Name: measurement of outgassing rates of steels
Uploaded: 2016-12-13T15:00:00.000+00:00
Duration: 8 min 32 s
Description: Watch this Scientific Journal Video about Measurement of Outgassing Rates of Steels at JoVE.com

This work was supported jointly by the Converging Research Center Program through the Ministry of Science, ICT and Future Planning, Korea (NRF-2014M3C1A8048817) and R&amp;D Convergence Program of NST (National Research Council of Science and Technology) of Republic of Korea (CAP-14-3-KRISS).

注意:请遵守所有相关的安全做法，同时装配设备和样品室。请佩戴个人防护设备（防护眼镜，手套，安全鞋等 ）。 1.样品真空室制作<ol><li> 设计和制造的真空室的 <ol><li>准备和提交设计图纸到商业供应商或内部机械加工车间制造样品真空室。设计图纸制成S20C钢的真空室的代表性例子示于图1。在这个实验中所设计的腔室是非常基本的，并且通常由真空公司雇用。 注:制造商应具有超高真空系统的基本知识。 </li><li>检查所有的尺寸，以确保符合图纸。 </li><li>成型（加工）真空室后，覆盖月底CF法兰塑料，以防止大在运输过程中的法师。 </li></ol></li><li> 清洁的 注意:按照化学清洗过程中当地的环境，健康和安全法规。佩戴个人防护装备。处理使用PVC手套的部分。不要用裸手触摸的部分。 <ol><li>清洁以下的钢特高压清洗过程中的钢部件。一个典型的清洗程序如下所述。 </li><li>脱脂用溶剂如丙酮的部分，在室温下5分钟。 </li><li>清洗在超声浴中的部件用于使用BN清洁器（pH为13）20分钟。 </li><li>用自来水冲洗该部位10分钟，接着用去离子水彻底漂洗20分钟。 </li><li>用酒精冲洗，然后用干燥的氮气吹干。 </li><li>包装在清洁，无绒纸部分，并允许部分风干一天。 </li></ol></li><li> 焊接 注意:不要用手直接触摸的部分。我们的lder连续应在特高压焊接培训。 <ol><li>将零件焊接板凳上。 </li><li>预装的部件和对齐部件按照设计图纸。 </li><li>背面吹扫用氩气（5升/分钟），以防止在焊接期间的腐蚀。 </li><li>钉焊接使用钨惰性气体（TIG）焊接技术（氩流速:8-9升/分钟）的端部凸缘。 15 </li><li>焊接端部法兰完全采用TIG技术和车削夹具。允许热影响区冷却至室温。停止氩气流量。 </li></ol></li><li> 泄漏测试 <ol><li>密封用的CF空白凸缘该室的一端。 </li><li>另一端连接到氦气检漏仪（HLD）。 </li><li>抽空用HLD样品真空室。 </li><li>放置热焊接接缝在乙烯袋中，并充满氦气的袋子。 </li><li>测量在氦水平的任何变化。确保室防漏。氦泄漏率寿LD为&lt;1×10 - 11帕米3秒- 1（1×10 - 10毫巴大号秒- 1）。 </li><li>如果没有泄漏，宣泄室。否则，reweld真空室排气之后（重复步骤1.3.3至1.4.5）。 </li></ol></li></ol> 2.烤箱的制作<ol><li>准备并提交设计图纸给供应商或内部机械加工车间制造烤箱。参阅图2所示的画面。 </li><li>在采购特定材料/设备清单的温度控制描述所需的零件和设备。 </li><li>连接冷却线。 </li><li>供应冷却水冷却器。运行机组，检查是否漏水。停止冷水机组。 </li></ol> 3.回报率测量实验装置<ol><li>收集中指定所需的真空设备/硬件具体的材料/设备清单。测试设置主要由一个SRG的，残余气体分析仪（RGA），配备有粗加工泵（RP）的涡轮分子泵（TMP），全金属角阀（AV CH），一个三通（CF35），和减速器（CF35到CF63）。其他项目可能包括一个氦气检漏仪和特高压计，如具体的材料/设备的列表中列出。该AV 通道应具有上阀座（密封）侧的旋转法兰盘来平整的SRG。 </li><li>收集了组装所需的扳手（M6和M8），铜垫片（CF35和CF63）和螺栓/螺母（M6和M8）。 </li><li>使用工业水平仪组装SRG。 </li><li>处理使用PVC手套的部分。请勿触摸暴露用手真空表面。穿安全鞋。 </li><li>实验装置的组件<ol><li>使用铜垫片从泵侧到样品面组装真空元件顺序，如图<st荣&gt;图3。始终把阀座侧面向样品室中。拧紧所有法兰接头面对面地脸用扳手（M6）铜垫圈（CF35），除了样品室和室隔离阀（AV 通道 ）之间的联合。 </li><li>调整SRG法兰组件和样品室，使得SRG头的轴线是垂直的使用水平仪;在±2°（最大）（ 图4）。拧紧在样品室和AV CH，面与面之间的法兰接头，同时保持了SRG凸缘的水平。