tag:blogger.com,1999:blog-63640257067929776012024-03-05T13:21:02.125+09:00FD‐MS日記 <a href="http://www.agr.hokudai.ac.jp/ms-nmr/fdms/">旧 FD-MS日記</a>
<a href="http://www.agr.hokudai.ac.jp/ms-nmr/">農学部GC-MS&NMR室のホームページ</a>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comBlogger37125tag:blogger.com,1999:blog-6364025706792977601.post-45558852866492341952016-07-06T15:54:00.000+09:002016-07-12T12:49:01.003+09:00GC/MSを測定する友へ(暫定、仮置き)随時更新予定<br />
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<a href="https://drive.google.com/file/d/0B-vDMt-S8b0JR25FaUFRdm9qR1E/view?usp=sharing">資料はこちら</a>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-23946558264162783782016-06-01T15:43:00.000+09:002016-07-08T14:54:24.181+09:00エミッター電顕<span style="font-family: "arial" , "helvetica" , sans-serif;"><span style="background-color: white; font-size: 13px; line-height: 18.2px;">Carbotec: </span><a href="http://www.carbotec-analytik.de/carbotec/carbotec-allround.html" style="background-color: white; color: #0058cd; font-size: 13px; line-height: 18.2px; text-decoration: none;">http://www.carbotec-analytik.de/carbotec/carbotec-allround.html</a></span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><span style="background-color: white; font-size: 13px; line-height: 18.2px;">Linden: </span><a href="http://www.linden-cms.de/index.php?id=5" style="background-color: white; color: #4495ff; font-size: 13px; line-height: 18.2px;">http://www.linden-cms.de/index.php?id=5</a></span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JM0hkYmZiV0huZ0E&usp=sharing" style="font-size: small;"><span style="font-family: "arial" , "helvetica" , sans-serif;">使用済み</span></a><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JS3BYNGdDeG9HUTQ&usp=sharing">20120511-5</a> >37</span><br />
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<span style="font-family: "arial" , "helvetica" , sans-serif;">---2014年---</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JRjFrcFlMcXk4d00&usp=sharing">0207-2</a> 31 34 30 19 24 *FI</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span></div>
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JSURmRVVpWVRlRFE&usp=sharing">0516-2</a> -- 16 -- 15 --</span><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JWGRpQWRaeUxyUkE&usp=sharing"><span style="font-family: "arial" , "helvetica" , sans-serif;">0516-4</span></a><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JdHY1MHdMUFBuRkU&usp=sharing">0522-3</a> 14 38 17 19 36</span><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JY0RRSjdibUpfdkE&usp=sharing"><span style="font-family: "arial" , "helvetica" , sans-serif;">0522-5</span></a><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JZ3FFR211eXlZcUE&usp=sharing">0528-4</a> 40 -- 27 -- 16</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JakFNVXNJNjRpdmM&usp=sharing">0530-2</a> 32 38 22 25 42</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;">これ以降、Indene</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JcXU0QnVIdERDNlk&usp=sharing">0603-2</a> 22 32 15 26 14</span><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JbzdYUEdIenN0T2c&usp=sharing"><span style="font-family: "arial" , "helvetica" , sans-serif;">0603-4</span></a><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JeTB5MldlVVRyb2s&usp=sharing">0605-4</a> 16 17 24 26 11 *FI</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JTTNlLVcxbnh4eTg&usp=sharing">0618-4</a> 17 23 18 20 15</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JaTRyX1lwU3VPUmc&usp=sharing">0714-2</a> 23 24 12 18 16</span><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JY1FERHAwRS1vZmc&usp=sharing"><span style="font-family: "arial" , "helvetica" , sans-serif;">0714-4</span></a><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;">渡部レシピ、2日間、</span>高電圧で炭化<br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JflZSVGFfTXk3RHlOMHFlaDBnWHhwdWZSRlNHaEVNazdhX2ZON1pObUUxMm8&usp=sharing">0718-2</a> -- 10 -- -- --</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span><span style="font-family: "arial" , "helvetica" , sans-serif;">13kV、5×10</span><sup style="font-family: Arial, Helvetica, sans-serif;">-3</sup><span style="font-family: "arial" , "helvetica" , sans-serif;">→7kV、1×10</span><sup style="font-family: Arial, Helvetica, sans-serif;">-2</sup><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JYTlYa05zUnFaRFU&usp=sharing">0728-4</a> 26 24 24 42 29</span> (初期過程1500℃)<br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JLWJ0YkloQXRMSk0&usp=sharing"><span style="font-family: "arial" , "helvetica" , sans-serif;">0728-5</span></a><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JQW93X0NEM3NMTEE&usp=sharing">0730-4</a> 30 11 27 32 18</span> (初期過程1350℃)<br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JNDhsb3Q2UUN4cWc&usp=sharing">0801-4</a> 11 10 7 8 18</span> (初期過程1300℃)<br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span><span style="font-family: "arial" , "helvetica" , sans-serif;">13kV、5×10</span><sup style="font-family: Arial, Helvetica, sans-serif;">-3</sup><span style="font-family: "arial" , "helvetica" , sans-serif;">→9kV、1×10</span><sup style="font-family: Arial, Helvetica, sans-serif;">-2</sup><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JNDlLV1o4V3d2TVU&usp=sharing">0807-4</a><span style="background-color: rgba(255, 255, 255, 0);"> 20 30 12 18 14</span></span> (初期過程1500℃)<br />
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<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span></div>
<span style="font-family: "arial" , "helvetica" , sans-serif;">13kV、</span><span style="font-family: "arial" , "helvetica" , sans-serif;">5×10</span><sup style="font-family: Arial, Helvetica, sans-serif;">-3</sup><span style="font-family: "arial" , "helvetica" , sans-serif;">、1時間半で中断</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JTkZhcl9rZEF0Njg&usp=sharing">0808-4</a> 32 22 16 26 18 *FI</span> (初期過程>1500℃)<br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;">13kV、途中で0kV超高温(>1500℃)</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JTXp4cHJtLXRqZ1E&usp=sharing">0815-4</a> 8 11 10 3 9</span><br />
<div>
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JYWVvV3g0VDIwWms&usp=sharing">0825-4</a> 7 5 10 5 13</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;">13kV、9.5×10<sup>-3</sup></span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JZDJmRHJRQi05c00&usp=sharing">0827-4</a> 18 19 10 8 16</span> (初期過程1400℃)<br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">13kV、9.5×10</span><sup style="font-family: Arial, Helvetica, sans-serif;">-3</sup><span style="font-family: "arial" , "helvetica" , sans-serif;">、昇温なし</span></div>
<div>
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0Jb0tNcDBaRWVwOUU&usp=sharing">0903-4</a> 0 8 6 3 10 *FI</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;">カーボンコート(10cm、シャッター閉)</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JTnpkM2o1dU91dkE&usp=sharing">0910-4</a> 21 12 10 16 21</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">カーボンコートなし</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JSkhncDlwbTRJUzQ&usp=sharing">0912-4</a> 18 12 20 16 16</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">カーボンコート(7cm、シャッター開)</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JMEVpTGI0aGJRNkU&usp=sharing">0919-4</a> 14 8 12 8 12 結晶成長領域2mm、結晶長さ28um 隙間がない</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">カーボンコートなし</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JMVljVVUtV0RfWTA&usp=sharing">0924-4</a> 26 21 19 7 3 結晶成長領域2mm、結晶長さ28um 隙間がある</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">カーボンコート(7cm、シャッター開)</span><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfnZfTFRrY1VqS2lDOFE3ZEd6Z0dRdWREcjhHRHlvMjBoQU9VdjdtZ1RxQXc&usp=sharing" style="font-family: Arial, Helvetica, sans-serif;">0929-4</a> 12 15 8 9 14 <span style="font-family: "arial" , "helvetica" , sans-serif;">結晶成長領域</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">(<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JNGFaWFNPVS12RWc&usp=sharing">コーティング前</a>)</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">(<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JaUhmM1R0R2dZa2c&usp=sharing">コーティング後</a>)</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><br /></span>
