化学吸附仪的测试原理和操作方法

<h1 style="font-size: 1.25em; margin: 0.63em 0px 1.8em; border: 0px; padding: 0px; color: #191919; line-height: 38px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">一、化学吸附仪的基本功能</span></h1> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;"><span style="color: #236fa1;"><a style="color: #236fa1;" title="化学吸附分析仪（TPD/TPR/TPO）" href="https://www.kexingtest.com/instrument/detail?id=115" target="_blank" rel="noopener">化学吸附仪</a></span>具有多种表征功能，能够对新鲜催化剂进行程序升温脱附(TPD)、程序升温还原（TPR)、程序升温表面反应（TPSR)等研究，也可对失活催化剂、干燥催化剂进行程序升温氧化（TPO）研究。利用化学吸附仪中的脉冲吸附技术还可对催化剂的酸性、表面金属分散度、金属与载体的相互作用等进行研究。这些分析方法的使用，在催化剂研制过程中起着至关重要的作用。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">TPR:确定催化剂中可被还原成分的数量、开始被还原的温度、还原的截止温度等;</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">TPO:催化剂在完成TPR还原之后重新被氧化，确定被重新氧化部分占总共被还原部分的比例，用这个比例来反映催化剂的循环氧化还原性能;</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">TPD:.确定催化剂表面可用活性点在吸附某种气体后，在一定温度下，这些被吸附的气体从表面活性点，完全脱出时所需要的能量（解吸附能），以便通过解吸附能的大小反应催化剂的活性强弱;脉冲化学吸附：确定催化剂活性表面积，催化剂表面金属分散率，活性颗粒大小。</span></p> <h1 style="font-size: 1.25em; margin: 0.63em 0px 1.8em; border: 0px; padding: 0px; color: #191919; line-height: 38px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">二、操作方法TPR</span></h1> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">1、反应器内装入样品。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">2、打开主机电源，打开操作软件。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">3、阀2接入氧气，打开阀2，阀7打向阀2，阀8打向放空，处理气流量计调至40-60mL/min，进行样品升温氧化，氧化温度及时间视具体样品而定。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">4、阀1接入氩气，阀7打向阀1，设定1、2号质量流量计流速为</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">30mL/min，放下加热炉，降温吹扫至加热炉降至室温。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">5、阀1切至氢氩混合气室温吹扫5-10min，阀8打向TCD。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">6、打开TCD，基线平稳后升起加热炉，开始程序升温。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">7、峰图出完基线平稳后，关闭TCD，关闭温控器，降下加热炉，保存数据。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">8、阀1切至氩气吹扫5-10min。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">9、关闭气体，关闭主机电源，关闭操作软件。</span></p> <h1 style="font-size: 1.25em; margin: 0.63em 0px 1.8em; border: 0px; padding: 0px; color: #191919; line-height: 38px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">三、操作注意事项</span></h1> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">1、先通载气再打开TCD，结束后先关闭TCD再处理其他操作（以防烧坏TCD) 。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">2、主机和软件不具备记忆功能，重新启动时必须重新设置阀门开关和软件内1、2号质量流量计流量。</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">3、连续通入氢气和氧气处理样品时，中间必须通入惰性气体吹扫。</span></p> <h1 style="font-size: 1.25em; margin: 0.63em 0px 1.8em; border: 0px; padding: 0px; color: #191919; line-height: 38px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">四、样品要求</span></h1> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">1、常规都是粉末、颗粒状样品，粒度为 40-80 目；</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">2、样品需充分干燥，样品量不得少于100mg；</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">3、如有块状、薄膜样品需考虑气体分子能否扩散到样品里面</span></p> <p style="border: 0px; font-size: 16px; margin: 0.63em 0px 1.8em; padding: 0px; counter-reset: list-1 0 list-2 0 list-3 0 list-4 0 list-5 0 list-6 0 list-7 0 list-8 0 list-9 0; color: #191919; font-family: 'PingFang SC', Arial, 微软雅黑, 宋体, simsun, sans-serif; background-color: #ffffff;"><span style="font-size: 12pt;">4、要求样品不含S、卤素等，测试温度范围内，样品稳定，不能产生腐蚀性气体。</span></p>