请参阅SRG用户的详细说明书。 </li><li>连接RP和与隔离阀的HLD（AV 滚装 ，AV HLD）的TMP的排气端的夹紧凸缘（KF）端口。 注意:确保没有机械震动的SRG法兰组装或转子。 </li></ol></li><li>泄漏测试<ol><li>打开HLD，等待探测器准备。打开AV HLD并关闭AV 罗 。 </li><li>抽空用HLD设置。请参阅HLD手册正确的操作步骤。等待〜30分钟以从安装泵出的残余的氦气。确保氦气水平是HLD的最小检测范围内。 </li><li>通过在凸缘的泄漏测试槽喷氦气。 </li><li>测量在氦水平的任何变化。确保室是密封防漏。氦泄漏率应&lt;1×10 - 11帕米3秒- 1（1×10 - 10毫巴大号秒- 1）。 </li><li>在从凸缘泄漏的情况下，应再次拧紧紧凸缘。 </li><li>如果没有发现泄漏，停止泄漏检测和排气真空系统。打开AV Ro和关闭AV HLD。 </li></ol></li></ol> 4.出气率的测量<ol&gt; <li> 抽空程序 <ol><li>通过同时接通在TMP和RP抽气真空系统。 </li><li>虽然抽工艺上，收集烘烤所需的物品;电加热器磁带，加热器控制器，手持万用表，铝箔，和温度传感器/电缆。 </li></ol></li><li> 烘烤过程 <ol><li>从法兰组件上取下SRG头。总结真空元件在带式加热器（SRG的法兰装配和TMP的入口法兰之间）。 </li><li>检查并确保有使用手持万用表加热器和真空部分之间没有电短路。 </li><li>加热器连接到相应控制器和包裹在铝箔的腔室。 </li><li>升温至150℃，在1℃-2℃/分的升温速率。 </li><li>保持在150℃的室中，使用烘烤程序控制器24-48小时。保持RGA的温度50°C以下使用电子冷却风扇。 </li><li>脱气每个RGA长丝通过电子轰击，至少5分钟的。 </li><li>测量从1 RGA光谱50米/ E要确保H 2 O峰（M / E = 18）为H 2峰（M / E = 2）小于一半。如果没有，继续烘烤。 </li><li>允许系统在1℃-2℃/分的升温速率冷却到室温。检查是否漏水指冷却过程中测得的频谱RGA。 </li><li>在样品室分析残留气体。测量RGA光谱。关闭AV 通道 ，并再次测量RGA光谱。样品室的RGA光谱对应于前和关闭该AV 通道后获得的光谱之间的差异。 </li><li>验证所有杂质气体，如的总和的 H 2 O，CO，和CO 2，在5％以下;否则，再次重复烘烤。 </li></ol></li><li> 操作SRG 注:在SRG的正确操作是很重要的。请参阅SRG操作手册的说明。 <ol><li>装配在SRG法兰装配SRG头。 </li><li>确保SRG头的轴线是在±2°（最大）（ 图4）。使用电平表，以供参考。 </li><li>启动SRG并等待残余拖累，SRG，这通常需要几个小时的压力无关信号的稳定化。 </li><li>输入正确的输入参数，如气体（H 2），温度（24℃），和测量的时间间隔（10秒）。 </li></ol></li><li> 程序发起温度控制 <ol><li>在等待信号，以稳定，稳定的样品的温度。交换机上的机组运行通过该系统冷却水。设置流体温度至15℃。 </li><li>启动用于样品的加热器控制器。设定目标温度至24℃。等待FOr处的温度在关闭炉门之后在±0.1℃下稳定。 </li></ol></li><li> 过程用于获取SRG信号 <ol><li>验证信号的偏移值的变动为±1×10内- 9帕/秒;否则，拆开从系统SRG和改变转子或法兰组件，然后重复3.5-4.4。 （如果这是不可能的，获得的8-24小时的偏移。这将是从测量放气速率数据中减去的斜率）。 </li><li>检查由SRG控制器提供的信号电平;它至少应为-10分贝。理想的是，它应该是0 dB之间和6。然而，高达12分贝值是可以接受的。如果信号是&gt;14分贝，停止SRG操作。分离的头部和加热顶针到200℃。重复从步骤4.5.1启动整个操作。 </li><li>检查由SRG控制器提供的阻尼水平;最佳值是间 -35和-60分贝，这是在使用TMP其上的橡胶垫铺设该系统和涡旋泵通常满足。否则，停止所有正在运行的设备，并移除所有的机械振动源。 </li></ol></li><li> 获取回报率数据 <ol><li>轻轻关闭AV启动压力增加。要小心，不要受到的SRG到机械冲击。 </li><li>关闭炉门和使用计算机获取压力数据为8-24小时。 </li><li>预检查所测量的数据，以验证在温度的变化是稳定后并且该压力上升为10％的误差范围内的线性内±0.1℃。如果这些条件得到满足，停止测量。否则，继续测量，直到压力上升10％的误差范围内变为线性至少16小时。 </li><li>关闭所有设备。 </li></ol></li><li> 该出气率的计算 <ol><li>选择温度STABI后设定压力补肾中药。 </li><li>使用线性最小二乘法拟合拟合压力上升数据和计算的斜率。斜率ðP / D t是压力上升的测得速率阀关闭之后。 </li><li>计算出气率，Q（H 2当量），用公式 Q =（V / A）（D P / D T）[帕米3秒- 1米 - 2] 其中，V是样品室的体积（m 3）的A是腔室（米2）的几何表面积。 </li></ol></li></ol>

