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yuanf2011

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[求助] 评审意见 已有1人参与

请问下大家,我这个PXRD测了很多次都是这样的,审稿人说我的样品晶相不纯,但事实上我合成的单晶样品很纯,产率很高。TGA and PXRD我也一起描述了,还让我分析什么呢?不知道下面这个问题如何回答。请指教,
评审意见如下:
Please incorporate the bulk phase purity of your synthesized complexes. Please incorporate the TGA and PXRD analysis with proper discussion.

TGA and PXRD正文 描述内容:
“The powder X-ray diffraction (PXRD) experiments for the three complexes were carried out to verify their phase purity at room temperature. The experimental PXRD diffraction patterns matches with the simulated PXRD from the single-crystal X-ray diffraction data, which implied high phase purity of the microcrystalline products. Moreover, the thermal stabilities of all three complexes were assessed with the aid of thermogravimetric analysis (TGA) (Fig. 6). Since, I, II and III are isostructural, the TG curves of these isomorphic complexes are very similar. Hence, I is selected as an example to analyze the thermal properties. In I, the first loss is ascribed to the loss of lattice and coordinated water molecules below 220 ℃ and the weight loss of 8.17% and 4.36% was consistent with that calculated values (8.78% and 4.39%). Thereafter, the dehydrated compound is stable up to 510 ℃ after which the skeleton starts to collapse till 1000oC.”

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PXRD和TG.jpg
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LeeofHIAM

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【答案】应助回帖

感谢参与,应助指数 +1
应该是合成的产物PXRD部分峰过强以至于部分峰显得很弱,建议提高显示比例,尽量保证主峰位都能肉眼对上。你这是HOF吧?
2楼2022-09-08 16:43:59
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yuanf2011

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引用回帖:
2楼: Originally posted by LeeofHIAM at 2022-09-08 16:43:59
应该是合成的产物PXRD部分峰过强以至于部分峰显得很弱,建议提高显示比例,尽量保证主峰位都能肉眼对上。你这是HOF吧?

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3楼2022-09-08 17:09:22
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4楼2022-10-30 18:50:07
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匿名

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5楼2022-11-11 21:37:27
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雷在北京

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充分研磨之后再去测PXRD试试,希望对你有所帮助

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6楼2023-09-23 11:45:27
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商艳雪

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局部提高峰强度,和模拟对比一下
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7楼2025-04-11 09:26:01
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