陈和陶都提供了大量的帮助。这项工作得到了中国主要国家研究发展计划 (2016YFC0600202) 和中国地质调查 (格兰特号) 的财政支持。DD20160183)。我们感谢匿名审阅者提出的建设性意见, 大大改善了这篇论文。

1. 样品准备
<ol><li>
样本特征
	<ol>
<li>使用 TOC 设备 (见材料表) 测量总有机碳 (toc) 的温度为20摄氏度, 相对湿度为 65% (每标准 GB/T 19145-2003)。</li>
		<li>使用光度计显微镜对页岩抛光剖面进行镜质体反射率测量 (见材料表)。</li>
	</ol>
</li>
	<li>
样品清洗和粉碎 注意: 为了避免各种内外因素的影响以及页岩的不均匀性, 本文从原水平床上用品中选取了一个大的泥岩岩样进行了试验。<ol>
<li>选择一个大的页岩岩石样品 (约20厘米长, 15 厘米宽, 2 厘米高) 从原来的水平寝具。</li>
		<li>用吸收棉、镊子和乙醛清洁样品和粉碎容器。</li>
		<li>将大型原卧页岩 beddingsample 用锤子粉碎成小块, 使其可放入残余气密磨床中。通过初步实验, 可以找到合适的粉碎时间 (约3分钟)。</li>
		<li>然后, 将样品筛入 20-40, 40-60, 60-80, 80-100, 和 100-120 标本通过第一筛分粒子通过一个 100-120 网格, 然后一个 80-100 网格, 60-80 网格, 40-60 网格, 最后 20-40 网格。</li>
		<li>丢弃任何不合格的页岩颗粒。当破碎时间为3分钟时, 将会有一些废弃的样品 (大约5克)。</li>
		<li>将每个样本标记为20-40-1、40-60-1、60-80-1、80-100-1 和 100-120-1 (这在代表结果中是 G1 的)。</li>
		<li>重复上述操作与另一个样品 (大约 20 cm 长, 15 cm 宽和 2 cm 高; 使用不同的页岩与不同的构成或 TOC), 并创建一组重复实验, 以对比。将每个示例标记为20-40-2、40-60-2、60-80-2、80-100-2 和 100-120-2 (在代表结果中 G2)。</li>
	</ol>
</li>
</ol>2. 实验方法
<ol><li>实验室设置
	<ol>
<li>将仪器放置在无电磁干扰的洁净实验室的安静无振动区域。实验室的温度应该是 10-40 °c。 注: 实验将在室温下进行, 延长时间 (多天)。</li>
		<li>使用230伏 (±10%) 和50赫兹的交流电流. 确保每个根电源线的电流大于 10 a, 并安全地处理地面引线。如果电网差, 应使用额外的电源。</li>
		<li>使用高纯度气体的气瓶 (不少于 99.999%)。牢固地固定所有钢瓶。</li>
		<li>如果实验中使用了危险气体, 确保实验室有通风和排气设施, 以及危险气体报警装置。定期使用 soap 气泡检测管道连接12中的任何泄漏。</li>
		<li>避免阳光直射。</li>
	</ol></li>
	<li>启动仪器
	<ol>
<li>在计算机上通电并启动主程序。</li>
		<li>打开气缸并调整其以适当的输出压力 (调整出气压力为 5-6 巴和气瓶压力到大约70酒吧)。</li>
		<li>打开仪器。当耦合控制器通电时, 旋钮需要保持在关闭位置。打开油浴和真空泵电源。</li>
	</ol></li>
	<li>空白测量
	<ol>
<li>拆卸样品池, 将空的清洁样品桶放入内, 并安装金属导套。检查 ZP/MP 耦合, 并将其调整到适当的状态。</li>
		<li>控制耦合控制器上的平衡, 并将其切换到 ZP/MP1/MP2 中的所有位置。观察平衡阅读的变化, 确认阅读的正常和稳定。如果读数不正确或不稳定, 则必须根据情况或支撑螺钉的高低位置调整平头4英尺的水平。</li>
		<li>装载样品池, 温控油浴夹克, 隔热盖。</li>
		<li>将耦合控制器旋钮移动到 ZP 位置。</li>
		<li>将其设置为软件中的空白测量程序。<ol>
<li>点击配置测量, 命名标题, 选择气体2和其他流体, 并选择液体浴。</li>
			<li>将试样温度设置为50摄氏度, 最大压力为70巴, 压力步骤为 7, 压力匝道为2条/分钟, 流体热至50摄氏度。 注: 对于空白测试, 使用 N2 (推荐) 或 He在适当的压力 (0-70 酒吧)。权衡空桶。当温度与吸附实验温度一致时, 启动程序运行, 通常需要 7-8 小时。最后, 在完成后可以手动获取空桶的质量和体积 (参见步骤 2.8.1)。 注意: 样品池法兰上的6套螺栓使用内部六角扳手和仪器的固定扳手拆卸。请注意, 当最后一组螺栓被移除时, 需要保持样本池以避免下落。</li>