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The authors have no conflict of interest to declare.

为出气率的测量许多方法已在文献中报道。实验方法包括吞吐量，电导调制，双路径，回报率，和这些方法的变体。然而，没有一种方法适合获得必要的放气数据。 10使用SRG的回报率的方法，但是，成为首选低释气材料的测定方法。 11-13 SRG 17通常被用作在高真空系统，而不错误泵送或除气作用的二级标准。使用SRG RoR的方法特别适合于烘烤后测量氢气脱气室温。相比之下?...

钢在建筑经常使用，因为其良好的机械性能。某些钢（亚铁钢，特别）是优选的材料包括真空应用。取决于类型和等级，这些钢具有足够低的出气率为高真空必不可少（HV，10 - 7 &lt;P &lt;10 - 5帕）或超高真空（UHV，10 -10 &lt;P &lt;10 - 7 Pa）的系统。此外，大量的研究已经朝着特殊的预处理程序，减少气体释放1-3的发展进行的。预处理措施旨在最小化泵送投资或改善真空从HV到UHV或从UHV极端高真空（P &lt;10 - 10帕）。 虽然许多实际的方法已被提出，以减少除气鼠亚铁钢即，最近的方法主要集中在减少，以获得较低的放气速率所需要的时间和温度。在350°C-450°热治疗C，而不是在真空800℃，950℃烧制，是这种方法的一个很好的例子。 1,4,5此外，选择理想的材料为特定真空的应用是至关重要的;例如，选择的铁素体材料具有非常低的放气速率为在磁场屏蔽使用。 6,7 在这样的调查中，放气速率的精确测量对于候选材料的筛选或验证的各种预处理程序的有效性的一个先决条件。 8,9-用于脱气测量中的最常见的实验技术是可以通过和速率的压力上升的方法。 10日前，各种实验已经进行测量基础上，采用RoR的方法旋氢出气率宁转子计（SRG）。 1，11-13使用SRG的回报率的方法是非常适合测量非常低的氢出气率，往往限制了最低压力在由钢制成的真空系统可以实现的。这是因为，SRG具有可忽略泵送或除气动作。另外，SRG还具有在高真空和超高真空范围内具有优异的精度和良好的线性。 14 鉴于上RoR的实验已发表的文献中是有限的，这是值得来描述的实验细节，开发的方法的更深入的了解。在这个视频文章中，我们详细描述了建立实验的过程，并提供了详细的说明执行使用RoR的方法放气测量。为了证明该方法的功效，之前和预热处理后测定两种常用的钢（不锈钢304和软钢S20C）的出气率降低氢outgassin摹率。前和治疗后的值进行比较。使用相当简单的设置典型的实验结果呈现演示评价低氢脱气率优化的方法的功效。

