The authors would like to acknowledge support from the Government of Canada's interdepartmental Program of Energy Research and Development, PERD 113, Petroleum Conversion for Cleaner Air. N.E.H would like to acknowledge her Natural Sciences and Engineering Research Council of Canada Visiting Fellowship.

注意：使用前请咨询所有相关的材料安全数据表（MSDS）的材料。具体而言，CS 2是高度易燃的，并且被储存并适当处理。 硫化氢气体是剧毒，和任何容器或含有硫化氢气体袋不应开启或一个正确排出通风柜之外处理。随着原油样工作都必须以饱满的个人防护设备（手套，防护眼镜，实验室外套，长裤和封闭趾鞋）来完成，所有的原油样品应被打开，传送和处理在通风柜。认证的标准气体会从制造商交付与失效日期，并为最准确的结果应谨慎使用未过期的标准。 1.准备标准<ol><li>液体标准<ol><li>使用自动移液管，取10微升的二硫化碳（CS 2）到50ml volumetrIC烧瓶中。容量瓶填至用HPLC（高效液相色谱）级甲苯标记行。盖上烧瓶并通过反转和漩至少五倍混合溶液;这是500ppm的股票校准解决方案。 </li><li>上分析的每一天，准备4小瓶的CS 2的用于校准。标签41.5毫升自动进样瓶，并把它们放在一个小瓶托盘。 </li><li>使用自动移液管，免除200微升500ppm的股票CS 2溶液到每个小瓶中。使用第二自动移液器，免除800微升HPLC级甲苯到四个小瓶。在分配CS 2和甲苯后，立即盖上每个小瓶中，颠倒三次混合;这些都是100 ppm的校准标准。 </li></ol></li><li>燃气标准<ol><li>动认证校准气体的气瓶到排气通风柜，并附加装配用于附连到气囊，一个调节器。 </li><li>打开无zzle上的空气袋与气袋连接到气瓶上的调节器。 </li><li>与调节关闭时，通过转动旋钮顶部逆时针打开气瓶。 </li><li>转动旋钮上逆时针直到气体源源不断的填充气袋的调节器。当气袋是满的，转动调节旋钮顺时针关闭燃气流动。 </li><li>关闭喷嘴上的气袋和从调节器分离。转动旋钮在顶部顺时针关闭气瓶。打开调节器以清除任何剩余的气体和释放压力，然后再将它关闭时，监管机构不再有任何气体就在里面。 </li></ol></li></ol> 2，仪器设置<ol><li>方法参数<ol><li>使用以下步骤，配置院长根据设置在气体色谱仪中的列开关，因为每个系统将具有独特的压力设置。 </li><li>在计算打开开关院长计算器程序<html> r和输入柱尺寸，载气，温度，所需的流动速率使用和检测器（ 参见图1）.The计算器将定义所需的入口和压力控制模块（PCM）的压力，和限流管所需要的长度对于院长开关和火焰离子化检测器（FID）之间的安装。注意这些压力并将其输入到方法文件。 </li><li>使用来自开关的Deans计算器的信息，并在表1中的信息，节目用的气体或液体分析正确的参数的方法文件。保存方法文件。 </li></ol></li></ol><img alt="图1" src="/files/ftp_upload/53416/53416fig1.jpg" /> 院长的图1.院长开关计算器。截图转换计算器程序。用户可调参数示于白框，和输出参数以蓝色显示框。EF =“htt​​ps://www.jove.com/files/ftp_upload/53416/53416fig1large.jpg”目标=“_空白”&gt;点击此处查看该图的放大版本。 <ol start="2"><li>色谱柱安装<ol><li>确保仪器，烤箱和进口都在室温。关闭气流入口和PCM供给流向的Deans开关。 </li><li>按照制造商的说明，安装分流/不分流进样口和院长开关，院长之间的PLOT柱切换和硫化学发光检测器（SCD）之间，以及限流管（在步骤2.1.2确定长度）之间的二甲基聚硅氧烷柱院长交换机和FID。 </li><li>使用气相色谱仪软件，打开载气流到入口和PCM，并通过在每列和在院长开关末端通过一个电子检漏仪在接头的紧密接近测试系统是否泄漏;泄漏通过在DET的光及/或声音通知指示埃克特。 <ol><li>如果泄漏存在，轻轻拧紧管接头，并重新测试与电子检漏仪。关闭烤箱门，并打开气相色谱仪烤箱和进气加热器。 </li></ol></li><li>通过增加炉温到PLOT柱（发现在柱的文档）的温度上限进行烘烤列和限流管;允许烤箱坐在该温度下至少3小时的。 </li><li>当烘烤完成后，冷却该炉至RT，并重新测试该烘箱气体泄漏与电子检漏仪内部连接，紧固在必要。 </li><li>加载利用软件控制气相色谱仪的预编程的方法文件;该仪器已准备好进行分析。 </li></ol></li></ol><img alt="图2" src="/files/ftp_upload/53416/53416fig2.jpg" /> 图2.气相色谱仪烤箱。Configurati在GC柱箱柱安排。 