		</ol>
</li>
	</ol></li>
	<li>仪表平衡 (如有必要) 注: 仪器的操作动作必须是软、均匀的力。<ol>
<li>不要强烈动摇平衡支持 (否则, 它可能会打乱平衡) 或移动框架的位置。当使用扳手时, 要小心不要把传感器导线管靠近法兰的位置。</li>
		<li>确认余额后, 将 ZP 移至 OFF 位置。</li>
		<li>检查示例池的法兰上的 O 形环是否已安装。如果损坏或变形严重, 请更换 O 形环。</li>
		<li>垂直设置示例池, 以便连接上、下法兰, 从而保持整体垂直状态。</li>
		<li>最后, 安装6组螺栓。<ol>
<li>使用扳手固定螺栓, 使用对称紧固方法, 以确保法兰面的连接紧密而不倾斜。6组螺栓的紧固程度应尽可能一致,13。</li>
			<li>要留心听的螺旋帽下的6组螺栓, 以保持每个边缘的法兰, 以避免困难时安装后油浴夹克。</li>
		</ol>
</li>
		<li>如果使用电加热, 安装绝缘的兵马俑, 并修复它与环形环没有外部绝缘棉包。</li>
		<li>如果使用油浴加热, 安装油浴夹克从底部到样品池, 直到顶部和上部法兰是平的。安装三螺丝在底部, 以修复油浴夹克到位。</li>
		<li>检查 ZP/MP1/MP2 位置和平衡读数是否正常, 然后将耦合控制器旋钮移动到 ZP 位置。</li>
	</ol></li>
	<li>预处理测量
	<ol>
<li>拆卸样品池, 将样品放入样品桶中。检查 ZP/MP 耦合, 并将它们调整到适当的状态。</li>
		<li>装载样品池和电热隔热盖。</li>
		<li>将耦合控制器旋钮移动到 ZP 位置。</li>
		<li>启动程序将自动运行。在软件中设置预处理程序。单击以配置测量, 命名标题, 选择真空, 选择电加热器, 将样品温度设置在150摄氏度和耦合温度20摄氏度, 并将持续时间设置为600分钟。这一步通常需要10小时。</li>
	</ol></li>
	<li>浮力测量
	<ol>
<li>拆卸电加热护套, 安装温控油浴套及隔热盖, isadhesive。</li>
		<li>在软件中启动浮力测量程序, 将油浴加热温度设在摄氏50摄氏度, 加热约4小时7的压力点, 在最大压力下将其除以70巴。启动程序将自动运行。 注: 浮力测量与空白测量相同。 注意: 在取出样品池底部的温度传感器接头前, 拔出电热电源接头。加载该示例后, 请记住检查是否插入了温度传感器。</li>
	</ol></li>
	<li>吸附测量
	<ol>
<li>在软件中设置吸附测量程序。启动程序, 它将自动运行。</li>
		<li>如果需要解吸过程, 将其设置在吸附测量程序中, 保持流体热温度在50摄氏度, 并设置19压力点 (如0, 10, 20, 40, 60, 80, 100, 150, 200, 250, 200, 150, 100, 80和0巴)。然后启动程序, 它将自动运行。</li>
		<li>当气体压力不能自动达到设定值时, 使用加压泵手动设置压力。 注意: 实验结束后, 仪器将自动排气并保持一段时间的真空状态。该程序将自动结束, 所有阀门将关闭。</li>
	</ol></li>
	<li>计算
	<ol>
<li>系统可选用以下原理自动校正实验结果。重量读数、托盘读数、样品浮力和吸附浮力的关系如下10、11、12、13: m = Δm m s + (vsc + v s + vA) X p mA: 大量吸附气体;Δm: 大量的平衡读数;mSC: 样品托盘的质量 (由空白测量获得);m: 样品质量 (通过浮力测量获得);VSC: 样品托盘容积 (通过空白测量获得);VS: 样品体积 (通过浮力测量获得);V.: 样品吸附气体量 (通过吸附测量获得);ρ (p, T, y): 密度计算的状态方程或通过测量确定。</li>
	</ol></li>
	<li>完成
	<ol>
<li>退出程序并关闭计算机。关闭实验气瓶。</li>
		<li>如果只有短时间的空转发生, 不超过3天, 停止电源的仪器, 这是不需要保持电源状态的每个系统。我们建议将耦合控制器旋钮移到关闭位置。</li>
		<li>如果仪器需要长时间停止, 则可以关闭每个系统的电源。在耦合控制器电源关闭之前, 旋钮首先需要移动到关闭位置。确认熄灭灯亮起, 其他指示灯熄灭, 然后关闭控制器电源。</li>
	</ol></li>
</ol>