<span style="font-family: "arial" , "helvetica" , sans-serif;">---2015年---</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;">13kV、5×10<sup>-3</sup>→9kV、1×10<sup>-2</sup></span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfmR6ZzR3cWxKY2djM2dxMmNMUVpiRFNmOE5icFBHQWE0TTl4SXd0b1pCSE0&usp=sharing">0416-4</a><span style="background-color: rgba(255, 255, 255, 0);"> 25 28 21 24 25 </span></span><span style="font-family: "arial" , "helvetica" , sans-serif;">カーボンコート(7cm、シャッター開)</span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfjJQMjlXV1prclZuTGZrRDU5LXRVOXhsbzVBcEFEZGJCbHJpX0x0VDNzMk0&usp=sharing">0423-4</a><span style="background-color: rgba(255, 255, 255, 0);"> 26 31 28 23 29</span></span><br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfmRqTG9XN2tKd3FTNFc3RVJzNXAtcnQtYUplT19qNmI0eXQ4RjJEUFBaSDg&usp=sharing">0501-4</a><span style="background-color: rgba(255, 255, 255, 0);"> 22 27 31 24 19</span></span> (初期過程1450℃)<br />
<span style="font-family: "arial" , "helvetica" , sans-serif;"><a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0Jfi1MTzg3OU1ubkdNY0hVSzEtT3BfNWtPTlJoOHc4SXRnUC11SjNyT1NrQVU&usp=sharing">0511-4</a><span style="background-color: rgba(255, 255, 255, 0);"> 31 27 28 25 28</span></span> (初期過程1500℃)</div>
<div>
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfndpTGxGZm40R1lpdDE5MXJZdlJtZUlVWkJzLVVIR05rMHg4cE5vaE1RamM&usp=sharing">0513-4</a><span style="background-color: rgba(255, 255, 255, 0);"> 21 26 26 24 23</span> (初期過程1450℃)<br />
<br />
13kV、5×10<sup>-3</sup>→13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfkpVTWozNG1Qc0d3czFhZjVINWRrV0dxcUg3a2l5REUyWUcwdkNxQjQyOFk&usp=sharing">0515-4</a> 30 24 28 22 24 (初期過程1500℃)<br />
<br />
<div>
13kV、1×10<sup>-2</sup><br />
<div>
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfjRKTHpuMEtkaWdoTUpmbnNpcExtdk5DVFotY2NVazlTTGxtdjlJSjBLaEE&usp=sharing">0519-4</a> 33 31 33 29 28 (初期過程1500℃)<br />
<br />
13kV、1×10<sup>-2</sup>→10kV→7kV→5kV<br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfjdLUV85M2VzVGxOdm1LeEJVS0lvVzVYaG1WV3VjVFExeE43TE9QNlJoRzg&usp=sharing">0521-4</a> 5 10 6 10 9 (初期過程1450℃)</div>
<br />
13kV、1.7×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfmZBcGJXdC1ZZjdMX05tQ3RyczlRU29mTG1XOEdvUzY4emVfak83aF9xRHc&usp=sharing">0525-4</a> 22 24 15 24 18 (初期過程1500℃)<br />
<br />
13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfjdMZ3ZJdksxdGJBZTAwczRiZFB1M2lvc21Oc1hhUVdpbm5mNThQWmpBQWc&usp=sharing">0527-4</a> 25 27 27 23 22 (初期過程1500℃)<br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfjZ5X3V3a0E4enhPdzdfT1BsdUp4bjdkS0Q5akIyaTJ0SnJ1bEswcDFXLW8&usp=sharing">0529-4</a> 16 25 17 25 25 (初期過程1280℃)<br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfmZ6QXRETDIxT0FrT005dlhxeXNzNE9XbzVWTHVqRmxreEt5aTVrNFVLa28&usp=sharing">0602-4</a> 25 23 21 24 25 (初期過程1400℃)<br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfnlWRE5uUVhhaDJZTDFPV3JFTXp6QlE5a1FJZXRvNTlBQy0wZ21TZnhSUTA&usp=sharing">0616-4</a> 20 21 20 14 17 (初期過程1500℃)<br />
<br />
*高電圧で炭化→13kV、5×10<sup>-3</sup>→13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0Jfmhpc21fSGZJNlNkcVhrV3RLM2hQdDFvQmJNQ1I4a0RQeFNwVkpOaXVGZG8&usp=sharing">0618-3</a> 32 27 31 28 27 (初期過程>1500℃)<br />
<br />
13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfjFFV3oyRDB0aFhDVnFZTENnNnJMcERzUmRwZWRJcWFlTnJwMnZFXzJqR1U&usp=sharing">0622-3</a> 28 21 28 25 28 (初期過程1400℃)<br />
<br />
*炭化中に高電圧→13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfmdEQ3BpWkxhWmM1V29hcU5ybTR4SUp0Yk01dmhGQ2tOVThfUkZDNUFHMms&usp=sharing">0625-4</a> 24 28 30 31 31 (初期過程1500℃)<br />
<div>
<br /></div>
<div>
13kV、5×10<sup>-3</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JflFLVVZUNnRyX3Q2c29LQ216QjZ5SUI3QlFQbWdFcXBDYkF3Q3IyWHFuZWs&usp=sharing">0629-1</a> 23 21 11 16 18 (初期過程1400℃)</div>
<div>
<br /></div>
<div>
*1×10<sup>-2</sup>で炭化→13kV、5×10<sup>-3</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JfnlMTXI4MUlLVVIwNHNSY2p4cXBjX3NvNEpYSE82dUtZR2QxNWo3UjMwamc&usp=sharing">0701-1</a> 17 16 11 6 12 (初期過程1500℃)</div>
<div>
<br /></div>
<div>
*1×10<sup>-2</sup>で炭化→13kV、5×10<sup>-3</sup>→9kV<br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JTVJmOVBGcFpEYlU&usp=sharing">0703-3</a> 22 13 21 21 19 (初期過程1500℃)</div>
<div>
<br /></div>
<div>
白金被膜</div>
<div>
13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JRktPQy1JRllGem8&usp=sharing">0707-3</a> 30 30 33<span style="font-family: "arial" , "helvetica" , sans-serif;"> -- </span>35 (初期過程1500℃)</div>
<div>
<br /></div>
<div>
金被膜</div>
<div>
13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JQ1pwUUd1WUdFRUk&usp=sharing">0715-3</a> 31 30 28 31 23 (初期過程1450℃)</div>
<div>
<br /></div>
<div>
カーボンコート</div>
<div>
13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JRVRjQ1VIZjQ0Wmc&usp=sharing">0723-3</a> 27 28 28 31 27 (初期過程1500℃)</div>
<br />
3, 4は白金、5はカーボン<br />
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13kV、1×10<sup>-2</sup><br />
<a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0Jb0ZEQkZGbS1ZdG8&usp=sharing">0811-1</a> <a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0Jc2FRLVFtbkpOS1k&usp=sharing">0811-2</a> <a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JbmJzb0tsSlRROFU&usp=sharing">0811-3</a> <a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JS0NnV2xLUkxnLWs&usp=sharing">0811-4</a> <a href="https://drive.google.com/folderview?id=0B-vDMt-S8b0JTUF6bjFxVENyREE&usp=sharing">0811-5</a> 15 11 17 20 34 (初期過程1500℃)</div>
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炭化の前後を比較する</div>
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Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-13826196172234395602015-06-15T16:13:00.001+09:002016-07-08T14:47:31.431+09:00エミッター電顕一覧<br />
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20120511-5 : >37
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2014207-2 : 34
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20140516-2 : 16
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20140516-4 : 15
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20140522-3 : 17
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20140522-5 : 36
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20140528-4 : --
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20140530-2 : 38
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20140603-2 : 32
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20140603-4 : 26
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20140605-4 : 26 *FI
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20140618-4 : 20
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20140714-2 : 24
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20140714-4 : 18
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20140718-2 : --
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20140728-4 : 42
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20140728-5 : 29
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20140730-4 : 32
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20140801-4 : 8
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20140807-4 : 18
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20140808-4 : 26 *FI
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20140815-4 : 3
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20140825-4 : 5
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20140827-4 : 8
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20140903-4 : 3 *FI
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20140910-4 : 16
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20140912-4 : 16
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20140919-4 : 8
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20140924-4 : 7
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20140929-4 : 9
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20150416-4 : 24
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20150423-4 : 23
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20150501-4 : 24
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20150511-4 : 25
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20150513-4 : 24
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20150515-4 : 22
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20150519-4 : 29
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20150521-4 : 10
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20150525-4 : 24
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20150527-3 : 27
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20150529-3 : 17
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Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-3533490516844040512014-09-22T17:11:00.001+09:002015-05-14T08:54:55.616+09:00エミッターのイオン化効率への影響混合物をGC/FIで測定したとき、<br />
それぞれのピークの強度比がエミッターによって変化する。<br />
<br />
クロロホルム(RT 1.74 min)とメチルグリシジルエーテル(RT 2.16 min)<br />
<br />
0603-2(32)おろしたて<br />
クロロホルムの方が強い<br />