FID：火焰离子化检测器，SCD：硫化学发光检测器<a href="https://www.jove.com/files/ftp_upload/53416/53416fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <ol start="3" style="margin-left: 0px;"><li>确定正确的院长开关时序<ol><li>作为院长开关是通过在气相色谱仪的阀控制;定位在所述方法参数的阀定时点部分。在软件，把开关设置为“ON”，并为控制院长开关阀时间的事件，与阀门在0.5分钟开启“关闭”开头，而变成“开”阀门再次在第二个事件3.0分钟。在本说明书中的“关”的位置对应于其中柱流出物将被运送到该SCD的方向。 </li><li>把这个包含校准气体的气体袋（已知的H 2 S在氦量）在通风柜，并放置一个橡胶奶嘴或同等穿透盖在气囊的喷嘴。打开上气袋的喷嘴。 </li><li>用250微升的气密玻璃注射器，穿刺橡皮奶嘴上的袋的顶部和撤回250微升校准气体。盖上注射器具有入口隔垫，并运送到注射器的气相色谱仪。 </li><li>除去从注射器的隔膜帽;手动和迅速地校准气体注入气相色谱仪，同时启动软件采集。为H 2 S会出现在SCD信号迹线的峰值;记录该峰的保留时间。 。 </li><li>开始降低心脏切割窗口的时间，一面在时间 （即，0.1分钟用于顺序注射减小阀“上”事件）;以这种方式继续，直到硫化氢峰从色谱中消失。添加0.2分钟至这个时间，并注意其作为心脏切窗口的上限。 </li><li> PERFORM对时间窗的下端相同的过程，逐渐增加所述阀的时间“关”的事件为连续喷射直到峰不再可见。减去0.2分钟从这个时候并注意其作为心脏切窗口的下限。 </li><li>保存阀“开”/“关”命令输入到方法文件。 </li></ol></li></ol> 3.仪器校准<ol><li>液体<ol><li>确保液体自动进样器被安装在气相色谱仪的分流/不分流进样口。将四个先前准备的校准小瓶在自动进样器托盘样品瓶位置1-4。 </li><li>使用玻璃吸管，填充用HPLC级甲苯的小瓶，并将其放置在用于在自动进样盘的清洗溶剂小瓶位置。确保废液瓶或水库自动进样器托盘是空的。 </li><li>加载有配置成用于连接到气体色谱软件液相分析的方法图形;确保这两个检测器被开启，并且在气体色谱仪处于准备状态。 </li><li>使用气相色谱仪软件每小瓶根据该方法来执行一个注射，并使用提供的气相色谱仪中的软件每个色谱整合在CS 2峰。 </li><li>使用电子表格程序，通过将CS 2峰的面积计算由校准溶液（100 ppm的）的浓度，然后将此除以2，得到每硫的一个原子响应计算该SCD的平均响应因子。 </li></ol></li><li>气体<ol><li>确保液体自动进样器塔已经从气相色谱仪除去，并装入用于气体分析的适当方法。确保这两个检测器被打开，并且该气相色谱仪处于准备状态。 </li><li>注入标定气体如步骤2.3.2说明2.3.4。 </li><li>重复手动注入标定气体最小的3倍。 </li><li>使用气相色谱仪的数据分析软件来整合硫化氢的峰在注射三次，并使用电子表格程序，通过用H的浓度除以的硫化氢的峰的平均面积计算为h的平均响应因子2 S的2 S在气囊。 </li></ol></li></ol> 4.样品分析<ol><li>液体<ol><li>通过将少量（&lt;1毫升）中，用玻璃移液器评估原油用于注射。如果粗传送与留在玻璃吸管无显著残余物中，将粗可以注射整齐。如果粗树叶在玻璃吸管一个显著量，稀释如在4.1.2中描述。对于可以注射整齐原油，调〜1毫升原油到气相色谱仪自动进样器小瓶中，并盖上小瓶。 </li><li>稀释高粘度的原油通过转移0.75 ml的粗的用自动移液器自动进样器小瓶中，一个次加入的HPLC级甲苯等体积。盖上盖子并翻转瓶振荡充分混合的解决方案。 </li><li>将填充的小瓶在自动进样器托盘，并加载在气体色谱仪软件的液体的分析方法。 </li><li>使用气相色谱仪的软件和以前配置方法（表1），使用自动采样器，以执行每个样品瓶三个重复注射。 </li></ol></li><li>气体<ol><li>顶空<ol><li>填写500毫升的琥珀色玻璃瓶进行分析450毫升的原油。附加一个隔膜平顶帽到瓶子的顶部。在执行排气通风柜任何原油转移步骤。 </li><li>放置瓶（多个）在温度控制的环境中，以进行分析（即，水浴30℃）。注意：原油样品可能会变得易失在升高的温度和护理应根据所用的样品来行使。 </li><li>使用1ml玻璃气密注射器，穿刺隔膜顶部并离开注射器在瓶子的顶部，以提供一个渠道压力释放，如果在顶部空间的气体应该建立。 </li><li>离开24小时，在温度控制的环境的瓶子上，轻轻提起和晃动一次一个小时瓶平衡为H液体和顶部空间之间2 S。 </li><li>分析顶空气体，穿破隔膜顶部和撤销微升气体进入气密性玻璃注射器。 </li><li>盖上注射器端用一块入口隔垫的和运输注射器向气相色谱仪。手动和迅速的气体喷入进气，同时开始以开始收集数据的软件。 </li><li>重复此过程，以获得最低的气体三次重复注射。如果H 2 S的峰过于集中，而不是在检测器的规模（ 见图 3），与气体的较小的注射器，使上规模的峰值执行的程序; 岛即，100微升或25微升。 </li></ol></li><li>气袋<ol><li>放置在气袋待分析的喷嘴的橡胶奶嘴或等效穿透罩，并将气囊在排气通风柜。 </li><li>确保正确的方法用于气体分析的气相色谱仪软件被加载，并且该气相色谱仪处于准备状态。 </li><li>打开上气袋的喷嘴，和穿刺乳头的顶端与250μl的气密注射器。填充注射器用250μl气体，撤回注射器，并关闭喷嘴上的气袋。 </li><li>盖上注射器端用一块入口隔垫的和输送到注射器的气相色谱仪，并手动将气体喷入所述入口，同时开始以开始数据收集的软件。 </li><li>重复此过程，以获得最低的气体三次重复注射。如果H 2 S的峰过于集中，并且没有被检测器的规模（See值图3），与气体的较小的注射器执行该程序以使峰上规模; 即，将100μl或25μl的。 </li></ol></li></ol></li></ol><img alt="图3" src="/files/ftp_upload/53416/53416fig3.jpg" /> 图3.气相色谱与重载H 2 s的峰值。气体注入，在30℃下保持液态原油样品，充分展示了SCD的超载的顶部空间。 <a href="https://www.jove.com/files/ftp_upload/53416/53416fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 5.数据分析<ol><li>液体<ol><li>确定硫化氢峰保留时间（只需要重复，如果仪器配置的变化） <ol><li>用玻璃吸管，以填补GC自动进样器小瓶液体粗品，确实没有牛逼需要稀释并盖上小瓶。 </li><li>加载适当的方法对气相色谱软件液体分析，并确保安装了液​​体自动进样器塔。 </li><li>放置在自动进样器托盘中的液体粗样品，并执行一次注射的原油。 </li><li>填充玻璃气密注射器750微升的 H 2 S-含氧气体（2.5％在氦）。除去从自动进样盘的小瓶中，并刺穿在与充满气体的注射器小瓶的帽隔片，并放置在管形瓶中的样品的表面下的注射器的端部。通过粗制样品压下柱塞上的注射器以气泡的气体。 </li><li>将小瓶放回自动进样器托盘和使用该软件直接自动进样器进行单注加标样品。 </li><li>利用伴随气相色谱仪的软件，前和H 2 S的穗后比较的色谱图。一个大的峰值应预先<html>发送，这是不存在于所述第一色谱图中的第二色谱图记录该峰的保留时间（参见图4）。 </li></ol></li><li>分析<ol><li>使用数据分析软件附带的气相色谱仪来整合峰面积的 H 2 S（识别使用在步骤5.1.1.6指出的保持时间）中的每个色谱图（ 图5），并计算平均峰面积用于与每个样本电子表格程序。 </li><li>使用在3.1节中确定的响应因子，由响应因子除以所述平均峰面积为样品，得到的H存在以ppm 2 S的量。用于稀释该样品，通过正确的稀释因子乘以浓度，得到的 H 2 S的未稀释的样品中的量（图6）。 </li></ol></li></ol></li></ol>上传/ 53416 / 53416fig4.jpg“/&gt; 图4.原油样品掺入H 2 S.两个叠加色谱图说明扣球与H 2粗样品S.当预期的变化<a href="https://www.jove.com/files/ftp_upload/53416/53416fig4large.jpg" target="_blank">，请点击此处查看该图的放大版本。</a> <img alt="图5" src="/files/ftp_upload/53416/53416fig5.jpg" /> 使用图5气相色谱数据分析，数据分析程序突出一个样品和峰面积在H 2 S峰值的位置的屏幕截图，以确定H 2的浓度S. <a href="https://www.jove.com/files/ftp_upload/53416/53416fig5large.jpg" target="_blank">请点击此处查看大图版本这个数字。请点击他</a>再查看该图的放大版本。 <img alt="图6" src="/files/ftp_upload/53416/53416fig6.jpg" /> 图6.示例电子表格进行数据分析。电子表格程序显示了如何计算使用校正标准峰的面积和样品的峰面积H 2 S的浓度的例子的截图。 <a href="https://www.jove.com/files/ftp_upload/53416/53416fig6large.jpg" target="_blank">请点击此处查看更大的版本这个数字。</a> <ol start="2"><li>气体<ol><li>通过匹配用在3.2节以校准硫化氢峰的保留时间确定每个色谱的硫化氢的峰。 </li><li>使用数据分析软件附带的气相色谱仪，以整合的峰面积为在所收集的数据为H 2 S的峰，并计算平均峰面积为每个样品。 </li><li>使用响应因子determin编在第3.2节，除以平均峰面积为样品由响应因子，得到H存在以ppm 2 S的量。对于所使用的更小的注射器容量，通过正确的稀释因子乘以浓度，得到的 H 2 S的将存在于250微升注射器的量的样品（即，（250微升/ 25微升为一25微升注射器）。 </li></ol></li></ol>