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H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Adsorption+capacity+and+controlling+factors+of+the+Lower+Silurian+Longmaxi+Shale+Play+in+southern+Sichuan+Basin.">Adsorption capacity and controlling factors of the Lower Silurian Longmaxi Shale Play in southern Sichuan Basin.</a> Natural Gas Industry. 34 (12), 63-69 (2014).</li><li>Gasparik, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Geological+controls+on+the+methane+storage+capacity+in+organic-rich+shales.">Geological controls on the methane storage capacity in organic-rich shales.</a> International Journal of Coal Geology. 123 (2), 34-51 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Technically+Recoverable+Shale+Oil+and+Shale+Gas+Resources:+An+Assessment+of+137+Shale+Formations+in+41+Countries+Outside+the+United+States.">Technically Recoverable Shale Oil and Shale Gas Resources: An Assessment of 137 Shale Formations in 41 Countries Outside the United States.</a> U.S. Energy Information Administration. , (2013).</li><li>Gao, H. Q., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Isotherm+adsorption+characteristic+of+marine+and+continental+shale+and+its+controlling+factors.">Isotherm adsorption characteristic of marine and continental shale and its controlling factors.</a> Natural Gas Geoscience. 24 (6), 1290-1297 (2013).</li><li>Josh, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Laboratory+characterization+of+shale+properties.">Laboratory characterization of shale properties.</a> Journal of Petroleum Science and Engineering. 88-89 (2), 107-124 (2012).</li><li>Li, W. G., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+new+model+for+shale+adsorption+gas+amount+under+a+certain+geological+condition+of+temperature+and+pressure.">A new model for shale adsorption gas amount under a certain geological condition of temperature and pressure.</a> Natural Gas Geoscience. 23 (4), 791-796 (2012).</li><li>Robens, E., Keller, J. U., Massen, C. H., Staudt, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Sources+of+error+in+sorption+and+density+measurements.">Sources of error in sorption and density measurements.</a> Journal of Thermal Analysis and Calorimetry. 55, 383-387 (1999).</li><li>Keller, J. U., Stuart, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Gas Adsorption Equilibria: Experimental Methods and Adsorptive Isotherms. , (2005).</li><li>Ji, W. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Geological+controls+and+estimation+algorithms+of+lacustrine+shale+gas+adsorption+capacity:+A+case+study+of+the+Triassic+strata+in+the+southeastern+Ordos+Basin,+China.">Geological controls and estimation algorithms of lacustrine shale gas adsorption capacity: A case study of the Triassic strata in the southeastern Ordos Basin, China.</a> International Journal of Coal Geology. 134-135 (1), 61-73 (2014).</li><li>Liang, M. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evolution+of+pore+structure+in+gas+shale+related+to+structural+deformation.">Evolution of pore structure in gas shale related to structural deformation.</a> Fuel. 197, 310-319 (2017).</li></ol>

作者没有什么可透露的。

本实验所用材料见材料表。在去除样品池之前, 必须确认样品池中的温度和压力在常压和常温下;否则, 就会有受伤的危险。如果温度过高, 等待温度下降, 然后 removethe 样品池。如果压力过高或过低, 则手动设置软件的气压, 并使用惰性气体13、14、15。在实验期间不要拆卸样品池。实验完成后, 仪器处于待机状态。耦?...