<a href="https://drive.google.com/open?id=0B-vDMt-S8b0JZVFLSkk2bE42NE0&authuser=0">クロマト</a><br />
<br />
(35→2)長期間使用<br />
クロロホルムがほとんど出ない<br />
<a href="https://drive.google.com/file/d/0B-vDMt-S8b0JVV9jTmtOeXU0VjQ/view?usp=sharing">クロマト</a>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-15757785965743391832014-09-22T16:58:00.001+09:002015-01-27T14:55:17.519+09:00エミッター作製まとめ(FI用)もとのファイルは<a href="https://drive.google.com/file/d/0B-vDMt-S8b0JbzAxdWhyX0t1enM/view?usp=sharing">こちら</a><br />
<br />
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1 M. D. Migahed, <i>et al</i>., <i>International Journal of Mass Spectrometry
and Ion Physics</i>, 7(1971)1-18.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">電圧、温度、蒸気圧が結晶成長に与える影響(詳細)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2 H. D. Beckey, <i>et al</i>., <i>International Journal of Mass Spectrometry
and Ion Physics</i>, 8(1972)169-179.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">エミッター作製と</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">測定の全般</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">3 J. H. Gross, </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">平岡賢三ら訳</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">, </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">マススペクトロメトリー</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">, </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">シュプリンガー・ジャパン</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">, 2007</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">年</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">注意</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">エミッター作製の初期の研究は</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">を念頭に置いており、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">用の検討は</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1970</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">年代後半に多い。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ここでは、初期の</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">用についてまとめる。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">用については別ファイルにする。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">背景</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶がなくても極めて細いワイヤーで</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">は行えるが十分ではなく、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">表面に針状結晶を成長させることで局所的に電界を強めることができる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ワイヤーの材質</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">初めのうちは白金が使われていた</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">が、タングステンが丈夫で扱いやすく</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p15, 2)p169</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">、よく使われる。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ワイヤーの太さ</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2.5-5 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">:細い、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">:太い</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ワイヤーが太いほど、成長は遅く、針状結晶は長くなる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p7</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">太いワイヤーを使う場合、初めの電圧を高くする</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p15</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">の太いワイヤーだと機械的に丈夫で、さらに表面積が大きいため、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">には適している</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p15</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">太いワイヤーだと、カソード側と土台側に同じくらいずつ結晶ができるが、細いワイヤーだと土台側により多くできる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p9</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶の長さ</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶の表面の電界強度は針状結晶の長さに比例し、直径に反比例する</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p3</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶の根元の部分は太く、密集しているため、ワイヤーの一部とみなすことができ、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">結晶が長くなるにつれて実質的なワイヤーの太さが増していく</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p4</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">The field enhancement due to the increase of the needle length is
compensated (or over-compensated) for by the virtual increase of the wire diameter,
and hence according to eqn. by a decrease of the field strength.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">F</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 8.0pt; mso-bidi-font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">(t)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">=F</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 8.0pt; mso-bidi-font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">0</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">・</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">(h</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 8.0pt; mso-bidi-font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">(t)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">/r</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 8.0pt; mso-bidi-font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">n(t)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> )</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">・</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">(r</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 8.0pt; mso-bidi-font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">0</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">/r</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 8.0pt; mso-bidi-font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">(t)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">)<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">タングステンワイヤーでは針状結晶が</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">3 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">のときに</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">感度が最大になる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2)p172</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">とても長い(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10-15 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">の)針状結晶(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5-10 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">タングステンワイヤー上)が</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">には必要である</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2)p172</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">炭素源</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ベンゾニトリルは実験的にも理論的にも適している</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">とされていたが、さらに良いものが見つかった。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">これについては、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">用の別ファイルにまとめる。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インダン、インデン、インドール、ナフタレンだと短時間で、ベンゼンだと数秒間で活性化できる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">3)p393</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">純粋なベンゾニトリルやインデンを用いて、カスタム化した特性を持つエミッターが商業的に作られている</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">3)p393</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">電圧</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">初めに高くすることで結晶成長の核を作り、途中から低くすることで針状結晶を大きくする</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p17</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">途中からはエミッション電流を一定にすべきであり、そのために電圧を徐々に下げていく</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p6</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">始めは</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">14kV</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">で、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">時間のうちに</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10kV</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">まで落とす</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2)p172</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">温度</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">高温で作ると、濃く、強い針状結晶ができる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p14</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">高温で作ると、熱に強いエミッターになる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p11</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">タングステンの酸化膜が結晶成長を阻害するため、真空中で</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1000</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃に加熱して取り除く</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p10<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">800-900</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃で</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">分</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2)p172</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">)。