<table><tbody><tr><td>&lt;strong&gt;Sample chamber&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Stainless steel, 304</td><td>POSCO&lt;br /&gt;(www.posco.co.kr)</td><td></td><td></td></tr><tr><td>Mild steel, D3752</td><td>Xiangtan Iron&amp;amp;Steel co.,LTD (http://www.hnxg.com)</td><td></td><td></td></tr><tr><td>Mild steel, D3752</td><td>SeAh Besteel (www.seahbesteel.co.kr)</td><td></td><td></td></tr><tr><td>&lt;strong&gt;Name&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>&lt;strong&gt;Cleaning&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Cleaning bath</td><td>Samill IDS</td><td></td><td>Ultrasonic cleaning, heating, timer, concentration control&amp;nbsp;</td></tr><tr><td>Acetone</td><td>Samchun Chemical (www.samchun.com)</td><td>A1759</td><td>HPLC grade (99.7%)</td></tr><tr><td>Tekusolv</td><td>NCH Co.&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp; (www.nch.com)</td><td>0368-0058J</td><td>Solvents</td></tr><tr><td>BN cleaner</td><td>Henkel surface technologies (na.henkel-adhesives.com)</td><td>6610263775</td><td>Alkaline, pH 13</td></tr><tr><td>Ethanol</td><td>Fisher Scientific (www.fishersci.com)</td><td>A995-4</td><td>HPLC Reagent (99.9%)</td></tr><tr><td>Deionized water (Electro deionizer SYSTEM)</td><td>A.T.A&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp; (www.atagroup.co)</td><td>EDI SYSTEM</td><td></td></tr><tr><td>Liquid N&lt;sub&gt;2&lt;/sub&gt; gas</td><td>Hanyoung (www.gasmaster.co.kr)</td><td>B/T 176 L</td><td>LN&lt;sub&gt;2&lt;/sub&gt; dewar, purity 99.999%</td></tr><tr><td>&lt;strong&gt;Name&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>&lt;strong&gt;Welding&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Tungsten Inert Gas wedling machine</td><td>Thermal Arc (www.victortechnologies.com/thermalarc)</td><td>400GTSW</td><td>Ar gas preflow and postflow 8 L/min, backflow 5 L/min</td></tr><tr><td>turning jig</td><td>Vactron&lt;br /&gt;(www.vactron.co.kr)</td><td>Made to order</td><td>Made to order</td></tr><tr><td>Ar gas</td><td>Lindekorea (www.lindekorea.com)</td><td></td><td>Purity 99.999%</td></tr><tr><td>&lt;strong&gt;Name&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>&lt;strong&gt;Leak test&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Leak detector</td><td>Adixen&lt;br /&gt;(www.adixen.fr/en/)</td><td>ASM380</td><td>Pumping Speed (air): 9.7 L/sec</td></tr><tr><td>He gas</td><td>Lindekorea (www.lindekorea.com)</td><td></td><td>Purity 99.999%</td></tr><tr><td>&lt;strong&gt;Name&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>&lt;strong&gt;Vacuum equipment&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Spinning rotor gauge&amp;nbsp;</td><td>MKS Instruments (www.mks.com)</td><td>SRG-3</td><td>Controller, head, and thimble set</td></tr><tr><td>Oscilloscope</td><td>Tektronix&lt;br /&gt;(www.tek.com)</td><td>TDS2012B</td><td></td></tr><tr><td>Residulal gas analyser</td><td>Balzers</td><td>QMA200</td><td>m/e 0-100&amp;nbsp;</td></tr><tr><td>TMP (HiPace 80)</td><td>Pfeiffer Vacuum (www.pfeiffer-vacuum.com)</td><td>PMP03941</td><td>Pumping Speed (N&lt;sub&gt;2&lt;/sub&gt;): 67 L/sec</td></tr><tr><td>Scroll pump</td><td>Anest Iwata&lt;br /&gt;(www.anest-iwata.co.jp)</td><td>ISP 90</td><td>Pumping Speed (Air): 1.8 L/sec</td></tr><tr><td>All-metall easy close angle valve (CF35)</td><td>VAT Inc.&lt;br /&gt;(www.vatvalve.com)</td><td>54032-GE02-0002</td><td>Rotatable flange</td></tr><tr><td>Angle valve (KF25)</td><td>MDC Vacuum Inc. (www.mdcvacuum.com)</td><td>KAV-100</td><td></td></tr><tr><td>&lt;strong&gt;Name&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>&lt;strong&gt;Temperature control&amp;nbsp;&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Chiller</td><td>JEIO Tech&lt;br /&gt;(www.jeiotech.com)</td><td>RW-2025G</td><td></td></tr><tr><td>Cooling line</td><td>LS Metal&lt;br /&gt;(www.lsmetal.biz)</td><td>C1100</td><td>Level Wound Coil, Diameter 10 mm</td></tr><tr><td>Heater controllers</td><td>HMT</td><td>Made to order</td><td>Bakeout program controller</td></tr><tr><td>Electrical heater tapes</td><td>Brisk heat (www.briskheat.com)</td><td>BIH101080L</td><td></td></tr><tr><td>Thermocouple (K type)</td><td>miraesensor (www.miraesensor.com)</td><td>MR-2290</td><td></td></tr><tr><td>Handheld multimeter</td><td>Saehan&lt;br /&gt;(www.saehan.co.kr)</td><td>3234</td><td></td></tr><tr><td>Data recorder (Temp.)</td><td>Yokogawa (www.yokogawa.com)</td><td>GP10-1E1F-UC10</td><td></td></tr></tbody></table>