页岩是一种粘土岩, 具有薄层的床上用品结构, 可作为页岩气源岩和储层。页岩具有很强的各向异性, 由纳米和微米的孔隙组成, 笔石化石通常被公认为1、2、3。
页岩气是中国南方长江板块的商业开采。页岩气作为一种非常规气体系统, 既用作源岩, 又作为甲烷的储层, 通过生物和/或热量过程4、5, 从页岩中的有机质中获得。储层中的天然气储存有三种形式: 孔隙和裂缝中的自由气体、有机质或无机矿物表面的吸附气体、沥青和水中溶解气体6、7。以往的研究表明, 在页岩地层中, 吸附气体占总气体的 20-85%, 为6。因此, 研究页岩的吸附能力及其控制因素对页岩气资源的勘探开发具有重要意义。
页岩的甲烷吸附能力在温度、压力、湿度、成熟度、矿物组成、有机质和特定表面积1、4、5 等方面得到了广泛的认可. ,6,7;先前的研究证实了温度、压力、湿度和甲烷吸附等外部因素之间的更大和更清晰的相关性。
然而, 研究颗粒粒度和甲烷吸附等内在因素之间的相关性是有争议的。康和纪表明, 同一页岩样品的甲烷吸附量随粒径8、14的减小而增大, 而 Rupple 和张认为颗粒粒度与吸附的相关性有限。根据等温吸附曲线9,10,11。此外, 在无页岩气吸附评价协议标准的情况下, 中国的实验室通常采用煤吸附评价协议评价页岩气的吸附。为了阐明颗粒粒度与吸附的关系, 并研究了一个远景勘探区, 本文从上扬子板块的五菱凹陷厚海洋页岩矿床中获得了页岩样品。采用重量吸附分析仪进行等温吸附 experimentand 得到颗粒尺寸与吸附的关系。
容积和重量法是测定页岩等温吸附的主要方法。容积是容积法的关键参数, 易受温度和压力12、13、14的影响。由于误差分析的不确定性, 用容积法计算吸附量的直接测量中的累积传播导致测量结果中出现较大误差, 导致异常吸附等温线14 ,15。与容积法相比, 重量法要求的参数少, 误差较小: 由于质量守恒, 重力法的重量和质量不受温度和压力12的影响。它被认为是一种比较科学、准确的测量活性炭纤维吸附量的方法。
本实验采用重量吸附分析仪, 其最大试验压力为70兆帕 (700 巴), 温度为150摄氏度。旧仪器产生的温度和压力过低 toaccurately 模拟深部地下地层的温度和压力。使用吸附分析装置的关键是达到磁悬浮平衡, 精确称量样品材料, 精度为10µg。该装置采用循环油浴加热方式, 温度范围可长期控制在0.2 摄氏度以内。旧仪器的精确度很低, 因此误差将大于用较新仪器获得的精度。实验操作用该仪器提供的软件进行。操作系统将定期更新, 以确保分析接近实际的地下条件12。
在重量法中, 采用磁悬浮平衡 (MSB) 测试了在正常温度和压力下, 试样与设备之间没有直接接触的甲烷等温吸附。样品放置在测量池中, 通过非接触悬浮耦合机构12、13, 可以将试样的重量传递到平衡。在平衡, 有一个悬浮磁铁, 由特别设计的控制器控制, 允许自由悬浮在下面的永久磁铁。永磁体将位置传感器和样品容器与联轴器架连接起来。耦合框架的作用是将样品容器耦合或解耦至永磁悬浮杆14、15、16。
我们测量的样品是在贵州省道真仡佬族苗族自治县的长的最大形成的海洋相沉积的黑色富有有机质的页岩, 下志留纪。研究区位于五菱凹陷, 上扬子板块, 毗邻四川盆地西北和雪峰山构造带, 西南17。五菱凹陷是四川盆地与雪峰山构造带之间的构造转移和过渡带, 受浅层深海陆架沉积, 在早期志留系中, 海洋黑页岩被广泛开发;当时的凹陷是由印支运动、燕山运动和喜马拉雅运动等构造事件强烈叠加而成, 形成了多级褶皱、断层和不整合面18。五菱凹陷海相黑色页岩受复杂地质条件的影响, 形成页岩气储量。作为构造传递带, 凹陷是页岩气勘探的一个亮点, 其特点是变形较弱, 页岩气的生成和保存条件较好, 而19圈闭的自然裂缝匹配较好。
高压吸附测量是在一个标准化的程序的基础上进行的, 在等温吸附设备协议的指导下, 已在若干出版物10、11中全面阐述。,12,13,14,15,16. 等温吸附实验完成于中国地质科学院页岩油气研究与评价重点实验室。用磁悬浮平衡 (MSB) 进行的重量测量是在四步骤中进行的: 空白测量、预处理、浮力测量和吸附和解吸测量 (图 1,图 2)。