導入過程については、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">用の別ファイルにまとめる。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">初めの成長は温度が高いほど(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">600</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃まで)速い。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">900</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃以上の高温にすると成長速度が少し落ち、針状結晶の構造に不可逆的な変化が起こる。高温だと枝分かれが少なく、樹状でなくなる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p7</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">蒸気圧</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">高い蒸気圧で作ったほうが、イオン化効率の高いエミッターができる。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10-3</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">より高くすると、実質的なワイヤー直径の増大が速くなりすぎるので良くない</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p9</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">総合的なこと</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">活性化効率は重合速度、架橋の度合い、針状結晶の物理的強度、形状、導電性に依存する</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p4</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">初めの</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">分は</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">900</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">14-5kV</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">で、その後、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">20</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃で</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">6</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">時間ほど置き、最後に</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">分ほど</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">900</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃にする</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p17</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">分以降は、エミッションが(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">8uA</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">など)一定になるように</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">9kV</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">くらいまで徐々に電圧を落とす</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p6,17</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">アクチベーター内でのイオン化効率の良し悪しと、質量分析計内でのイオン化効率の良し悪しは必ずしも一致しない</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2)p170</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。→エミッターの評価は質量分析計で行うべき</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-29015032982960290552014-09-22T16:56:00.003+09:002015-01-27T14:57:06.493+09:00エミッター作製まとめ(FD)もとのファイルは<a href="https://drive.google.com/file/d/0B-vDMt-S8b0JY0hFeVRzcTdfS1E/view?usp=sharing">こちら</a><br />
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">文献</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1 M. D. Migahed, <i>et al</i>., <i>International Journal of Mass Spectrometry
and Ion Physics</i>, 7(1971)1-18.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">電圧、温度、蒸気圧が結晶成長に与える影響(詳細)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2 H. D. Beckey, <i>et al</i>., <i>International Journal of Mass Spectrometry
and Ion Physics</i>, 8(1972)169-179.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">エミッター作製と</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">測定の全般</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">3 J. H. Gross, </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">平岡賢三ら訳</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">, </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">マススペクトロメトリー</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">, </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">シュプリンガー・ジャパン</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">, 2007</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">年</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">4 H. D. Beckey</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">,</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">Principles of Field Ionization and Field Desorption Mass Spectrometry,
Pergamon</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">,</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1977.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">導入、第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">、第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">の三段階、後の条件検討の基礎になっている</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">5 W. D. Lehmann, <i>et al.</i>, <i>Analytical Chemistry</i>,
53(1981)743-747<o:p></o:p></span></div>
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<span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">活性化中の抵抗、温度</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">6 JEOL </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">エミッターアクチベータ取扱説明書</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> FD, FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">用エミッター(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">タングステン、ベンゾニトリル、結晶長</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">15-30 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7 M. Rabrenovic, <i>et al</i>., <i>International Journal of Mass Spectrometry
and Ion Physics</i>, 37(1981)297-307.<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インデン使用、条件はほぼ</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">Beckey</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">の本</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">4)</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">の通り</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">背景</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1970</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">年代前半の基礎研究を前提として、同後半以降に</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">に適したエミッターの作り方が検討されている。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ここでは、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">用の丈夫で結晶の長いエミッターについてまとめる。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FI</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">のイオン化効率が高くするには、細いワイヤー上に短い結晶を成長させれば良い</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1)p4, 2)p172</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">に適した長い結晶を再現性よく作るために、活性化前の導入過程にも力が入れられている</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p743</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ワイヤー</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">タングステン</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">4)p66,5)p743,6)p2-1,7)p298<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">スポット溶接</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">溶接後のワイヤーの長さの違いにより、活性化前エミッターの抵抗にばらつきが出る</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p743</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">溶接が不完全だと、抵抗が大きくなり、そのようなものは活性化に使わない</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p743</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶の長さ</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">35-40 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">が</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">FD</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">に適している</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p299</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">15-30 um6)p4-2<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">30-40 um4)p70,5)p743<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">最大で</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">100 