measurement of outgassing rates of steels

钢被常用材料在真空系统的制造，因为它们的良好的机械，腐蚀和真空特性。各种钢材满足低放气的高或超高真空应用所需的标准。然而，给定的材料可呈现取决于其制造过程中或在制造过程中涉及的各种前处理过程中不同出气率。因此，除气率的测量是对一个特定的真空应用高度期望的。出于这个原因，速率的压力上升（ROR）方法通常用于测量氢的烘烤后的释气。在这篇文章中，提供了设计和涉及回报率方法的实验方案的执行的详细描述。 RoR的方法使用纺纱转子计，以减少从脱气或真空计的泵送作用茎错误。两个普通钢的出气率（不锈钢和MILD钢）进行测定。该测量之前和钢的热预处理之后进行。进行钢的热预处理，以减少除气。除气极低的利率（10的顺序- 11帕米3秒- 1米 - 2）可以使用相对小样本进行常规检测。

正如预期的，烘烤后的残余气体主要是氢。 7使用SRG测得的压力上升是在相当长的时间周期（ 图5）是线性的。因此，再吸附效果可能会微不足道和用于本研究中测试的钢固有放气速率（Q）可使用的RoR方法进行评价。使用线性最小二乘拟合方法10所测得的压力上升数据进行了分析。的样品室的出气率从斜率（ 图5）确定了。 <...

Watch this Scientific Journal Video about Measurement of Outgassing Rates of Steels at JoVE.com

Measurement of Outgassing Rates of Steels

A protocol for the measurement of outgassing rates of hydrogen from ordinary steel vacuum chambers using the rate-of-pressure rise method is presented.

钢的出气率的测量

Steels are commonly used materials in the fabrication of vacuum systems because of their good mechanical, corrosion, and vacuum properties. A variety of ...

measurement-of-outgassing-rates-of-steels

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Unit 1

Units, Dimensions, and Measurements

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11.5K 次观看.  POSTECH. A protocol for the measurement of outgassing rates of hydrogen from ordinary steel vacuum chambers using the rate-of-pressure rise method is presented.

视频: Measurement of Outgassing Rates of Steels

Measurement of Greenhouse Gas Flux from Agricultural Soils Using Static Chambers

Measurement of greenhouse gas (GHG) fluxes between the soil and the atmosphere, in both managed and unmanaged ecosystems, is critical to understanding the biogeochemical drivers of climate change and to the development and evaluation of GHG mitigation strategies based on modulation of landscape management practices. The static chamber-based method described here is based on trapping gases emitted from the soil surface within a chamber and collecting samples from the chamber headspace at regular intervals for analysis by gas chromatography. Change in gas concentration over time is used to calculate flux. This method can be utilized to measure landscape-based flux of carbon dioxide, nitrous oxide, and methane, and to estimate differences between treatments or explore system dynamics over seasons or years. Infrastructure requirements are modest, but a comprehensive experimental design is essential. This method is easily deployed in the field, conforms to established guidelines, and produces data suitable to large-scale GHG emissions studies.

This article showcases the static chamber-based method for measurement of greenhouse gas flux from soil systems. With relatively modest infrastructure investments, measurements may be obtained from multiple treatments/locations and over timeframes ranging from hours to years.

从农业土壤使用静态钱伯斯温室气体流量测量

Measurement of greenhouse gas (GHG) fluxes between the soil and the atmosphere, in both managed and unmanaged ecosystems, is critical to understanding the ...

科研

环境科学

Mechanical Expansion of Steel Tubing as a Solution to Leaky Wellbores

Wellbore cement, a procedural component of wellbore completion operations, primarily provides zonal isolation and mechanical support of the metal pipe (casing), and protects metal components from corrosive fluids. These are essential for uncompromised wellbore integrity. Cements can undergo multiple forms of failure, such as debonding at the cement/rock and cement/metal interfaces, fracturing, and defects within the cement matrix. Failures and defects within the cement will ultimately lead to fluid migration, resulting in inter-zonal fluid migration and premature well abandonment. Currently, there are over 1.8 million operating wells worldwide and over one third of these wells have leak related problems defined as Sustained Casing Pressure (SCP)1. 
The focus of this research was to develop an experimental setup at bench-scale to explore the effect of mechanical manipulation of wellbore casing-cement composite samples as a potential technology for the remediation of gas leaks. 
The experimental methodology utilized in this study enabled formation of an impermeable seal at the pipe/cement interface in a simulated wellbore system. Successful nitrogen gas flow-through measurements demonstrated that an existing microannulus was sealed at laboratory experimental conditions and fluid flow prevented by mechanical manipulation of the metal/cement composite sample. Furthermore, this methodology can be applied not only for the remediation of leaky wellbores, but also in plugging and abandonment procedures as well as wellbore completions technology, and potentially preventing negative impacts of wellbores on subsurface and surface environments.