<table><tbody><tr><td>XRF D8 DISCOVER X-Ray diffractometer</td><td>Brook,Germany</td><td>204458</td><td>For mineralogy X-ray diffraction</td></tr><tr><td>EBSD three element integration system with spectrum&amp;nbsp;</td><td>EDAX,USA</td><td>Trident XM4</td><td>For nanoscale imaging (SEM)</td></tr><tr><td>Mercury injection capillary pressure (MICP)</td><td>USA micromeritics Instrument company</td><td>AutoPore IV 9520</td><td>For the immersion method to measure macropores(Porosity)</td></tr><tr><td>Nitrogen gas adsorption at low temperature</td><td>USA micromeritics Instrument company</td><td>ASAP2460/2020</td><td>For the low pressure nitrogen gas adsorption to measure mesopores and micropores(BET)</td></tr><tr><td>Finnigan MAT-252 mass spectrometer</td><td>ThermoFinnigan,USA</td><td>TRQ/Y2008-004</td><td>For C isotope</td></tr><tr><td>LECO CS-230 analyzer&amp;nbsp;</td><td>Research Institute of Petroleum Exploration and Development</td><td>617-100-800</td><td>TOC apparatus</td></tr><tr><td>3Y-Leica MPV-SP photometer microphotometric system&amp;nbsp;</td><td>Leica,Germany</td><td>M090063016</td><td>Ro apparatus</td></tr><tr><td>Magnetic Suspension Balance Isothermal adsorption analyzer</td><td>Rubotherm,Germany</td><td>2015-1974CHN</td><td>For methane adsorption tests</td></tr><tr><td>Sieve(20/40/60/80/100/120mesh)</td><td>Sinopharm Chemical Reagent Beijing Co.Ltd</td><td>200*50GB6003.102012</td><td>Used to screen samples</td></tr><tr><td>Absorbent cotton, hammer, tweezers and acetaldehyde</td><td>Sinopharm Chemical Reagent Beijing Co.Ltd</td><td>standard</td><td>Used to clean materials</td></tr><tr><td>Residual gas tight grinder</td><td>Nantong Huaxing Petroleum Instrument Co., Ltd</td><td>TY2013000237</td><td>Sample smasher</td></tr></tbody></table>

experimental study of the relationship between particle size and methane sorption capacity in shale