um</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">にまでできるが、その場合、結晶の短い周辺部が高温になりすぎて切れやすい</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p745</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">図の</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">c</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">で支柱の近くが高温になりすぎる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p746<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">炭素源</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ベンゾニトリル</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">4)p65,5)p743,6)p2-1<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ベンゾニトリル、インダン、インデン、ナフタレン、インドールのどれでも出来は同じだが</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p306</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インデンだと結晶の成長が早い</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p301</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インデンを使う場合もベンゾニトリルと同じ手順で活性化する</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p299</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">金属、シリコンなどのエミッターは炭素のものより劣るが、短時間で作れる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p298</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">温度</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">4)p69<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃(上限</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1250</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃、下限</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">950</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">6)p2-1<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃、ただし、導入段階後の初期は中心部を高め(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1250-1300</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃)にして周辺部が低すぎないようにする</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p746</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インデンの場合、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃で</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">6</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">時間かかるところ、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1300</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃では</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">時間で作れる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p299</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ベンゾニトリルは温度を変えてもあまり効果が無い</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p299</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">図の</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">b</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">のように、中心部がやや熱すぎる場合に、周辺部が適温になる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p746<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">電圧</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">始めは高く、途中から低くすることで、根元は密で先端はまばらにする</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p745</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">蒸気圧</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">電圧を下げることによる結晶成長速度の低下を補うため、蒸気圧を上げていく</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p745</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">蒸気圧は各時点で安定して使える最大値にする</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p745</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">エミッション</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">始めに</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">0.1uA</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ほどだったのが、</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">時間で</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10uA</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">まで急上昇するのが、結晶成長開始の指標になる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p745</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">40uA</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">になったら、電圧を下げ始めて、それ以降エミッションを一定に保つ</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p745</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">。</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">導入段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">0kV1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">10-2</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃から</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1400</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃に上昇</span><span style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">炭化タングステン生成の発熱反応</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">4)p69<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">12kV 1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">36mA</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 3uA 4)p69<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5kV </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">蒸気増加</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 4)p70<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">導入段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">0kV 1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10-2 10min 1400</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃から</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1800</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃に上昇</span><span style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ワイヤーが部分的に炭化</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p743<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">*</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">望みの温度にしてから蒸気を入れる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">抵抗が</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1.5</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">倍ほどに増加する</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">始め</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10kV 1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10-2 1h 5uA 5)p745<o:p></o:p></span></div>
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<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">*</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">頻繁にエミッションをチェックしてこまめに電圧を下げる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">終わり</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">4kV 5</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">10-2 </span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">5)p745<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">14kV 5</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10-3 1200</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃(</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">35mA</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">)</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 2h 1uA </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶の芽をつくる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">6)p3-1<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">12kV 8</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10-3 1h 5uA </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">の芽を育成する</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">6)p3-1<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">第</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">3</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">段階</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">10kV 1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">10-2 60mA</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">まで</span><span style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">エミッション飽和</span><span style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";"> </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">針状結晶を成長させる</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">6)p3-1<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">導入段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">0kV </span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インデン 1200</span>℃<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">ワイヤーが炭化</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">7)p299</span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">段階</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">12-14kV 5</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">10-3</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インデン</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 1300</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 7)p299,301<o:p></o:p></span></div>
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<span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">第</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";">2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">段階</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">6-7kV 1</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ansi-language: DA; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">×</span><span lang="DA" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-ansi-language: DA; mso-fareast-font-family: "MS P明朝";">10-2</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">インデン</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 1300</span><span style="font-family: "MS P明朝"; font-size: 10.0pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">℃</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10.0pt; mso-fareast-font-family: "MS P明朝";"> 7)p299,301<o:p></o:p></span></div>
Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-56922643640600779962014-05-31T13:39:00.006+09:002014-09-22T17:14:40.254+09:00CIテストCIを試すことにした経緯は<a href="http://fd-ms.blogspot.jp/2014/05/fdfi.html" style="background-color: white; color: #0058cd; font-family: Arial, Tahoma, Helvetica, FreeSans, sans-serif; line-height: 18.2px; text-decoration: none;">5/27の記事</a><br />
<br />
二重収束型のJMS-SX102AでCI測定をしてみた.<br />
CI用イオン源チャンバーとフランジをセットしたが,<br />
試薬ガスはつないでいない.<br />
<br />
「よりよいCIスペクトルを得るために」(日本電子,1980年代)を参考にした.<br />
試薬ガスをボンベから以外に,リザーバーから供給することが紹介されている.<br />
リザーバーに入れる試薬としては,アセトンやメタノール,エチルアミンが挙げられている.<br />
<br />
アセトンのPA(下記)はイソブタンとほぼ同じで,メタノールは少し小さい.<br />
アセトンで測定すると[M+H]+だけが出たが,弱かった.<br />
メタノールで測定すると[M+H]+のほかに数本のフラグメントピークが出た.<br />
メタノール中に痕跡量のアセトンが含まれた状態では,<br />
[M+H]+だけが出て,アセトンの場合より強かった.<br />
<br />
手元にiso-プロピルアミンがあるので,<br />
アセトンでもフラグメントが出る場合に使ってみようと思う.<br />
<br />
<br />
リザーバー内は液面が見えず,枯渇や入れすぎに気づきにくいので,<br />
リザーバーに取り付ける液体試料注入ビンをセットするために準備をしている.<br />
混合試薬ガスを試す場合にも,ビン内で両液を混ぜればいいので簡単である.<br />
<br />
<br />
PA(プロトン親和力,kJ/mol)<br />
メタン552<br />
<span style="color: red;">イソブタン820</span><br />
アンモニア854<br />
<br />
<span style="color: blue;">アセトン812</span><br />
<span style="color: blue;">メタノール754</span><br />
エタノール776<br />
プロパノール787<br />
<br />
メチルアミン896<br />
エチルアミン912<br />
ジエチルアミン952<br />
トリエチルアミン981<br />
プロピルアミン918<br />
<span style="color: lime;">イソプロピルアミン924</span>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-85315219122376273872014-05-27T21:25:00.001+09:002014-12-18T10:53:42.699+09:00付加イオンによるフラグメント抑制FDではEIに比べてソフトにイオン化できるが,<br />
フラグメンテーションがまったくないわけではない.<br />
生成する分子イオンはラジカルを有しているため,<br />
安定なラジカルが生じるようなフラグメンテーションが特に起こりやすい.<br />
典型的な例として,tert-ブチル基の脱離による[M-57]+の生成がある.<br />
<br />
ラジカルが関与するフラグメンテーションの多くは,<br />
プロトン付加分子([M+H]+),アルカリイオン付加分子([M+Na]+,[M+K]+など)からは起こらない.<br />
低極性分子の場合,試料量を増やしたり,良くないエミッターを使ったりして<br />
[M+H]+をたくさん生成させ,フラグメンテーションを抑えることができる.<br />
ある程度極性があれば,上記のほかに,アルカリ金属塩(NaIなど)の添加も使える.<br />
<br />
<br />
低極性化合物のイオン化法に,CI(化学イオン化)というのがあり,<br />
これは,流通している多くの装置で利用できる.<br />
FDには及ばないものの,試薬ガスを厳選すればある程度ソフトにできる.<br />
<br />
CIではラジカルを有する分子イオンはほとんど生成せず,多くの場合,<br />
プロトンか試薬ガス由来の反応イオンが分子に付加したものが生成する.<br />
<br />
イオン化後のフラグメンテーションにラジカルが大きく関与する場合は<br />
多少エネルギーが高くとも,CIでラジカルなしのイオンにする方が有利だと考える.<br />
<br />
有用性を確かめるために,近々CIとFDの比較をしようと思っている.<br />
試薬ガスを使い切るほど測定しない可能性が高いので,<br />
ガスボンベではなく,リザーバーからガスを供給することにする.<br />
<br />
<br />
CIは1970年代に熱心に研究されたが,最近,過去の知見を再発見した論文が出ている.<br />
James L. Little and Adam S. Howard, <i>Journal of The American Society for Mass Spectrometry</i>, <b>24</b>, 1913-1918 (2013)<br />
試薬ガスとしてメチルアミンを用いればかなりソフトにイオン化できるが,<br />
実用的でないほど感度が落ちてしまう.<br />
大過剰のメタンと数%のメチルアミンの混合ガスを用いれば,感度が大幅に向上する.<br />
この場合,メタン由来の反応イオンはほぼすべてメチルアミンのイオン化に使われるため,<br />
サンプルのイオン化に寄与するのはメチルアミン由来の反応イオンとなる.<br />
<br />
<br />
<br />
低極性化合物をFD/FIよりもさらにソフトにイオン化する手法として<br />
IA(イオン付着)イオン化がある.<br />
分子にリチウムイオンを付加させ,ラジカルを持たないイオン([M+Li]+)を生成する.<br />
<br />
1970年代に,未活性化エミッターによる無機塩の測定から発展した.<br />
下記書籍の78ページ(2.4.5.2章)<br />
<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10pt; mso-fareast-font-family: "MS P明朝";">H. D. Beckey<span style="font-family: "MS P明朝"; font-size: 10pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">,</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10pt; mso-fareast-font-family: "MS P明朝";">Principles of Field Ionization and Field Desorption Mass Spectrometry, Pergamon</span><span style="font-family: "MS P明朝"; font-size: 10pt; mso-ascii-font-family: "Times New Roman"; mso-hansi-font-family: "Times New Roman";">,</span><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10pt; mso-fareast-font-family: "MS P明朝";">1977.</span></span><br />
<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10pt; mso-fareast-font-family: "MS P明朝";"><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10pt; mso-fareast-font-family: "MS P明朝";"></span></span><br />
<span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10pt; mso-fareast-font-family: "MS P明朝";"><span lang="EN-US" style="font-family: "Times New Roman"; font-size: 10pt; mso-fareast-font-family: "MS P明朝";"><o:p></o:p></span></span><br />
このイオン源を装着した質量分析計は現在,販売されていない.<br />
過去にはIA-LabというQ-MSがキャノンアネルバから出ていた.<br />
<a href="http://www.jeol.co.jp/corporate/envi/seminar/2008.html" style="background-color: white; color: #0058cd; font-family: Arial, Tahoma, Helvetica, FreeSans, sans-serif; font-size: 13px; line-height: 18.2px; text-decoration: none;">JEOL環境セミナー講演集 (2008)</a><br />
<br />
産総研でIA-TOF-MSを製作されているが,まだ製品化されていない.<br />
<a href="http://www.aist.go.jp/aist_j/aistinfo/aist_today/vol06_08/vol06_08_main.html" style="background-color: white; color: #0058cd; font-family: Arial, Tahoma, Helvetica, FreeSans, sans-serif; font-size: 13px; line-height: 18.2px; text-decoration: none;">産総研TODAY,Vol6-8,28ページ (2006)</a>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-83297044234053192472014-05-27T12:30:00.003+09:002016-04-28T10:45:13.477+09:00電界電子放出(FE)エミッターFI-MS,FD-MS用のエミッタでは,針状結晶が長くなるにつれて<br />
見た目のワイヤー径が太くなり,発生させる電界強度が落ちてしまう.<br />
カーボンナノチューブやカーボンファイバーならば<br />
根元が太くないため,長く成長させても見た目のワイヤー径が変わらない.<br />
イオン化効率が格段に向上すると思うので,ぜひとも試してみたい.<br />
<br />
<br />
FI-MS,FD-MS用のエミッターと非常によく似た技術に<br />
電界放出電子源(FE)がある.<br />
<br />
X線源(電子源)としてのカーボンナノチューブの利用には賛否両論ある.<br />
<br />
<br />
奥山 文雄:使える<br />
ドイツ,Hans-Dieter BeckeyのもとでFI-MS,FD-MS用のエミッター開発をしていた.<br />
その後,名古屋工業大学でX線源を開発した.<br />
1990年代後半に,世界で初めて,電界電子によるX線像を得た.<br />
FI-MS,FD-MS用エミッターの炭素結晶成長を応用して,<br />
カーボンナノチューブ群を用いたX線源を作製した.<br />
<a href="http://ci.nii.ac.jp/naid/110003445399">日本放射線技術学会雑誌,2002年3月,309-313ページ</a><br />
<div style="text-align: left;">
X線源の作製に関する論文で用いている基板は,</div>
<div style="text-align: left;">
材質,形状からして,FI-MS,FD-MS用のエミッターと同じである.</div>
<div style="text-align: left;">
つまり,<span style="color: red;">針状結晶の代わりにカーボンナノチューブを成長させたものを作っている</span>.</div>
<div style="text-align: left;">
<span style="color: red;">これが質量分析に使えるか</span>気になるが,適用したという記述はない.</div>
<div style="text-align: left;">
M. Tanemura <i>et al</i>., <i>J. Appl. Phys.</i> <b>90</b>, 1529 (2001).</div>
<div style="text-align: left;">
<br /></div>
<div style="text-align: left;">
現在(2014年)の研究室名はナノ機能材料研究室,教授は種村 眞幸で,</div>
カーボンナノチューブを用いたSPMカンチレバーを開発している.<br />
<a href="http://tane-lab.web.nitech.ac.jp/index.html">http://tane-lab.web.nitech.ac.jp/index.html</a><br />
<br />
<br />
鈴木 良一:よくない<br />
カーボンナノチューブをX線源として用いると<br />
強力な電界でカーボンナノチューブが基板から剥がれてしまう.<br />
カーボンナノチューブは,その径が基板から先端まで同一であり,<br />
根元にまで高電界が及ぶことが破損の原因であるため,<br />
根元に向かうにつれて太くなる形を採用した.<br />
針葉樹型をしており,先端にはナノレベルの針状突起が出ている.<br />
産総研計測フロンティア部門公開シンポジウム報告集<br />
<a href="https://unit.aist.go.jp/riif/ja/results/publication.html">
https://unit.aist.go.jp/riif/ja/results/publication.html</a><br />
第9回シンポジウム,117ページ,極微欠陥評価研究グループ<br />
<br />
<br />
<br />
<br />
電界イオン顕微鏡(1951年)<br />
エミッターに正電圧をかけて,試料を電界イオン化(FI)する.<br />
これにより,世界で初めて原子の観察に成功した.<br />
<br />
電界放射顕微鏡(1937年)<br />
エミッターに負電圧をかけて,電子を放出させる.Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-13084762594340957602014-05-26T16:08:00.004+09:002014-05-29T09:03:57.651+09:00活性化ガスカーボンエミッタが開発された当初は<br />
benzonitrileが最善の活性化ガスだと報告されていた.<br />
<br />
その後,FD用エミッター作製にかかる時間を短縮するために<br />
活性化ガスの再検討が行われた.<br />
M. Rabrenovic and T. AST, Alternative Organic Substances for Generation of CarbonEmitters for Field Desorption Mass Spectrometry. <em>Int. J. Mass Spectrom. Ion Phys.</em> <strong>1981</strong>, 37, 297-307.<br />
<br />
その中でIndeneとNaphthaleneが推奨されており,<br />
CarbotecではIndeneが使用されていることから,<br />
Indeneを試すことにした.<br />
<br />
これまでは,benzonitrileを用いて<br />
2日以上かけて作製していたため,<br />
条件検討が一向に進まなかった.<br />
<br />
Indeneを使えばbenzonitorileのときに比べて<br />
所要時間が10分の1ほどに短縮できるため,<br />
条件検討の効率が飛躍的に向上すると期待している.Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-73687418357382910352014-05-26T15:45:00.002+09:002014-05-29T09:03:39.539+09:00エミッターの評価完成したエミッターはリザーバーから流したアセトンの<br />
分子イオンの強度を測定して比較している.<br />
<br />
作製条件は針状結晶が長くなるように設定しており,<br />
完成後の目視でも,長いことを確認している.<br />
<br />
このように,FIとFDの両面で評価しているため,<br />
FIもしくはFDに特化したエミッターは生まれない.<br />
<br />
FI用ならば,針状結晶が短くなるように設定して<br />
アセトンの測定で強度が出るものを選抜すればいい.<br />
<br />
FD用は再現性よくイオン化効率を実測するのが難しいと思う.<br />
できたとしても,評価のためにエミッターが消耗することになる.<br />
<br />
FIに比べて,FDの測定が圧倒的に多いので,<br />
FD用エミッターを作り,評価する方法を考えている.<br />
<br />
Carbotec Allround: <a href="http://www.carbotec-analytik.de/carbotec/carbotec-allround.html">http://www.carbotec-analytik.de/carbotec/carbotec-allround.html</a><br />
Carbotec FI用: <a href="http://www.carbotec-analytik.de/carbotec/carbotec-fi.html">http://www.carbotec-analytik.de/carbotec/carbotec-fi.html</a><br />