This article reports on a laboratory scale investigation of an existing field procedure and its adaptation for sealing of leaky wellbores. It consists of mechanical expansion of metal pipe, which results in an improved metal/cement bond, ultimate sealing of hydraulic pathways and prevention of gas leaks caused by the presence of a microannular channel.

钢管机械性扩张为解决井眼漏

Wellbore cement, a procedural component of wellbore completion operations, primarily provides zonal isolation and mechanical support of the metal pipe ...

工程学

Lab-Scale Model to Evaluate Odor and Gas Concentrations Emitted by Deep Bedded Pack Manure

A lab-scaled simulated bedded pack model was developed to study air quality and nutrient composition of deep-bedded packs used in cattle mono-slope facilities. This protocol has been used to effectively evaluate many different bedding materials, environmental variables (temperature, humidity), and potential mitigation treatments that can improve air quality in commercial deep-bedded mono-slope facilities. The model is dynamic and allows researchers to easily collect many chemical and physical measurements from the bedded pack. Weekly measurements, collected over the course of six to seven weeks, allows sufficient time to see changes in air quality measurements over time as the bedded pack matures. The data collected from the simulated bedded packs is within the range of concentrations previously measured in commercial deep-bedded mono-slope facilities. Past studies have demonstrated that 8 - 10 experimental units per treatment are sufficient to detect statistical differences among the simulated bedded packs. The bedded packs are easy to maintain, requiring less than 10 minutes of labor per bedded packs per week to add urine, feces, and bedding. Sample collection using the gas sampling system requires 20 - 30 minutes per bedded pack, depending on the measurements that are being collected. The use of lab-scaled bedded packs allows the researcher to control variables such as temperature, humidity, and bedding source that are difficult or impossible to control in a research or commercial facility. While not a perfect simulation of &#34;real-world&#34; conditions, the simulated bedded packs serve as a good model for researchers to use to examine treatment differences among bedded packs. Several lab-scale studies can be conducted to eliminate possible treatments before trying them in a research or commercial-sized facility.

A protocol has been developed to measure gases, odors, and nutrient composition in lab-scaled bedded manure packs, which can be used to study ways to improve air quality in commercial cattle facilities using deep-bedded manure packs.

用实验室尺度模型评价深层包粪排放的恶臭和气体浓度

A lab-scaled simulated bedded pack model was developed to study air quality and nutrient composition of deep-bedded packs used in cattle mono-slope ...

Metal Corrosion and the Efficiency of Corrosion Inhibitors in Less Conductive Media

Material corrosion can be a limiting factor for different materials in many applications. Thus, it is necessary to better understand corrosion processes, prevent them and minimize the damages associated with them. One of the most important characteristics of corrosion processes is the corrosion rate. The measurement of corrosion rates is often very difficult or even impossible especially in less conductive, non-aqueous environments such as biofuels. Here, we present five different methods for the determination of corrosion rates and the efficiency of anti-corrosion protection in biofuels: (i) a static test, (ii) a dynamic test, (iii) a static test with a reflux cooler and electrochemical measurements (iv) in a two-electrode arrangement and (v) in a three-electrode arrangement. The static test is advantageous due to its low demands on material and instrumental equipment. The dynamic test allows for the testing of corrosion rates of metallic materials at more severe conditions. The static test with a reflux cooler allows for the testing in environments with higher viscosity (e.g., engine oils) at higher temperatures in the presence of oxidation or an inert atmosphere. The electrochemical measurements provide a more comprehensive view on corrosion processes. The presented cell geometries and arrangements (the two-electrode and three-electrode systems) make it possible to perform measurements in biofuel environments without base electrolytes that could have a negative impact on the results and load them with measurement errors. The presented methods make it possible to study the corrosion aggressiveness of an environment, the corrosion resistance of metallic materials, and the efficiency of corrosion inhibitors with representative and reproducible results. The results obtained using these methods can help to understand corrosion processes in more detail to minimize the damages caused by corrosion.

The testing of processes associated with material corrosion can often be difficult especially in non-aqueous environments. Here, we present different methods for short-term and long-term testing of corrosion behavior of non-aqueous environments such as biofuels, especially those containing bioethanol.

