主题:【讨论】为什么同样的方法和样品5973比5975的峰高和峰面积要大???

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怪侠一把刀
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During the calibration using ATUNE.U file the valve containing calibrant opens and the high vacuum pump draws the calibrant into the ion source in the vacuum chamber. Here calibrant gets ionized and measured. The physical positioning of the calibration valve will determine how much calibrant and the path of the calibrant into the vacuum chamber. The location of the calibration valve on the 5973 MSD was located on the front of the vacuum manifold while for the 5975 MSD it is located on top of the manifold above the source. In 5975 the position of the valve will result in more calibrant into the ion source chamber and as a result it will lower electron multiplier voltages (EMV) for the tune results. The tune criteria will still be correct and acceptable but the EMV will be slightly lower.
The tune criteria/targets for the 5975 and the 5973 are the same for Autotune (ATUNE.U).
Set Tune Masses are 69, 219, and 502 Tune Limits 。Target abundance counts is 500000 Peak width is 0.6 amu Maximum Repeller voltage is 35 Emission Current is set to 34.6 (35) Maximum Ion Focus voltage is 90
Using the same tune criteria for the 5975 and for the 5973 will result in different results when samples are injected in 5975. This is because the calibrant is infused closer to the source and through a larger restrictor on the 5975 compared to the 5973. The algorithms and calculations which are done are the SAME for the tuning process for the 5975 MSDs and the 5973 MSDs. Customers using the same EMV offset for the method will see a lower response when a sample is injected. Customers who want the same response (peak height/areas) need to adjust the Electron Multiplier Voltage until the response matches their 5973. This can be done via the EMV offset within the method or another alternative is to adjust the abundance targets in the tune file which has the same effect
当用自动调谐校正的时候,标准调谐物质通过真空管路进入真空离子源。在此,标准品被离子化和测定。标准品的物理位置影响有多少标准品进入和通过什么途径进入真空腔内。5793的标准品位于真空管的前面,然而5975的标准品位于离子源的上面。这样的位置于是导致5975中会吸取多的标准物质调谐,然而得到一个较低的EMV电压。这样的调谐结果校正完之后,导致EMV电压相对5973要小。
两者的自动调谐标准物质都一样。
设置调谐质量为69、219、502。目标离子丰度为500000;峰宽为0.6amu;最大推斥电压为35,目前设置为34.6;最大离子聚焦电压为90。
在5973和5975中使用相同的标准调谐物质会导致不同的结果。这个是因为在5975中,标准物质会通过一个更大的限流器、更加接近离子源地进入真空管路。然而5973和5975两者的运算法则一致,当测定同一样品用户使用相同的EMV的时候5975会得到更加低的信号响应,如果需要得到一样的响应值,用户需要自己调节EMV使之与5973接近。这个可以通过调节方法中EMV的抵消值或调节调谐文件中丰度目标值来完成。


我自己翻译的,不当的地方希望大家指出……
很遗憾没有人响应!
怪侠一把刀
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接下来我打算列出一些经典的TROUBLE-shootings
英文部分,欢迎大家来协助翻译!
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我如何解决“扩散泵过热或过冷的问题”?
这个问题有三种可能的原因:
1 不正确的扩散泵的换油方式。太多的油会导致过冷、太少而导致过热。放空系统,检查油的位置是否位于手册中推荐的位置。
2 扩散泵的冷气扇没有正确运转,或者正对着一堵逆空气流。测试:将手放置于扩散泵后面,感受是否有热气从MS中溢出。
3 泵的热开关故障。您可以按照硬件手册中的问题解答中的提示解决。如果一个或者多个开关故障,扩散泵就需要更换了。按照用户维护手册中检查你仪器版块上的电缆,如果更换需要用到#8710-0614号工具,此工作并没有随机附带。
How do I clear the error: The diffusion pump is too hot, or too cold?
This error has three likely causes.
A. The diffusion pump has an improper charge of diffusion pump oil, where too much will make it run cold, too little fluid will run too hot. Vent the system and check the fluid level versus the volume recommended in the hardware manual
B. The diffusion pump cooling fan is not operating at the correct speed, or being up against a wall restricts the airflow. Place your hand behind the diffusion pump, and feel if warm air is being exhausted out of the MSD.
C. The thermal switches on the pump are faulty. You can check this using the troubleshooting section of the hardware manual. If one or both switches are faulty, the diffusion pump cable will require replacing. Check your hardware manual parts section for the cable for your instrument model. To replace the cable, a tool, Agilent Technologies part # 8710-0614 will be required. This tool is not part of the tool kit shipped with the instrument
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留下一个欢迎大家来翻译:关于调谐周期的问题!!!!!!!