<ol>
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The authors have nothing to disclose.

为了达到硫化氢的最佳的测量，该方法使用的Deans开关，反冲和硫化学发光检测器（SCD）。甲二甲基聚硅氧烷列用作第一维GC柱，并用于延缓样品中存在的较重烃的流动，使它们不会污染PLOT柱。这种效果是通过一个凉（50℃）初步分离增强。光气体通过第一维列和由心脏切进​​一步分离期间PLOT柱捕获。在SCD只响应含硫化合物，加入选择性的附加 ​​层，和防止干扰通过任何烃或其他的?...

原油的准确的分析是对石油和天然气工业必不可少的，健康和安全法规和经济性油质量的功能。为了保障原油样品的运输，有必要确定原油样品的特性制定安全法规将在释放或溢出的情况下实现的。具体地，硫化氢量化（H 2 S）是重要的，由于在气相中的高毒性;曝光低至100 ppm的可致命（http://www.cdc.gov/niosh/idlh/7783064.html）1,2。溶解硫化氢粗样品中通常被认为是腐蚀性的3,4，和可以停用用于处理油5-7的催化剂。从原油流除去硫化氢的是理想的，但没有一种方法来测量溶解的 H 2 S，这是难以评估的去除治疗的成功。由于这些原因，该协议被开发用于测量dissoLVED 硫化氢重质原油样品中如加拿大的油砂的原油。 为硫化氢的量化打火机基于石油或燃料样品中的许多标准方法存在的，但都没有被验证为与重质原油从加拿大的油砂通常提取中使用。 的 H 2 S和硫醇使用由通用石油产品（UOP）方法163 8滴定技术确定，但这种方法从用户解释偏压导致从滴定曲线的手动阅读受到影响。石油（IP）的方法570研究所采用的是专业硫化氢分析仪，加热燃油样品9，并从简单性和便携性的好处，但缺少准确性较重的样品10。美国社会测试和材料协会（ASTM）方法D5623使用气相色谱（GC）用低温冷却和硫选择性检测来测量的 H 2 S在光石油液体11,12。这个标准可以改善使用环境分离和也可以应用到重质原油，因此它被用来作为基础本文所讨论的协议。 GC是一个频繁使用的技术石油样品的分析。样品被蒸发在热入口和分离发生在气相中。气相分离使得GC理想的 H 2 S的分析，因为它是从液体样品加热在入口时容易释放出来。气相色谱方法可以创建并针对不同的样品，根据所使用的温度程序，柱实现，并且使用多维色谱13-15中 。已经有一些最近的事态发展，使用GC H 2 S的测量。 。良等证实 的 H 2 S和其它轻质硫化合物测量在光线和中间馏分使用多维GC和院长切换，但该方法具有不尚未应用到重质原油16。二三藏等人还定量ħ用GC，2 S在汽油然而它也还没有被使用于重质原油，并且需要子周围冷却17。该方法提出这里演示相当多的时间节省了这些以前的方法，用5分钟的完成分析的时间，相对于10分钟（良）和40分钟（迪三藏）。不幸的是，落实在我们的实验室进行比较准确这些方法是不可能的，由于设备和时间的限制。 多维气相色谱允许用户利用两列的选择性，而不是单一的塔。在传统的气相色谱，分离发生在一列。在多维气相色谱的情况下，将样品上分离两个不同的列，增强了分离和选择性。院长开关是用于采用一个两维列配置中的一个装置。该开关使用外部阀门可怕从到的两个出口18-20之一交换机上的入口克拉气流。从第一塔流出物可以被定向在两个方向上;在这种情况下，光硫气体是“心脏切”21从第一分离到多孔层开管（PLOT）柱进行二次分离，这已被证明是非常适合的H分离来自其他光硫气体2 S的 （http://www.chem.agilent.com/cag/cabu/pdf/gaspro.pdf）22-24。甲硫化学发光检测器用于检测，提供选择性硫化合物和消除可能干扰从可能已经在心脏切期间被转移到PLOT柱任何其他轻质气体。从原油样品烃被保留在第一维列和反吹过程期间被除去;这种保护的情节列从任何污染25-27。这种方法也被成功地实施了肛门氧化抑制剂的变压器油28 ysis。 这里，二维气相色谱方法用于重质原油样品中的分析和溶解硫化氢的定量。该方法被证明是适用在宽范围H 2 S的浓度，并且也可以被用于测量硫化氢气体相位样本在。

