主题:【已应助】Fe重复性差。

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xie20051106
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出现这样的情况应该是进样系统污染了吧,楼主有没有清洗过进样系统呢?
砂锅粥
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原文由 xie20051106(xie20051106) 发表:
出现这样的情况应该是进样系统污染了吧,楼主有没有清洗过进样系统呢?
没做过Fe基含量高的样品呀。一般都是进完样之后冲洗,没有特意拆出来清洗,除非用得比较久了就会把雾化室,中心管,炬管等拆下来洗。
hbmy2008hbmy
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原文由 czcht(czcht) 发表:
原文由 hbmy2008hbmy(hbmy2008hbmy) 发表:
楼主要注意仪器的提示是目标元素饱和,还是其旁边的元素饱和
请问怎么区别目标元素饱和还是旁边的元素饱和?


楼主可以看光谱图或result,里面有提示,是Code No提示

代码 描述
2 “饱和 2”显示在“结果显示”中的“净强度”列中。此信息也显示在“光谱显示”窗口中。此代码和消息只适用于全谱型 ICP 光谱仪。 在预采光时测量到某些波长强度太高,检测器无法读出数据。只能重新运行分析并只选择其中的一个波长,以防止出现饱和。
3 “饱和 3”显示在“结果显示”中的“净强度”列中。此信息也显示在“光谱显示”窗口中。 在预采光时测量到的分析物强度太高,即使使用 1 毫秒(最短积分时间)的积分时间,也是如此。为分析物选择的波长太灵敏,或试样包含的分析物浓度太高。
4 “饱和 4”显示在“结果显示”中的“净强度”列中。此信息也显示在“光谱显示”窗口中。 在重复测定读数期间测量到的分析物强度太高。出现这种情况可能是因为在预采光测量之前信号尚未稳定,以致在“预采光”读数读到重复测定开始的这一段时间内信号强度发生了变化。 首先,尝试增加读数延迟并重新运行分析。如果仍然出现饱和,则说明为分析物选择的波长太灵敏,或试样包含的分析物浓度太高。
5 在自动积分时,在“结果显示”窗口中显示消息“在自动积分窗口外达到饱和”。表明存在强度太高的峰,它已超出自动积分窗口范围,但在观察窗口范围内。在手工积分时,在“结果显示”窗口中显示消息“在观察窗口内达到饱和”。对于两种类型的积分,都在“光谱显示”窗口中显示消息“已饱和。代码 = 5”。 有关积分和观察窗口的详细信息,请参阅方法编辑器的“光谱窗口”页。 饱和的峰可能不属于所需的分析物,而是干扰。如果使用背景校正,请确保检查背景校正点不在出现饱和的范围内,否则校正可能无效。
6 在自动积分时,在“结果显示”窗口中显示消息“在自动积分窗口外达到饱和”。在手工积分中,消息“在观察窗口外达到饱和”显示在结果显示中。出现强度较高的峰,它已超出观察窗口。对于两种类型的积分,都在“光谱显示”窗口中显示消息“已饱和。代码 = 6”。 有关积分和观察窗口的详细信息,请参阅方法编辑器的“光谱窗口”页。 饱和的峰可能不属于所需的分析物,而是干扰。如果使用背景校正,请确保检查背景校正点不在出现饱和的范围内,否则校正可能无效。
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该帖子作者被版主 czcht5积分, 2经验,加分理由:谢应助。
hbmy2008hbmy
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下面给出英文版

Code

Description

2

"Saturated2" appears in the Net Intensity column in the Results Display. This information also appears in the Spectra Display window. This code and message applies only to simultaneous ICP spectrometers.

The intensity measured during pre-shot is too high for several wavelengths and the detector cannot read out the data. You may be able to rerun the analysis and select only one of the wavelengths to prevent saturation from occurring.

3

"Saturated3" appears in the Net Intensity column in the Results Display. This information also appears in the Spectra Display window.

The intensity measured for the analyte during pre-shot is too high, even for a 1 ms integration (the shortest integration time available). Either the wavelength chosen for the analyte was too sensitive or the sample contained too high a concentration of the analyte.

4

"Saturated4" appears in the Net Intensity column in the Results Display. This information also appears in the Spectra Display window.

The intensity measured for the analyte during the replicate readings is too high. This may have occurred because the signal wasn’t stabilized before the pre-shot measurement, so the signal intensity changed between the "pre-shot" reading and the time the replicate was measured.

For the Optima 2000/2100, in manual integration, the message "Saturation within survey window" appears in the Results Display. For either type of integration, the message "Saturated. Code = 4" appears in the Spectra Display.

First, try increasing the read delay and rerunning the analysis. If saturation still occurs, the wavelength chosen for the analyte was too sensitive or the sample contained too high a concentration of the analyte.

5

In automatic integration, the message "Saturation outside of integration window" appears in the Results Display. A peak with too high an intensity was found outside of the auto integration window but within the survey window.

For the Optima 3000/4000/5000, in manual integration, the message "Saturation within survey window" appears in the Results Display. For either type of integration, the message "Saturated. Code = 5" appears in the Spectra Display.

For more information on the integration and survey windows, refer to the Spectral Windows page in the Method Editor.

The saturated peak may not be the analyte of interest, but an interferent. If you are using background correction, be sure to check that the background correction points are not placed in the range where saturation is occurring, which can invalidate your results.

6

In automatic integration, the message "Saturation outside of integration window" appears in the Results Display. In manual integration, the message "Saturation outside survey window" appears in the Results Display. A peak with too high an intensity was found outside the Survey window. For either type of integration, the message "Saturated. Code = 6" appears in the Spectra Display.

For more information on the integration and survey windows, refer to the Spectral Windows page in the Method Editor.

The saturated peak may not be the analyte of interest, but an interferent. If you are using background correction, be sure to check that the background correction points are not placed in the range where saturation is occurring, which can invalidate your results.
手机版: Fe重复性差。
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