金属腐蚀与腐蚀抑制剂在低导电介质中的效率

Material corrosion can be a limiting factor for different materials in many applications. Thus, it is necessary to better understand corrosion processes, ...

Design and Use of a Full Flow Sampling System (FFS) for the Quantification of Methane Emissions

The use of natural gas continues to grow with increased discovery and production of unconventional shale resources. At the same time, the natural gas industry faces continued scrutiny for methane emissions from across the supply chain, due to methane&#39;s relatively high global warming potential (25-84x that of carbon dioxide, according to the Energy Information Administration). Currently, a variety of techniques of varied uncertainties exists to measure or estimate methane emissions from components or facilities. Currently, only one commercial system is available for quantification of component level emissions and recent reports have highlighted its weaknesses.
In order to improve accuracy and increase measurement flexibility, we have designed, developed, and implemented a novel full flow sampling system (FFS) for quantification of methane emissions and greenhouse gases based on transportation emissions measurement principles. The FFS is a modular system that consists of an explosive-proof blower(s), mass airflow sensor(s) (MAF), thermocouple, sample probe, constant volume sampling pump, laser based greenhouse gas sensor, data acquisition device, and analysis software. Dependent upon the blower and hose configuration employed, the current FFS is able to achieve a flow rate ranging from 40 to 1,500 standard cubic feet per minute (SCFM). Utilization of laser-based sensors mitigates interference from higher hydrocarbons (C2+). Co-measurement of water vapor allows for humidity correction. The system is portable, with multiple configurations for a variety of applications ranging from being carried by a person to being mounted in a hand drawn cart, on-road vehicle bed, or from the bed of utility terrain vehicles (UTVs). The FFS is able to quantify methane emission rates with a relative uncertainty of &#177; 4.4%. The FFS has proven, real world operation for the quantification of methane emissions occurring in conventional and remote facilities.

Design and Use of a Full Flow Sampling System FFS for the Quantification of Methane Emissions

We have designed, developed, and implemented a novel full flow sampling system (FFS) for quantification of methane emissions and greenhouse gases from across the natural gas supply chain.

设计和全流采样系统（FFS）的使用甲烷排放的量化

The use of natural gas continues to grow with increased discovery and production of unconventional shale resources. At the same time, the natural gas ...

The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, building and food industries, amongst others. Polyester and coatings containing both polyester and silica nanoparticles (SiO2NPs) have been widely used to protect steel substrata from corrosion. In this study, we utilized X-ray photoelectron spectroscopy, attenuated total reflection infrared micro-spectroscopy, water contact angle measurements, optical profiling and atomic force microscopy to provide an insight into how exposure to sunlight can cause changes in the micro- and nanoscale integrity of the coatings. No significant change in surface micro-topography was detected using optical profilometry, however, statistically significant nanoscale changes to the surface were detected using atomic force microscopy. Analysis of the X-ray photoelectron spectroscopy and attenuated total reflection infrared micro-spectroscopy data revealed that degradation of the ester groups had occurred through exposure to ultraviolet light to form COO&#903;, -H2C&#903;, -O&#903;, -CO&#903; radicals. During the degradation process, CO and CO2 were also produced.

Two types of surfaces, polyester-coated steel and polyester coated with a layer of silica nanoparticles, were studied. Both surfaces were exposed to sunlight, which was found to cause substantial changes in the chemistry and nanoscale topography of the surface.

表面上的纳米硅聚酯涂料暴露在阳光下的演变

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, ...

Determining the Chemical Composition of Corrosion Inhibitor/Metal Interfaces with XPS: Minimizing Post Immersion Oxidation

An approach for acquiring more reliable X-ray photoelectron spectroscopy data from corrosion inhibitor/metal interfaces is described. More specifically, the focus is on metallic substrates immersed in acidic solutions containing organic corrosion inhibitors, as these systems can be particularly sensitive to oxidation following removal from solution. To minimize the likelihood of such degradation, samples are removed from solution within a glove box purged with inert gas, either N2 or Ar. The glove box is directly attached to the load-lock of the ultra-high vacuum X-ray photoelectron spectroscopy instrument, avoiding any exposure to the ambient laboratory atmosphere, and thus reducing the possibility of post immersion substrate oxidation. On this basis, one can be more certain that the X-ray photoelectron spectroscopy features observed are likely to be representative of the in situ submerged scenario, e.g. the oxidation state of the metal is not modified.

A protocol to avoid the oxidation of metallic substrates during sample transfer from an inhibited acidic solution to an X-ray photoelectron spectrometer is presented.

确定缓蚀剂/金属界面的化学成分与XPS:最小化后浸入氧化

An approach for acquiring more reliable X-ray photoelectron spectroscopy data from corrosion inhibitor/metal interfaces is described. More specifically, ...