<table border="0" cellpadding="0" cellspacing="0" width="700">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Deans switch</td>
			<td style="width:199px;">Agilent</td>
			<td style="width:119px;">G2855A</td>
			<td style="width:167px;">Or equivalent flow switching device</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Restrictor tubing&#160;</td>
			<td style="width:199px;">Agilent</td>
			<td style="width:119px;">160-2615-10</td>
			<td style="width:167px;">Fused silica, deactivated, 180 &#181;m</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">HP-PONA column</td>
			<td style="width:199px;">Agilent</td>
			<td style="width:119px;">19091S-001</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">GasPro column</td>
			<td style="width:199px;">Agilent</td>
			<td style="width:119px;">113-4332</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Sulfur chemiluminescence detector, 355</td>
			<td style="width:199px;">Agilent/Sievers</td>
			<td style="width:119px;">G6603A</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:216px;">H2S calibration standard, in He</td>
			<td style="width:199px;">Air Liquide</td>
			<td style="width:119px;">Custom order</td>
			<td style="width:167px;">211 ppm H2S</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:216px;">CS2</td>
			<td style="width:199px;">Fisher Scientific</td>
			<td style="width:119px;">C184-500</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Toluene, HPLC grade</td>
			<td style="width:199px;">Fisher Scientific</td>
			<td style="width:119px;">T290-4</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Gas bag, 2 L</td>
			<td style="width:199px;">Calibrated Instruments, Inc.</td>
			<td style="width:119px;">GSB-P/2</td>
			<td style="width:167px;">Twist on/off nozzle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">250 &#181;L gas tight syringe</td>
			<td style="width:199px;">Hamilton</td>
			<td style="width:119px;">81130</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">500 mL amber glass bottle</td>
			<td style="width:199px;">Scientific Specialties</td>
			<td style="width:119px;">N73616</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Open top screw caps</td>
			<td style="width:199px;">Scientific Specialties</td>
			<td style="width:119px;">169628</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Tegrabond disc for screw caps</td>
			<td style="width:199px;">Chromatographic Specialties</td>
			<td style="width:119px;">C889125C</td>
			<td style="width:167px;">25 mm, 10/90 MIL</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">1 mL gas tight syringe</td>
			<td style="width:199px;">Hamilton</td>
			<td style="width:119px;">81330</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:216px;">2.5% H2S in He gas standard</td>
			<td style="width:199px;">Air Liquide</td>
			<td style="width:119px;">Custom order</td>
			<td style="width:167px;"></td>
		</tr>
	</tbody>
</table>

measurement of h2s in crude oil and crude oil headspace using multidimensional gas chromatography, deans switching and sulfur-selective detection

使用一种用于溶解的硫化氢的原油样品中的分析方法中证明气相色谱。为了有效地消除干扰，一个两维列配置的情况下，与用来从所述第一转移硫化氢到第二列（心脏切割）一个的Deans开关。液体粗采样首先分离二甲基聚硅氧烷柱，和轻质气体是心脏切割，并进一步上分离键合的多孔层开管（PLOT）柱，其能够从其他光含硫物质分离硫化氢。硫化氢然后用硫化学发光检测器检测，添加选择性的附加层。以下分离和检测的硫化氢，系统被反冲以除去存在于粗样品中的高沸点烃和保留色谱完整性。溶解的硫化氢已量化液体样品中为1.1至500 p下午，展示出广泛的应用到各种样品。该方法也已成功地用于气体样品从原油顶部空间和工艺气体袋进行分析，以测量在0.7至9700 ppm的硫化氢。

为了得到硫化氢的液体和气体样品可靠的量化，适当的校准是必要的。用于校准注射和样品注射时，H 2 S的峰不应当重叠与相邻峰和应该具有可再现的峰面积。 图3示出了注入一个气体样品，其中气体过于集中于该方法的。已经发现，大于500ppm的使用250微升注射器气体浓度过载探测器。这个问题是没有遇到过的液体样品，如气相浓度的硫化氢普遍要比液体较高?...

Watch this Scientific Journal Video about Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection at JoVE.com

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

A multidimensional gas chromatography method for the analysis of dissolved hydrogen sulfide in liquid crude oil samples is presented. A Deans switch is used to heart-cut light sulfur gases for separation on a secondary column and detection on a sulfur chemiluminescence detector.

h的测量<sub&gt; 2</sub&gt; S在原油和原油顶空用多维气相色谱法，院长交换和选择性硫检测

A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate ...

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Environment

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

19.0K 次观看.  Natural Resources Canada. A multidimensional gas chromatography method for the analysis of dissolved hydrogen sulfide in liquid crude oil samples is presented. A Deans switch is used to heart-cut light sulfur gases for separation on a secondary column and detection on a sulfur chemiluminescence detector. 