页岩气的吸附量是页岩油气资源评价和靶区选择的关键参数, 也是评价页岩气开采价值的重要标准。目前, 关于颗粒粒度与甲烷吸附的相关性研究具有争议性。本研究采用等温吸附仪 (重量吸附分析仪) 对页岩中不同粒径的吸附能力进行测定, 以确定页岩的粒度与吸附能力之间的关系。Thegravimetric 方法需要较少的参数, 并且在精度和一致性方面比体积法等方法产生更好的结果。重量测量执行四步: 空白测量, 预处理, 浮力测量, 吸附和解吸测量。重力测量被认为是一种比较科学、准确的测定吸附量的方法;然而, 这是耗时的, 需要一个严格的测量技术。磁悬浮平衡 (MSB) 是验证该方法的准确性和一致性的关键。结果表明, 吸附能力和粒度是相关的, 但不是线性相关的, 而被筛入 40-60 和 60-80 网格的粒子中的吸附往往较大。我们建议, 在页岩气压裂中, 与颗粒尺寸相对应的最大吸附量约为250µm (60 目)。

<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57705/57705fig1.jpg"> 图 1: 在高温和高压下对重力气体的吸附实验设置.该图显示了等温吸附实验的设置: (a) 液浴用油浴加热装置;(b) 电加热的电热装置;(c) 磁悬浮平衡-重量吸附分析仪 (图 2);(d) 操作系统 (主机和显示器);和 (<...

Watch this Scientific Journal Video about Experimental Study of the Relationship Between Particle Size and Methane Sorption Capacity in Shale at JoVE.com

Experimental Study of the Relationship Between Particle Size and Methane Sorption Capacity in Shale

页岩中粒径与甲烷吸附能力关系的实验研究

采用等温吸附装置, 重量吸附分析仪, 对不同粒径的页岩的吸附能力进行了测试, 找出了泥页岩的粒度与吸附能力之间的关系。

The amount of adsorbed shale gas is a key parameter used in shale gas resource evaluation and target area selection, and it is also an important standard ...

experimental-study-relationship-between-particle-size-methane

Research

JoVE Journal

Environment

7.5K 次观看.  Chinese Academy of Geological Sciences. 采用等温吸附装置, 重量吸附分析仪, 对不同粒径的页岩的吸附能力进行了测试, 找出了泥页岩的粒度与吸附能力之间的关系。

视频: Experimental Study of the Relationship Between Particle Size and Methane Sorption Capacity in Shale

Protocol for Measuring the Thermal Properties of a Supercooled Synthetic Sand-water-gas-methane Hydrate Sample

Methane hydrates (MHs) are present in large amounts in the ocean floor and permafrost regions. Methane and hydrogen hydrates are being studied as future energy resources and energy storage media. To develop a method for gas production from natural MH-bearing sediments and hydrate-based technologies, it is imperative to understand the thermal properties of gas hydrates.
The thermal properties' measurements of samples comprising sand, water, methane, and MH are difficult because the melting heat of MH may affect the measurements. To solve this problem, we performed thermal properties' measurements at supercooled conditions during MH formation. The measurement protocol, calculation method of the saturation change, and tips for thermal constants' analysis of the sample using transient plane source techniques are described here.
The effect of the formation heat of MH on measurement is very small because the gas hydrate formation rate is very slow. This measurement method can be applied to the thermal properties of the gas hydrate-water-guest gas system, which contains hydrogen, CO2, and ozone hydrates, because the characteristic low formation rate of gas hydrate is not unique to MH. The key point of this method is the low rate of phase transition of the target material. Hence, this method may be applied to other materials having low phase-transition rates.

We present a protocol for measuring the thermal properties of synthetic hydrate-bearing sediment samples comprising sand, water, methane, and methane hydrate.

协议测量过冷的合成砂水 - 气 - 甲烷水合物样品的热性能

Methane hydrates (MHs) are present in large amounts in the ocean floor and permafrost regions. Methane and hydrogen hydrates are being studied as future ...