化学

Applicability Analysis of Assessment Methods for Morphological Parameters of Corroded Steel Bars

The irregular and uneven residual sections along the length of a corroded steel bar substantially change its mechanical properties and significantly dominate the safety and performance of an existing concrete structure. As a result, it is important to measure the geometry and amount of corrosion of a steel bar in a structure properly to assess the residual bearing capacity and service life of the structure. This paper introduces and compares five different methods for measuring the geometry and amount of corrosion of a steel bar. A single 500 mm long and 14 mm diameter steel bar is the specimen that is subjected to accelerated corrosion in this protocol. Its morphology and the amount of corrosion were carefully measured before and after using mass loss measurements, a Vernier caliper, drainage measurements, 3D scanning, and X-ray micro-computed tomography (XCT). The applicability and suitability of these different methods were then evaluated. The results show that the Vernier caliper is the best choice for measuring the morphology of a non-corroded bar, while 3D scanning is the most suitable for quantifying the morphology of a corroded bar.

This paper measures the geometry and the amount of corrosion of a steel bar using different methods: mass loss, calipers, drainage measurements, 3D scanning, and X-ray micro-computed tomography (XCT).

钢筋形态参数评价方法的适用性分析

The irregular and uneven residual sections along the length of a corroded steel bar substantially change its mechanical properties and significantly ...

Quantitative Analysis by Thermogravimetry-Mass Spectrum Analysis for Reactions with Evolved Gases

During energy conversion, material production, and metallurgy processes, reactions often have the features of unsteadiness, multistep, and multi-intermediates. Thermogravimetry-mass spectrum (TG-MS) is seen as a powerful tool to study reaction features. However, reaction details and reaction mechanics have not been effectively obtained directly from the ion current of TG-MS. Here, we provide a method of an equivalent characteristic spectrum analysis (ECSA) for analyzing the mass spectrum and giving the mass flow rate of reaction gases as precise as possible. The ECSA can effectively separate overlapping ion peaks and then eliminate the mass discrimination and temperature-dependent effect. Two example experiments are presented: (1) the decomposition of CaCO3 with evolved gas of CO2 and the decomposition of hydromagnesite with evolved gas of CO2 and H2O, to evaluate the ECSA on single-component system measurement and (2) the thermal pyrolysis of Zhundong coal with evolved gases of inorganic gases CO, H2, and CO2, and organic gases C2H4, C2H6, C3H8, C6H14, etc., to evaluate the ECSA on multi-component system measurement. Based on the successful calibration of the characteristic spectrum and relative sensitivity of specific gas and the ECSA on mass spectrum, we demonstrate that the ECSA accurately gives the mass flow rates of each evolved gas, including organic or inorganic gases, for not only single but multi-component reactions, which cannot be implemented by the traditional measurements.

Precise determination of the evolved gases&#39; flow rate is key to study the details of reactions. We provide a novel quantitative analysis method of equivalent characteristic spectrum analysis for thermogravimetry-mass spectrum analysis by establishing the calibration system of the characteristic spectrum and relative sensitivity, for obtaining the flow rate.

热重分析-质谱分析对演化气体反应的定量分析

During energy conversion, material production, and metallurgy processes, reactions often have the features of unsteadiness, multistep, and ...

Identification and Quantification of Decomposition Mechanisms in Lithium-Ion Batteries; Input to Heat Flow Simulation for Modeling Thermal Runaway

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of thermal runaway (TR), the exothermic decomposition reactions in anode and cathode were studied, using a Simultaneous Thermal Analysis (STA)/Gas Chromatography-Mass Spectrometry (GC-MS)/Fourier Transform Infrared (FTIR) spectrometer system. These techniques allowed the identification of the reaction mechanisms in each electrode, owing to the analysis of evolved gaseous species, the amount of heat released and mass loss. These results provided insight into the thermal events happening within a broader temperature range than covered in previously published models. This allowed the formulation of an improved thermal model to depict TR. The heat of reaction, activation energy, and frequency factor (thermal triplets) for each major exothermic process at material level were investigated in a Lithium Nickel-Manganese-Cobalt-Oxide (NMC (111))-Graphite battery cell. The results were analyzed, and their kinetics were derived. These data can be used to successfully simulate the experimental heat flow.

This work aims at determining the reaction kinetics of Li-ion battery cathode and anode materials undergoing thermal runaway (TR). Simultaneous Thermal Analysis (STA)/Fourier Transform Infrared (FTIR) spectrometer/Gas Chromatography Mass Spectrometry (GC-MS) were used to reveal thermal events and to detect evolved gases.

锂离子电池分解机理的鉴定和量化;用于模拟热失控的热流仿真输入

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of ...