视频: Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Optimize Flue Gas Settings to Promote Microalgae Growth in Photobioreactors via Computer Simulations

Flue gas from power plants can promote algal cultivation and reduce greenhouse gas emissions1. Microalgae not only capture solar energy more efficiently than plants3, but also synthesize advanced biofuels2-4. Generally, atmospheric CO2 is not a sufficient source for supporting maximal algal growth5. On the other hand, the high concentrations of CO2 in industrial exhaust gases have adverse effects on algal physiology. Consequently, both cultivation conditions (such as nutrients and light) and the control of the flue gas flow into the photo-bioreactors are important to develop an efficient &ldquo;flue gas to algae&rdquo; system. Researchers have proposed different photobioreactor configurations4,6 and cultivation strategies7,8 with flue gas. Here, we present a protocol that demonstrates how to use models to predict the microalgal growth in response to flue gas settings. We perform both experimental illustration and model simulations to determine the favorable conditions for algal growth with flue gas. We develop a Monod-based model coupled with mass transfer and light intensity equations to simulate the microalgal growth in a homogenous photo-bioreactor. The model simulation compares algal growth and flue gas consumptions under different flue-gas settings. The model illustrates: 1) how algal growth is influenced by different volumetric mass transfer coefficients of CO2; 2) how we can find optimal CO2 concentration for algal growth via the dynamic optimization approach (DOA); 3) how we can design a rectangular on-off flue gas pulse to promote algal biomass growth and to reduce the usage of flue gas. On the experimental side, we present a protocol for growing Chlorella under the flue gas (generated by natural gas combustion). The experimental results qualitatively validate the model predictions that the high frequency flue gas pulses can significantly improve algal cultivation.

Flue gas from power plants is a cheap CO2 source for algal growth. We have built prototype &#34;flue gas to algal cultivation&#34; systems and described how to scale up the algal cultivation process. We have demonstrated the use of a mass-transfer bio-reaction model to simulate and to design the optimal operation of flue gas for the growth of Chlorella sp. in algal photo-bioreactors.

优化烟气设置通过电脑模拟来促进微藻生长的光生物反应器中

Flue gas from power plants can promote algal cultivation and reduce greenhouse gas emissions1. Microalgae not only capture solar energy more efficiently ...

科研

环境科学

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 ...

EPA Method 1615. Measurement of Enterovirus and Norovirus Occurrence in Water by Culture and RT-qPCR. Part III. Virus Detection by RT-qPCR

EPA Method 1615 measures enteroviruses and noroviruses present in environmental and drinking waters. This method was developed with the goal of having a standardized method for use in multiple analytical laboratories during monitoring period 3 of the Unregulated Contaminant Monitoring Rule. Herein we present the protocol for extraction of viral ribonucleic acid (RNA) from water sample concentrates and for quantitatively measuring enterovirus and norovirus concentrations using reverse transcription-quantitative PCR (RT-qPCR). Virus concentrations for the molecular assay are calculated in terms of genomic copies of viral RNA per liter based upon a standard curve. The method uses a number of quality controls to increase data quality and to reduce interlaboratory and intralaboratory variation. The method has been evaluated by examining virus recovery from ground and reagent grade waters seeded with poliovirus type 3 and murine norovirus as a surrogate for human noroviruses. Mean poliovirus recoveries were 20% in groundwaters and 44% in reagent grade water. Mean murine norovirus recoveries with the RT-qPCR assay were 30% in groundwaters and 4% in reagent grade water.

Here we present a procedure to quantify enterovirus and norovirus in environmental and drinking waters using reverse transcription-quantitative PCR. Mean virus recovery from groundwater with this standardized procedure from EPA Method 1615 was 20% for poliovirus and 30% for murine norovirus.

EPA方法1615测量肠道病毒和诺瓦克病毒发生水由文化和RT-qPCR的了。第三部分。病毒检测用RT-qPCR的

EPA Method 1615 measures enteroviruses and noroviruses present in environmental and drinking waters. This method was developed with the goal of having a ...

Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system requires the careful preparation of the sample in order to accurately replicate the natural formation of the water-accommodated fraction that occurs in nature. Low-energy water-accommodated fractions (LEWAF) are carefully prepared by mixing crude oil and water at a set ratio. Aspirator bottles are then irradiated, and at set time points, the water is sampled and extracted using standard techniques. A second challenge is the representative characterization of the sample, which must take into consideration the chemical changes that occur over time. A targeted analysis of the aromatic fraction of the LEWAF can be performed using an atmospheric-pressure laser ionization source coupled to a custom-built trapped ion mobility spectrometry&#8211;Fourier transform&#8211;ion cyclotron resonance mass spectrometer (TIMS-FT-ICR MS). The TIMS-FT-ICR MS analysis provides high-resolution ion mobility and ultrahigh-resolution MS analysis, which further allow the identification of isomeric components by their collision cross-sections (CCS) and chemical formula. Results show that as the oil-water mixture is exposed to light, there is significant photo-solubilization of the surface oil into the water. Over time, the chemical transformation of the solubilized molecules takes place, with a decrease in the number of identifications of nitrogen- and sulfur-bearing species in favor of those with a greater oxygen content than were typically observed in the base oil.

