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回复haibingxu发表于：2020/7/26 22:08:44悬赏金额：4积分状态：未解决

请教各位专家一个问题。

我是做碳纤维表面的改性的，最近投了一篇稿子，其中XPS分析，用的是C1s（284.8 ev）校准的。相关的文献也是这么做的。

审稿人提出了这样的问题：

C1s is used to calibrate the binding energy ofother chemical elements. However, in this manuscript, C1s should have achemical shift as it is bonded with other element. Therefore, the bingdingenergies of the analyzed elements should be re-calibrated by another element. Most possiblely, the author should introduce Pt or Ag in order to do this.

审稿人，让我们再用Pt 或者Ag校准一遍，事实上，我们觉得没有重复实验的必要。因为相关文献都是这么做的，而且，我们的结果也是与文献相符的。

但是，不知道如何去说服审稿人。

1# v2721826 回复于：2020-07-31 08:58:44

Calibration using the C1s peak is indeed the most common way of peak-calibration before determining the Chemical state in XPS spectra.

But calibrating what you think is "a known peak" as C-C peak to 284.8eV meaning = You believe or have made an ASSUMPTION, that this particular peak is in the Chemical state form of C-C. The judgment from your auditor is challenging that from the nature of your sample the peak you calibrated to 284.8eV may NOT be purely in C-C Chemical state because he/she is expecting that with sample nature it is something more than C-C (meaning its energy would not fall at exactly 284.8eV). So the Auditor is simply challenging the ASSUMPTION you made is not correct.

If you do not want to do like the auditor suggested to introduce standard thin-layer of pure metal so be able to use its peak for calibration, what you should do is that to show and prove your final result and ASSUMPTION is "reasonable" instead of simply saying "All other papers did the same way and got expected result".

My suggestion is that I am guessing your sample mainly just have some O1s and C1s signal. If there are other signals, then your final result should have Chemical state of all elements. To prove a correct Chemical state judgment, one will need to do a complete data interpretation including:
(1) Determine all presented elements
(2) Do curve fitting for all presented elements and assign Chemical state
(3) With all elements assigned with Chemical state, one should do a Quantification of all presented elements in each Chem-state.

If the final quantification between Chem-state is matching to the assigned Chem-state formula, then you can show this is a good proof to the auditor your result is correct.

For example, if C1s peak after curve fitting have 2's Oxide-related Chem-state as CO, CO2 state and corresponding quantification are 10% and 20% > then respectively in the O1s peak there should be corresponding 10% and 40% (because CO2=1C+2O), so O1s concentration should be roughly 50%.

If the quantification result between ALL elements in final assigned Chem-state forms can match roughly your judgment, then you can say to the auditor your result is correct.

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