科研

环境科学

Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS

Different sulfur isotope compositions of authigenic pyrite typically result from the sulfate-driven anaerobic oxidation of methane (SO4-AOM) and organiclastic sulfate reduction (OSR) in marine sediments. However, unravelling the complex pyritization sequence is a challenge because of the coexistence of different sequentially formed pyrite phases. This manuscript describes a sample preparation procedure that enables the use of secondary ion mass spectroscopy (SIMS) to obtain in situ &#948;34S values of various pyrite generations. This allows researchers to constrain how SO4-AOM affects pyritization in methane-bearing sediments. SIMS analysis revealed an extreme range in &#948;34S values, spanning from -41.6 to +114.8&#8240;, which is much wider than the range of &#948;34S values obtained by the traditional bulk sulfur isotope analysis of the same samples. Pyrite in the shallow sediment mainly consists of 34S-depleted framboids, suggesting early diagenetic formation by OSR. Deeper in the sediment, more pyrite occurs as overgrowths and euhedral crystals, which display much higher SIMS &#948;34S values than the framboids. Such 34S-enriched pyrite is related to enhanced SO4-AOM at the sulfate-methane transition zone, postdating OSR. High-resolution in situ SIMS sulfur isotope analyses allow for the reconstruction of the pyritization processes, which cannot be resolved by bulk sulfur isotope analysis.

Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS

Analyses of the sulfur isotopic composition (&#948;34S) of pyrite from methane-bearing sediments have typically focused on bulk samples. Here, we applied secondary ion mass spectroscopy to analyze the &#948;34S values of various pyrite generations to understand the diagenetic history of pyritization.

原位含甲烷沉积物中自黄铁矿的制备及应用模拟器硫同位素分析

Different sulfur isotope compositions of authigenic pyrite typically result from the sulfate-driven anaerobic oxidation of methane (SO4-AOM) and ...

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 ...

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 ...

工程学

A Uniaxial Compression Experiment with CO2-Bearing Coal Using a Visualized and Constant-Volume Gas-Solid Coupling Test System

Injecting carbon dioxide (CO2) into a deep coal seam is of great significance for reducing the concentration of greenhouse gases in the atmosphere and increasing the recovery of coalbed methane. A visualized and constant-volume gas-solid coupling system is introduced here to investigate the influence of CO2 sorption on the physical and mechanical properties of coal. Being able to keep a constant volume and monitor the sample using a camera, this system offers the potential to improve instrument accuracy and analyze fracture evolution with a fractal geometry method. This paper provides all steps to perform a uniaxial compression experiment with a briquette sample in different CO2 pressures with the gas-solid coupling test system. A briquette, cold-pressed by raw coal and sodium humate cement, is loaded in high-pressure CO2, and its surface is monitored in real-time using a camera. However, the similarity between the briquette and the raw coal still needs improvement, and a flammable gas such as methane (CH4) cannot be injected for the test. The results show that CO2 sorption leads to peak strength and elastic modulus reduction of the briquette, and the fracture evolution of the briquette in a failure state indicates fractal characteristics. The strength, elastic modulus, and fractal dimension are all correlated with CO2 pressure but not with a linear correlation. The visualized and constant-volume gas-solid coupling test system can serve as a platform for experimental research about rock mechanics considering the multifield coupling effect.

A Uniaxial Compression Experiment with CO2-Bearing Coal Using a Visualized and Constant-Volume Gas-Solid Coupling Test System

This protocol demonstrates how to prepare a briquette sample and conduct a uniaxial compression experiment with a briquette in different CO2 pressures using a visualized and constant-volume gas-solid coupling test system. It also aims to investigate changes in terms of coal&#8217;s physical and mechanical properties induced by CO2 adsorption.

使用可视化和恒定体积气体-固体耦合测试系统使用 CO2轴承煤的单轴压缩实验

Injecting carbon dioxide (CO2) into a deep coal seam is of great significance for reducing the concentration of greenhouse gases in the atmosphere and ...

Methane Hydrate Crystallization on Sessile Water Droplets

This paper describes a method to form methane hydrate shells on water droplets. In addition, it provides blueprints for a pressure cell rated to 10 MPa working pressure, containing a stage for sessile droplets, a sapphire window for visualization, and temperature and pressure transducers. A pressure pump connected to a methane gas cylinder is used to pressurize the cell to 5 MPa. The cooling system is a 10 gallon (37.85 L) tank containing a 50% ethanol solution cooled via ethylene glycol through copper coils. This setup enables the observation of the temperature change associated with hydrate formation and dissociation during cooling and depressurization, respectively, as well as visualization and photography of the morphologic changes of the droplet. With this method, rapid hydrate shell formation was observed at ~-6 &#176;C to -9 &#176;C. During depressurization, a 0.2 &#176;C to 0.5 &#176;C temperature drop was observed at the pressure/temperature (P/T) stability curve due to exothermic hydrate dissociation, confirmed by visual observation of melting at the start of the temperature drop. The "memory effect" was observed after repressurizing to 5 MPa from 2 MPa. This experimental design allows the monitoring of pressure, temperature, and morphology of the droplet over time, making this a suitable method for testing various additives and substrates on hydrate morphology.