The low-energy water-accommodated fraction (LEWAF) of crude oil is a challenging system to analyze, because over time, this complex mixture undergoes chemical transformations. This protocol illustrates methods for the preparation of the LEWAF sample and for performing photo-irradiation and chemical analysis by trapped ion mobility spectrometry&#8211;FT-ICR MS.

原油水容纳组分的化学分析泄漏使用TIMS-FT-ICR MS

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system ...

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The system comprises a high-pressure rheometer which is connected to a circulation loop. The rheometer has a rotational flow-through measurement cell with two alternative geometries: coaxial cylinder and double gap. The circulation loop contains a mixer, to bring the crude oil sample into equilibrium with CO2, and a gear pump that transports the mixture from the mixer to the rheometer and recycles it back to the mixer. The CO2 and crude oil are brought to equilibrium by stirring and circulation and the rheology of the saturated mixture is measured by the rheometer. The system is used to measure the rheological properties of Zuata crude oil (and its toluene dilution) in equilibrium with CO2 at elevated pressures up to 220 bar and a temperature of 50 &#176;C. The results show that CO2 addition changes the oil rheology significantly, initially reducing the viscosity as the CO2 pressure is increased and then increasing the viscosity above a threshold pressure. The non-Newtonian response of the crude is also seen to change with the addition of CO2.

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

A method for measuring the rheology of crude oil in equilibrium with carbon dioxide at reservoir conditions is presented.

与CO平衡的原油流变学测量<sub&gt; 2</sub&gt;在水库条件

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The ...

Microfluidic Devices for Characterizing Pore-scale Event Processes in Porous Media for Oil Recovery Applications

Microfluidic devices are versatile tools for studying transport processes at a microscopic scale. A demand exists for microfluidic devices that are resistant to low molecular-weight oil components, unlike traditional polydimethylsiloxane (PDMS) devices. Here, we demonstrate a facile method for making a device with this property, and we use the product of this protocol for examining the pore-scale mechanisms by which foam recovers crude oil. A pattern is first designed using computer-aided design (CAD) software and printed on a transparency with a high-resolution printer. This pattern is then transferred to a photoresist via a lithography procedure. PDMS is cast on the pattern, cured in an oven, and removed to obtain a mold. A thiol-ene crosslinking polymer, commonly used as an optical adhesive (OA), is then poured onto the mold and cured under UV light. The PDMS mold is peeled away from the optical adhesive cast. A glass substrate is then prepared, and the two halves of the device are bonded together. Optical adhesive-based devices are more robust than traditional PDMS microfluidic devices. The epoxy structure is resistant to swelling by many organic solvents, which opens new possibilities for experiments involving light organic liquids. Additionally, the surface wettability behavior of these devices is more stable than that of PDMS. The construction of optical adhesive microfluidic devices is simple, yet requires incrementally more effort than the making of PDMS-based devices. Also, though optical adhesive devices are stable in organic liquids, they may exhibit reduced bond-strength after a long time. Optical adhesive microfluidic devices can be made in geometries that act as 2-D micromodels for porous media. These devices are applied in the study of oil displacement to improve our understanding of the pore-scale mechanisms involved in enhanced oil recovery and aquifer remediation.

The goal of this procedure is to easily and rapidly produce a microfluidic device with customizable geometry and resistance to swelling by organic fluids for oil recovery studies. A polydimethylsiloxane mold is first generated, and then used to cast the epoxy-based device. A representative displacement study is reported.

微流体器件用于表征多孔介质中的孔隙尺度事件过程, 用于采油应用

Microfluidic devices are versatile tools for studying transport processes at a microscopic scale. A demand exists for microfluidic devices that are ...

Assessment of Methane and Nitrous Oxide Fluxes from Paddy Field by Means of Static Closed Chambers Maintaining Plants Within Headspace

This protocol describes the measurement of greenhouse gas (GHG) emissions from paddy soils using the static closed chamber technique. This method is based on the diffusion theory. A known volume of air overlaying a defined soil area is enclosed within a parallelepiped cover (named &#34;chamber&#34;), for a defined period of time. During this enclosure period, gases (methane (CH4) and nitrous oxide (N2O)) move from soil pore air near their microbial source (i.e., methanogens, nitrifiers, denitrifiers) to the chamber headspace, following a natural concentration gradient. Fluxes are then estimated from chamber headspace concentration variations sampled at regular intervals throughout the enclosure and then analyzed with gas chromatography. Among the techniques available for GHG measurement, the static closed chamber method is suitable for plot experiments, as it does not require large homogenously treated soil areas. Furthermore, it is manageable with limited resources and can identify relationships among ecosystem properties, processes, and fluxes, especially when combined with GHG driving force measurements. Nevertheless, with respect to the micrometeorological method, it causes a minimal but still unavoidable soil disturbance, and allows a minor temporal resolution. Several phases are key to the method implementation: i) chamber design and deployment, ii) sample handling and analyses, and iii) flux estimation. Technique implementation success in paddy fields demands adjustments for field flooding during much of the cropping cycle, and for rice plant maintenance within the chamber headspace during measurements. Therefore, the additional elements to be considered with respect to the usual application of non-flooded agricultural soils consist of devices for: i) avoiding any unintended water disturbance that could overestimate fluxes, and ii) including rice plants within the chamber headspace to fully consider gases emitted through aerenchyma transportation.