Carbotec FD用: <a href="http://www.carbotec-analytik.de/carbotec/carbotec-fd.html">http://www.carbotec-analytik.de/carbotec/carbotec-fd.html</a>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-391214720525774082014-05-26T15:05:00.000+09:002014-05-26T15:05:01.176+09:00アクチベーターののぞき窓アクチベーターのチャンバーにはのぞき窓があり,<br />
直径23.6 mm,厚さ2.5 mmのガラスをはめている.<br />
<br />
エミッタを作る度にガラスが汚れるため<br />
数回に一度,紙やすりで研磨していた.<br />
<br />
アクチベーター内のエミッタの温度確認は<br />
パイロメーターを使って目視で行うため,<br />
ガラスの汚れ具合によって不正確になると考えた.<br />
<br />
代用品として,アクリル板に取り替えてみると,<br />
これまでのところ問題なく使えている.<br />
<br />
東急ハンズで厚さ2 mmのアクリル板を買い,<br />
加工コーナーで円カットしてもらった.<br />
<br />
使用後は茶色の膜ができるが,<br />
消しゴムでこすることできれいに除去できた.<br />
3um(#4000相当)のラッピングフィルムシートで研磨すると,<br />
細かい傷が付いて,透明度が落ちてしまった.Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-50672205660663028962014-05-26T14:40:00.002+09:002014-08-17T09:00:50.223+09:00活性化中に生じるたわみ高電圧をかけた状態で1400℃程度の高温になると<br />
やわらかくなったワイヤーが対向電極に引っ張られてたわむ.<br />
<br />
活性化していないワイヤーの場合,<br />
45 mAなら数秒で,<br />
42 mAなら3分でたわむ.<br />
<br />
32 mAから5 mA/hrで42 mAまで上げ,<br />
42 mAで3分保持すると,5個中3個がたわんでいた.<br />
<br />
<br />
針状結晶ができやすくなるするための初期の高温処理は,<br />
電圧をかけなくても効果があるのか調べたい.<br />
効果があるなら,電圧をかける前に高温処理をして回避できる.<br />
<br />
初期の高温処理で温度を控えめにしてたわまないようにしても,<br />
電流を上げていく過程で高温になり,たわむことがある.<br />
電流の上昇は,針状結晶の形成による電気抵抗の減少を補うためのものなので<br />
針状結晶の成長が遅れていると,過剰補正されて温度が上がってしまう.<br />
<br />
CarbotecやLindenのホームページに載っているエミッターは<br />
どれもわずかにたわんでいる.<br />
Carbotec: <a href="http://www.carbotec-analytik.de/carbotec/carbotec-allround.html">http://www.carbotec-analytik.de/carbotec/carbotec-allround.html</a><br />
Linden: <a href="http://www.linden-cms.de/index.php?id=5">http://www.linden-cms.de/index.php?id=5</a>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-66125513899767584492013-06-30T15:32:00.002+09:002013-06-30T20:59:41.699+09:006月まとめ<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">・FD/FI(GCv)</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">FDで対向電圧をかけた時点で大量のイオンが生成していることに気付いた.</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">測定を行わないときは,</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">スペクトルモニターで監視をしながら</span><span style="line-height: 18px;">対向電圧のON/OFFを制御できる.</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">一方,本測定を行う際は,測定開始以前に対向電圧がONになるので</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">上述の大量のイオンを取り逃がしてしまう.</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">これを回避するためには,プローブを引っ込めておけば良い.</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">プローブを引っ込めた状態で対向電圧をかけて測定を開始すれば,</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">プローブを挿したときに大量のイオンを観測できる.</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">ただし,このやり方だと,試料を塗布した状態でのチューニングができない.</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;"><br /></span></span>
<span style="font-family: inherit;"><span style="line-height: 18px;">---4月まとめ---</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">GCvでFDの測定時にデフレクタバランスがずれる.</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;"> サンプルを載せるときにワイヤーが動くのか</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;"> </span></span><span style="background-color: white; font-family: inherit; line-height: 18px;">カソード電圧のOFF→ONで動くのか</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;"> たるみのないエミッターにすることで回避できるか</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;"> EIのフィラメントと同様に,初めて電流を流すときに穏やかにするとどうか</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;">------</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;"><br /></span>
<span style="background-color: white; font-family: inherit; line-height: 18px;">たるみのないエミッターを作るために,</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;">EIフィラメントの使い始めと同様に</span><span style="background-color: white; font-family: inherit; line-height: 18px;">じっくり焼成することを試していた.</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;">対向電圧をかけない状態で使用最大電流に達するまで焼成しても,</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;">対向電圧をかけて同じだけ電流を流すとたるんでしまう.</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;">EIと違い,近接する対向電圧から大きな引力がかかるため,</span><br />
<span style="background-color: white; font-family: inherit; line-height: 18px;">焼成ではたるみを防げないのだと考えている.</span><br />
<span style="font-family: inherit; line-height: 18px;">初期過程前に1400度まで加熱する際の微妙なさじ加減によって,</span><br />
<span style="font-family: inherit; line-height: 18px;">たるみがなくてもイオン化効率の高いエミッターができることがある.</span><br />
<span style="font-family: inherit; line-height: 18px;">このようになる条件を探し,確実に再現することを目指すことにする.</span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;"><br /></span></span>
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">・MALDI(Voyager)</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">DHBを用いた場合に外部標準として使用するために</span><span style="background-color: white; line-height: 18px;">糖の混合物を検討していたが,</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">糖のイオン化効率が小さく,難航していた.</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">イオン化効率が小さいと,</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">レーザーを強くするか場所を変えながら積算しなくてはならない.</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">どちらの場合も分解能が落ちてしまう.</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">出来るだけ少ない標準試料の使用で感度を稼ぐため,</span></span><br />
<span style="font-family: inherit;"><span style="background-color: white; line-height: 18px;">DHB由来のピークと1,2種類のシクロデキストリンを使うことにした.</span></span><br />
<span style="font-family: inherit;"><span style="line-height: 18px;">広範囲のキャリブレーションを行う際はPEGを用いている.</span></span><br />
<br />Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-34853644012823880862013-06-09T20:53:00.003+09:002013-06-30T21:03:05.475+09:005月まとめ・FD/FI(GCv)<br />
GCで通常使用するカラムをDB-1HTからHP-5に変更した.<br />
これにより,クロマトのテーリングは改善された.<br />
DB-1HTが劣化していたのかもしれないし,<br />
液相の変更により分離が改善されただけかもしれない.<br />
<br />
<br />
・MALDI(Voyager)<br />
低極性溶媒(CHCl3やacetone)にしか溶けない<br />
高分子合成化合物を測定した.<br />
主な官能基はフェニル基とアミド基があった.<br />
<br />
DHBを用いた場合に外部標準として使用するために<br />
糖の混合物を検討した.<br />
<span style="background-color: white; line-height: 18px;"><span style="font-family: inherit;">pullulanは三残基刻みで出ず,</span></span><br />
<span style="background-color: white; line-height: 18px;">一残基刻み(162間隔)だった.</span><br />
<br />
CHCAを用いた場合に外部標準として使用するために<br />
angiotensinⅠとinsulin(bovine)<br />
<br />
<br />
<br />
<br />
<br />
--------------------------------------------<br />
default calibrationを用いた場合,<br />
<i>m/z</i> 1000程度ではどの条件でもずれが1Da未満だった.<br />
<i>m/z</i> 5000程度では条件によっては10Da以上ずれていた.<br />
<br />
PEGを測定してキャリブレーションに使おうと試みた.<br />
PEG3350まではうまく測定できたが,PEG6000は弱く,また,ベースライン分離しなかった.<br />
<i>m/z</i> 4000弱まではキャリブレーションに使えそうだった.<br />
ペプチドに比べて強度が出にくく,照射位置を固定して十分な強度を得ようとすると,<br />
大きめの結晶を使うことになってしまう.<br />
大きな結晶を使うと前述のように横軸がずれるので,キャリブレーションに適さない.<br />
間隔の広い混合物を使うと,生成するイオン量が同じ場合に各ピークの強度が上がる.<br />
質量ベースで炭素の割合が低いほどモノアイソの相対強度が高くなる.<br />
モノアイソの相対強度が高いものを用いて,モノアイソでキャリブレーションをしたい.<br />
<br />
同位体分離していないと重心値の算出と正しい計算値の算出が難しい.<br />
<div>
同位体分離しておらず左右非対称の場合,その重心値をどう扱えばいいのかわからない.</div>
<div>
<br /></div>
<br />
ピペッターを使わず,ピペットキャップを使うと<br />
キャップを押しすぎて噴き出す場合がある.<br />
ピペッターを使っている限り,空気を吐き出す心配がない.<br />
<br />
エアコンの設定を変えると,ピークがとても弱くなった.<br />
以前の設定は冷房,22℃,風速強だった.寒かった.<br />
試しに冷暖自動,24℃,風速自動にしてみた.暑かった.<br />
結局,冷房,22℃,風速自動にした.<br />
次にメンテナンスがあるときに室温を(冷房,24℃程度に)変更することにする.<br />
<br />
<br />
・持ち越し<br />
SXで測定中にQ1,2がずれる.<br />
<br />
GCvでFDの測定時にデフレクタバランスがずれる.<br />
サンプルを載せるときにワイヤーが動くのか<br />
カソード電圧のOFF→ONで動くのか<br />
たるみのないエミッターにすることで回避できるか<br />
EIのフィラメントと同様に,初めて電流を流すときに穏やかにするとどうか<br />
<br />
HP-5でテーリングが起きるか確認する.<br />
<br />
FDでフラグメントが強いサンプルをMALDIで測定してみる.<br />
ヘテロ原子の少ない低極性化合物<br />
ラジカルが発生しないため,フラグメント化を防げると期待<br />
<br />
MALDIでキャリブレーションに使える糖,ペプチドを探す.<br />
三糖の繰り返しで約500Da刻みになるpullulanはどうか<br />
キャリブレーション作成時と異なる条件(レーザー,マトリックス,測定範囲など)でのずれ<br />
<br />Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-24948861852396658002013-05-16T15:58:00.000+09:002014-05-26T14:42:50.751+09:00エミッター活性化(5回目)<br />
<br />
5/9真空引き,準備<br />
<br />
5/14~16活性化<br />
<br />
値付け<br />
アセトンを使ったイオン化効率の評価(基準のエミッターを12万としたときで単位は万)<br />
1:5<br />
2:14<br />
3:15<br />
4:12<br />
5:5<br />
1はのぞき穴が付いている場所<br />
2→5は1から時計回り(アクチベーターから取り出して上を向けた状態で)<br />
<br />
スカスカで,中心のごく一部だけが密集している.<br />
<div>
<br />
光高温度計は確認にのみ使用し,<br />
電流値はあらかじめ設定した通りにした.<br />
<br />
ベンゾニトリルを流さず,高真空(<e-4)の状態で徐々に電流値を上げた.<br />
5mA:30分<br />
10mA:30分<br />
15mA:30分<br />
20mA:30分<br />
25mA:30分<br />
30mA:30分<br />
35mA:60分<br />
40mA:60分<br />
<br />
ベンゾニトリルを流して以降は通常通りに進めた.<br />
<br />
35mA:5分<br />
40mA:5分<br />
35mAで保持</div>
Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-39670623496245029492013-05-09T11:00:00.000+09:002014-05-26T14:43:05.053+09:00エミッター活性化(4回目)<br />
4/25真空引き,準備<br />
<br />
5/7~9活性化<br />
<br />
値付け<br />
アセトンを使ったイオン化効率の評価(基準のエミッターを12万としたときで単位は万)<br />
1:36<br />
2:36<br />
3:39<br />
4:38<br />
5:34<br />
1はのぞき穴が付いている場所<br />