We describe a method to form gas hydrate on sessile water droplets to study the effects of various inhibitors, promoters, and substrates on the hydrate crystal morphology.

甲烷水合物在无柄水滴上的结晶

This paper describes a method to form methane hydrate shells on water droplets. In addition, it provides blueprints for a pressure cell rated to 10 MPa ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

合成纳米碳和二氧化硅矩阵的表面性能

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

化学

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 ...

A Practical and Low-Cost Setup to Measure Methane in Aqueous Samples

Measuring Dissolved Methane in Aquatic Ecosystems Using An Optical Spectroscopy Gas Analyzer

Measuring greenhouse gas (GHG) fluxes and pools in ecosystems are becoming increasingly common in ecological studies due to their relevance to climate change. With it, the need for analytical platforms adaptable to measuring different pools and fluxes within research groups also grows. This study aims to develop a procedure to use portable optical spectroscopy-based gas analyzers, originally designed and marketed for gas flux measurements, to measure GHG concentrations in aqueous samples. The protocol involves the traditional headspace equilibration technique followed by the injection of a headspace gas subsample into a chamber connected through a closed loop to the inlet and outlet ports of the gas analyzer. The chamber is fabricated from a generic mason jar and simple laboratory supplies, and it is an ideal solution for samples that may require pre-injection dilution. Methane concentrations measured with the chamber are tightly correlated (r2 &#62; 0.98) with concentrations determined separately through gas chromatography-flame ionization detection (GC-FID) on subsamples from the same vials. The procedure is particularly relevant for field studies in remote areas where chromatography equipment and supplies are not readily available, offering a practical, cheaper, and more efficient solution for measuring methane and other dissolved greenhouse gas concentrations in aquatic systems.

This study demonstrates an approach to measure methane gas concentrations in aqueous samples using portable optical analyzers coupled to an injection chamber in a closed loop. The results are similar to conventional gas chromatography, presenting a practical and low-cost alternative particularly suitable for remote field studies.

Measuring greenhouse gas (GHG) fluxes and pools in ecosystems are becoming increasingly common in ecological studies due to their relevance to climate ...

胺化化合物的浸渍和接枝到二氧化硅基材上

A Synthetic Methodology for Preparing Impregnated and Grafted Amine-Based Silica Composites for Carbon Capture

Recently, there has been a significant effort towards reducing or mitigating CO2 emissions through the use of carbon capture materials for point source or direct air capture (DAC) methods. This work focuses on amine-functionalized CO2 adsorbents for DAC. These materials show promise for CO2 removal because they have low regeneration energy consumption and high adsorption capacity. The incorporation of amine species into a porous substrate combines the advantages of the amine species&#39; affinity to CO2 with the large pore volumes and surface areas of the porous substrate. There are three methods commonly used to prepare amine-based CO2 sorbents, depending on the selection of the amine species, material support, and preparation method. These methods are impregnation, grafting, or chemical synthesis. Silica is a prevalent choice of substrate material because of its adjustable pore size, moisture tolerance, temperature stability, and ability to adsorb CO2 in low concentrations for DAC applications. Typical synthetic procedures and primary attributes of both impregnated and grafted amine-silica composites are described herein.

作者聚焦:胺基二氧化硅复合材料作为直接空气捕获的 CO2 吸附剂的标准化开发 

This work aims to facilitate the development of standardized techniques for impregnating or grafting aminated compounds onto silica substrates, which are often broadly described in the literature. Specific amounts of solvent, substrate, amines, and the values of other important experimental parameters will be discussed in detail.

一种制备浸渍接枝胺基二氧化硅复合材料的合成方法

Recently, there has been a significant effort towards reducing or mitigating CO2 emissions through the use of carbon capture materials for point source or ...