How often should I perform tuning?
The frequency of tuning depends on a wide range of factors including the number of analyses and the characteristics and concentration of the measurement samples. It is not possible to give an answer that covers all situations.
However, as it is unlikely that the state of the MSD will change significantly in one day, one approach is to combine an autotune and quick tuning.
For a unit that is operating continuously, a schedule whereby you perform tuning and check the condition every two days and perform an autotune every week will keep the MSD in optimum condition.
However, an autotune must be performed in the following cases.
1. After replacing the column, maintenance of the MS, or a system shutdown.
2. When a method that changes the ion source temperature, MS transfer line temperature, or column flow is used.
3. If the reference is not achieved for a sensitivity variation test.
If no reference of the type in case 3 above is specified, it is recommended that this be performed before the quantitative analysis. Remember to always keep the gc oven temperature, ion source temperature, MS transfer line temperature, and column flow rate constant when performing the autotune.
天下为公
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应该多长时间进行一次調諧?
調諧的频率取决于分析样品的数量、特性、濃度范围。 但沒有確切的統一的標准。
在一天裡沒必要對質譜做兩次調諧,解決的辦法之一是结合自動調諧和快速調諧。 
对于待機的機器来说,有必要做一份每二天調諧并且检查状态并且每周执行一次自動調諧的时刻表並凭此将保持機器在最佳状态。
不过,自動調諧必须在下列狀況下执行:
1.換柱子,質譜的維護,或者系统关機之后。
2.新的方法改編了离子源、傳輸線温度以及柱流量。
3.如果沒有通過靈敏度測試。
如果上面沒有提及,建议这被在定量分析之前执行調諧。 並保持炉度,离子源温度,傳輸線温度和柱子流量不變。
怪侠一把刀
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正当我等的花儿都快谢了的时候,楼上来了场及时雨啊!
很经典的翻译!谢谢支持!!!!!!!!!
不知道大家对这个问题是否关注?
怪侠一把刀
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For a unit that is operating continuously, a schedule whereby you perform tuning and check the condition every two days and perform an autotune every week will keep the MSD in optimum condition.

其中这句两天一次的调协,建议为manual调协,查看系统真空状态怎么样?
这样可否?
gentlehorse
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怪侠一把刀
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TS:4  MS的灵敏度降低,如何纠正?
The MS sensitivity has deteriorated. How can I correct it?
There are various possible causes for a deterioration in the sensitivity. The most common are listed below.

1. A problem with the sample. (The target component has transformed, or is volatile and has been lost)
2. A problem with the column (Column is dirty, liquid phase is broken, etc.)
3. A problem with the gc inlet (Insert is dirty, septum is holed or has been transformed, etc.)
4. A problem with the MSD (Ion source is dirty, mass axis is out of alignment, poor vacuum due to leak, etc.)
5. A connection problem (Sample has escaped due to a leak, length of column emerging from ferrule is incorrect, etc.)
6. A problem with the injection conditions (Split has changed, purge time is too short, etc.)
7. A problem with injection (Metering is inaccurate, septum particles are jammed in needle preventing sample from being taken in, etc.)
8. Fault in Instrument (Fault in the MSD, fault in the gc flow system)
The MSD can be checked by looking at the autotune results.
Check each of the potential causes and make necessary corrections.
If the problem is still not fixed, contact the Agilent customer service center
灵敏度减弱有很多因素,以下列出较常见的部分:
1.样品的问题(目标组分转化,或者不稳定而丢失)
2.柱子的问题(柱子脏了或者其固定液破坏流失等)
3.gc进样口的问题(进样口污染,隔垫扎破、变形等)
4 MS的问题(离子源污染,质谱轴脱离校准轴、真空度差)
5.gc与MS之间的连接问题(由于伸入MS部分的柱子长度不合适而导致样品丢失)
6.进样条件的问题(分流改变,进样切换时间太短)
7.进样针的问题(进样针未正确校准、或者针头被隔垫颗粒堵住影响进样量)
8.仪器自身错误(MS错误、gc分离错误)
质谱部分的问题可以通过自动调谐的结果检查出来,检查每个可能的潜在因素,并且进行必要的更正。
如果问题依然存在,可以致电服务中心。
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原文由 gentlehorse 发表:
那信噪比有什么差别吗?


??????
哪两者之间的差别?
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