2→5は1から時計回り(アクチベーターから取り出して上を向けた状態で)<br />
<div>
<br />
光高温計は確認にのみ使用し,<br />
電流値はあらかじめ設定した通りにした.<br />
5mA:1分<br />
10mA:1分<br />
15mA:1分<br />
20mA:1分<br />
25mA:1分<br />
30mA:1分<br />
35mA:10分<br />
40mA:10分<br />
35mAで保持</div>
<div>
<br /></div>
Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-27466654742968079502013-05-02T09:35:00.000+09:002014-05-26T14:43:15.282+09:00エミッターのワイヤー張り<span style="font-family: Arial, Helvetica, sans-serif;">エミッター活性化には,あらかじめワイヤーを溶接したエミッターを用いる.</span><br />
<span style="font-family: Arial, Helvetica, sans-serif;"><br /></span>
<span style="font-family: Arial, Helvetica, sans-serif;">使用するものは日本電子から売られているエミッター支柱と,</span><span style="font-family: Arial, Helvetica, sans-serif;">タングステンワイヤーで,</span><br />
<span style="font-family: Arial, Helvetica, sans-serif;">溶接は</span><span style="font-family: Arial, Helvetica, sans-serif;">スポット溶接機で行う.</span><br />
<span style="font-family: Arial, Helvetica, sans-serif;"><br /></span>
<br />
<br />
<br />
<br />
<br />
<br />
張り終わったものは実体顕微鏡下で,はみ出しやたるみがないかチェックする.<br />
<br />
<br />
失敗した場合は,ワイヤーを取り除き,先端を研磨してから再度ワイヤーを張る.<br />
<br />
<span style="font-family: Arial, Helvetica, sans-serif;">使用済みのエミッターはワイヤーを取り除き,洗剤を使って超音波洗浄する.</span><br />
<span style="font-family: Arial, Helvetica, sans-serif;">その後,先端を研磨してからワイヤーを張る.</span><br />
<br />
<br />
<br />
ピンと張った状態で溶接棒を押しあてると<br />
上向きに弓なりにたわむことがある.Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-45971274475525278132013-04-30T18:50:00.000+09:002014-05-27T21:27:05.408+09:004月まとめ・FD/FI(GCv)<br />
ずっと使っていたDB-1HTでGCFIを行うとクロマトがテーリング気味だった.<br />
エミッターの焼き出しが不十分だと考え,焼きだし時間を長くした.<br />
これに合わせて,スペクトル記録間隔(積算間の待ち時間)を長くした.<br />
同じGCの条件でGCEIを測定すると,同様にテーリング気味だった.<br />
カラムを変えてDB-17HTにしてもテーリング気味で,注入口を疑った.<br />
注入口ライナー,金シールが目に見えて汚れていたため,交換した.<br />
それでも改善しなかったことから,カラムが劣化していると判断した.<br />
ある濃度より下がるとテーリングだけでなく,極度の強度低下があった.<br />
カラムが劣化しているとすると,この強度低下も説明が付く.<br />
<br />
極性の高いrutinやsucroseを高温(80℃)で測定したが,<br />
フラグメントの量は変わらなかった.<br />
NaIを添加するとフラグメント化を抑えることができたが,<br />
[M+2Na+I]+も弱いながら出た.<br />
<br />
DB-1HT(0.25mm,30m)の注入口側を外して,<br />
末端をサンプルチューブにかざすことでヘッドスペースの測定を試みた.<br />
CHCl3は問題なく測定できたが,<br />
mentholは一向に出てこず,カラムをオーブンで加熱する必要があった.<br />
<br />
<br />
・MALDI(Voyager)<br />
分子酵素から基本的な使用法を教わり,その後,試薬を測定してみた.<br />
基本的には希釈した溶液をエッペンで混合して,そこから1ul未満をスポットした.<br />
ピペットマンP20は最少で2ulしか量れないため,2ulの設定で軽く押すようにした.<br />
サンプル量が少ない場合は,ulレベルの溶液をパラフィルム上で混合して,<br />
そこから一部をスポットした.<br />
<br />
分解能はレーザー照射の仕方によって大きく変わった.<br />
照射位置をずらしながら積算していくと,<br />
常に新しい結晶を使えるため強度は出るが,ピークがブロードになり,分解能が落ちる.<br />
ある地点を照射し始めてしばらくは爆発的にイオンが出る.<br />
このときもピークが若干ブロードになり,分解能が落ちる.<br />
数スキャン空打ちしてから積算を始めると安定したピークが得られ,分解能が上がる.<br />
<br />
ダマになった大きな結晶を使うと,3Daほど小さく出た.<br />
大きな結晶だと強度が出やすいが,使ってはいけないようだ.<br />
<br />
default calibrationを用いた場合,<br />
<i>m/z</i> 1000程度ではどの条件でもずれが1Da未満だった.<br />
<i>m/z</i> 5000程度では条件によっては10Da以上ずれていた.<br />
<br />
PEGを測定してキャリブレーションに使おうと試みた.<br />
PEG3350まではうまく測定できたが,PEG6000は弱く,また,ベースライン分離しなかった.<br />
<i>m/z</i> 4000弱まではキャリブレーションに使えそうだった.<br />
ペプチドに比べて強度が出にくく,照射位置を固定して十分な強度を得ようとすると,<br />
大きめの結晶を使うことになってしまう.<br />
大きな結晶を使うと前述のように横軸がずれるので,キャリブレーションに適さない.<br />
間隔の広い混合物を使うと,生成するイオン量が同じ場合に各ピークの強度が上がる.<br />
質量ベースで炭素の割合が低いほどモノアイソの相対強度が高くなる.<br />
モノアイソの相対強度が高いものを用いて,モノアイソでキャリブレーションをしたい.<br />
<br />
同位体分離していないと重心値の算出と正しい計算値の算出が難しい.<br />
<div>
同位体分離しておらず左右非対称の場合,その重心値をどう扱えばいいのかわからない.</div>
<div>
<br /></div>
<br />
ピペッターを使わず,ピペットキャップを使うと<br />
キャップを押しすぎて噴き出す場合がある.<br />
ピペッターを使っている限り,空気を吐き出す心配がない.<br />
<br />
エアコンの設定を変えると,ピークがとても弱くなった.<br />
以前の設定は冷房,22℃,風速強だった.寒かった.<br />
試しに冷暖自動,24℃,風速自動にしてみた.暑かった.<br />
結局,冷房,22℃,風速自動にした.<br />
次にメンテナンスがあるときに室温を(冷房,24℃程度に)変更することにする.<br />
<br />
<br />
・持ち越し<br />
SXで測定中にQ1,2がずれる.<br />
<br />
GCvでFDの測定時にデフレクタバランスがずれる.<br />
サンプルを載せるときにワイヤーが動くのか<br />
カソード電圧のOFF→ONで動くのか<br />
たるみのないエミッターにすることで回避できるか<br />
EIのフィラメントと同様に,初めて電流を流すときに穏やかにするとどうか<br />
<br />
HP-5でテーリングが起きるか確認する.<br />
<br />
FDでフラグメントが強いサンプルをMALDIで測定してみる.<br />
ヘテロ原子の少ない低極性化合物<br />
ラジカルが発生しないため,フラグメント化を防げると期待<br />
<br />
MALDIでキャリブレーションに使える糖,ペプチドを探す.<br />
三糖の繰り返しで約500Da刻みになるpullulanはどうか<br />
キャリブレーション作成時と異なる条件(レーザー,マトリックス,測定範囲など)でのずれ<br />
<br />
<br />Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-40189229459330455692013-04-25T20:38:00.000+09:002014-05-26T14:43:23.207+09:00エミッター活性化(3回目)<br />
4/11真空引き,準備<br />
のぞき窓とお釜の底の土台を磨いた.<br />
<br />
4/23~25活性化<br />
<br />
値付け<br />
アセトンを使ったイオン化効率の評価(基準のエミッターを12万としたときで単位は万)<br />
1:18<br />
2:9<br />
3:<br />
4:16<br />
5:23<br />
1はのぞき穴が付いている場所<br />
2→5は1から時計回り(アクチベーターから取り出して上を向けた状態で)<br />
<div>
<br />
初期過程を始めたところで誤って電源を切った.<br />
その後,電源を入れた際に,急に33mA流してしまった.<br />
<br />
取り出してみると3番が切れていた.<br />
中心部でもウィスカーが密集しておらず,とびとびで生えていた.</div>
Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-27091724878431999222013-04-13T20:47:00.001+09:002013-04-13T20:47:16.595+09:00エミッターの消耗エミッターには微小細針があり,これがイオン化に必要な高電界を生んでいる.<br />
エミッターの使用によりその細針は消耗していく.<br />
消耗には,細針の数の減少と,各細針の鋭利さの低下がある.<br />
<br />
消耗したエミッターを使うとイオン量が少なく,フラグメント化が強くなる.<br />
<br />
-細針の数の減少<br />
-各細針の鋭利さの低下<br />
Lイオンの生成による<br />
L電流の通電による<br />
<br />
・細針の数が異なる新品のエミッター間で比較<br />
・イオン生成や通電の前後のエミッターの状態を顕微鏡で観察Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-11234236329896436582013-04-11T20:38:00.000+09:002014-05-26T14:43:32.516+09:00エミッター活性化(2回目)<br />
4/4真空引き,準備<br />
4/9~11活性化<br />
大きな失敗は無かった.<br />
<br />
値付け<br />
アセトンを使ったイオン化効率の評価(基準のエミッターを12万としたときで単位は万)<br />
1:22<br />
2:22<br />
3:22<br />
4:16<br />
5:22<br />
1はのぞき穴が付いている場所<br />
2→5は1から時計回り(アクチベーターから取り出して上を向けた状態で)<br />
<br />
1400℃にする過程は45 mAで一瞬に留めた.Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-2597310336386484542013-04-09T20:24:00.002+09:002013-04-09T20:24:15.696+09:00チューニングチューニングはすべてリザーバーから導入したガスをFIでイオン化させて行っている.<br />
<br />
・<i>m/z</i> 207, 222, 281, 355, 429のいずれか<br />
ドリフト補正に用いるcyclosiloxane混合物をそのまま使用する.<br />
五量体,六量体は沸点が高く,エミッターに残りやすい.<br />
強度が下がっていく中で手早くチューニングするか,頻繁に焼きだしをする.<br />
<br />
・<i>m/z</i> 281<br />
cyclosiloxaneの四量体だけを使用する.<br />
エミッターへの吸着はほとんどない.<br />
<i>m/z</i> 281はEIでもチューニングに使用する値なので,ピーク形状の比較ができる.<br />
<br />
・<i>m/z</i> 58<br />
アセトンを使用する.<br />
イオン化効率が極めて高い.<br />
エミッターへの吸着はない.<br />
実際に測定する質量範囲よりかなり低質量である.Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-40055884583048510032013-04-04T20:46:00.001+09:002013-04-04T21:03:02.205+09:00α-cyclodextrin<span style="font-family: Arial, Helvetica, sans-serif;">C</span><span style="font-family: Arial, Helvetica, sans-serif; font-size: xx-small;">36</span><span style="font-family: Arial, Helvetica, sans-serif;">H</span><span style="font-family: Arial, Helvetica, sans-serif; font-size: xx-small;">60</span><span style="font-family: Arial, Helvetica, sans-serif;">O</span><span style="font-family: Arial, Helvetica, sans-serif; font-size: xx-small;">30</span><br />
<span style="font-family: Arial, Helvetica, sans-serif;">単同位体質量:972</span><br />
<span style="font-family: Arial, Helvetica, sans-serif;">boiling point:℃</span><br />
<span style="font-family: Arial, Helvetica, sans-serif;"><br /></span><a href="https://docs.google.com/file/d/0B-vDMt-S8b0JLW5uU3ZMSUctMVE/edit?usp=sharing">スペクトル</a><br />
<span style="font-family: Arial;"><em>m/z</em> 995:[M+Na]+</span><br />
<span style="font-family: Arial;"><br /></span>
Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.comtag:blogger.com,1999:blog-6364025706792977601.post-88102142736483794952013-04-04T17:24:00.000+09:002014-05-26T14:43:43.606+09:00エミッター活性化(1回目)<span style="font-family: Arial;">真空引き,準備が済んでいる状態から開始</span><br />
<span style="font-family: Arial;">4/2~4活性化</span><br />
<div style="font-family: "MS PGothic";">
<span style="font-family: Arial;"><span style="font-family: Arial, Helvetica, sans-serif;">2日目の夕方,エミッター電流を2 mA / hrで上昇させるのを<span style="color: red;">忘れてしまった</span></span></span><span style="font-family: Arial, Helvetica, sans-serif;">.</span></div>
<div style="font-family: "MS PGothic";">
<span style="font-family: Arial;"><span style="font-family: Arial, Helvetica, sans-serif;">3日目の朝,活性化を中止しFI用エミッターとする.</span></span></div>
<br />
<span style="font-family: Arial;"><br /></span>
<span style="font-family: Arial;">値付け</span><br />
<span style="font-family: Arial;">アセトンを使ったイオン化効率の評価(基準のエミッターを12万としたときで単位は万)</span><br />
<span style="font-family: Arial;">1:14</span><br />
<span style="font-family: Arial;">2:26</span><br />
<span style="font-family: Arial;">3:37</span><br />
<span style="font-family: Arial;">4:32</span><br />
<span style="font-family: Arial;">5:21</span><br />
<span style="font-family: Arial;">1はのぞき穴が付いている場所</span><br />
<span style="font-family: Arial;">2→5は1から時計回り(アクチベーターから取り出して上を向けた状態で)</span>Anonymoushttp://www.blogger.com/profile/01220924264963176462noreply@blogger.com