepare biological cryosamples for synchrotron-based X-ray absorption spectroscopy experiments. We describe all the steps required to optimize sample preparation and cryopreservation with examples of the protocol with cancer and phytoplankton cells. This method provides a universal standard of sample cryo-preparation.

使用高分辨率X射线吸收光谱在低温下制备生物样品以进行形态分析

The study of elements with X-ray absorption spectroscopy (XAS) is of particular interest when studying the role of metals in biological systems. Sample ...