The overall goal of this protocol is to measure greenhouse gas emissions from paddy fields using the static closed chamber technique. The measurement system needs specific adjustments due to the presence of both a permanent water layer in the field and of the plants within the chamber headspace.

用静止封闭室维持顶空装置对稻田甲烷和一氧化二氮通量的评价

This protocol describes the measurement of greenhouse gas (GHG) emissions from paddy soils using the static closed chamber technique. This method is based ...

The Effect of the Application of Thyme Essential Oil on Microbial Load During Meat Drying

Meat is a high protein meal that is used in the preparation of jerky, a popular food snack, where preservation and safety are important. To assure food safety and to extend the shelf life of meat and meat products, the use of either synthetic or natural preservatives have been applied to control and eliminate foodborne bacteria. A growing interest in the application of natural food additives for meat has increased. Microorganisms, such as Escherichia coli, contaminate meat and meat products, causing foodborne illnesses. Therefore, it is necessary to improve the meat conservation process. However, the use of essential oils when the meat is being dried has not been deeply studied. In this regard, there is an opportunity to increase the value of dried meat and reduce the risk of foodborne illnesses by applying essential oils during the drying process. In this protocol, we present a novel method of applying thyme essential oil (TEO) during meat drying, specifically in vapor form directly in a drying chamber. For evaluation, we use Minimal Inhibitory Concentration (MIC) to detect the number of harmful bacteria in the treated samples compared to raw samples. The preliminary results show that this method is a viable and alternative option to synthetic preservatives and that it significantly reduces microbial load in dried meat.

Microorganisms such as Escherichia coli that contaminate meat products cause foodborne illnesses. The use of essential oils in the meat drying process has not been deeply studied. Here, we present a novel method of applying thyme essential oil to meat during drying to reduce the microbial load in dried meat.

百里香精油应用于肉类干燥过程中微生物负荷的影响

Meat is a high protein meal that is used in the preparation of jerky, a popular food snack, where preservation and safety are important. To assure food ...

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

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 for evaluating the mining value of shale gas. Currently, studies on the correlation between particle size and methane adsorption are controversial. In this study, an isothermal adsorption apparatus, the gravimetric sorption analyzer, is used to test the adsorption capacity of different particle sizes in shale to determine the relationship between the particle size and the adsorption capacity of shale. Thegravimetric method requires fewer parameters and produces better results in terms of accuracy and consistency than methods like the volumetric method. Gravimetric measurements are performed in four steps: a blank measurement, preprocessing, a buoyancy measurement, and adsorption and desorption measurements. Gravimetric measurement is presently considered to be a more scientific and accurate method of measuring the amount of adsorption; however, it is time-consuming and requires a strict measuring technique. A Magnetic Suspension Balance (MSB) is the key to verify the accuracy and consistency of this method. Our results show that adsorption capacity and particle size are correlated, but not a linear correlation, and the adsorptions in particles sieved into 40 - 60 and 60 - 80 meshes tend to be larger. We propose that the maximum adsorption corresponding to the particle size is approximately 250 &#181;m (60 mesh) in the shale gas fracturing.

We use an isothermal adsorption apparatus, the gravimetric sorption analyzer, to test the adsorption capacity of different particle sizes of shale, in order to find out the relationship between particle size and the adsorption capacity of shale.

页岩中粒径与甲烷吸附能力关系的实验研究

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 ...

Detection of Viruses from Bioaerosols Using Anion Exchange Resin

This protocol demonstrates a customized bioaerosol sampling method for viruses. In this system, anion exchange resin is coupled with liquid impingement-based air sampling devices for efficacious concentration of negatively-charged viruses from bioaerosols. Thus, the resin serves as an additional concentration step in the bioaerosol sampling workflow. Nucleic acid extraction of the viral particles is then performed directly from the anion exchange resin, with the resulting sample suitable for molecular analyses. Further, this protocol describes a custom-built bioaerosol chamber capable of generating virus-laden bioaerosols under a variety of environmental conditions and allowing for continuous monitoring of environmental variables such as temperature, humidity, wind speed, and aerosol mass concentration. The main advantage of using this protocol is increased sensitivity of viral detection, as assessed via direct comparison to an unmodified conventional liquid impinger. Other advantages include the potential to concentrate diverse negatively-charged viruses, the low cost of anion exchange resin (~$0.14 per sample), and ease of use. Disadvantages include the inability of this protocol to assess infectivity of resin-adsorbed viral particles, and potentially the need for the optimization of the liquid sampling buffer used within the impinger.

An anion exchange resin-based method, adapted to liquid impingement-based bioaerosol sampling of viruses is demonstrated. When coupled with downstream molecular detection, the method allows for facile and sensitive detection of viruses from bioaerosols.