清晨好,您是今天最早来到科研通的研友!由于当前在线用户较少,发布求助请尽量完整地填写文献信息,科研通机器人24小时在线,伴您科研之路漫漫前行!

Characterizing the thermal phase behaviour of fipronil polymorphs

升华(心理学) 再结晶(地质) 亚稳态 结晶学 化学 多态性(计算机科学) 粉末衍射 溶剂 熔点 材料科学 有机化学 基因型 基因 古生物学 生物 生物化学 心理学 心理治疗师
作者
Dennis Simbarashe Moyo,Elizabet M. van der Merwe,M. Rademeyer,Frederick P. Malan,Maria Atanasova,António Benjamim Mapossa,Walter W. Focke
出处
期刊:Journal of Thermal Analysis and Calorimetry [Springer Science+Business Media]
卷期号:148 (14): 6761-6777 被引量:1
标识
DOI:10.1007/s10973-023-12198-x
摘要

Abstract This manuscript reports the investigation of the polymorphic behaviour of fipronil using a systematic comparison of the thermochemical and structural properties of different crystal forms obtained in this study as well as those previously reported in literature. The analytical techniques employed include DSC, TGA, PXRD, SCXRD and hot stage microscopy. DSC proved particularly useful because it made it possible to differentiate between the two different crystal forms found in the as-received neat fipronil. The DSC scans revealed the presence of two polymorphs which had melting endotherms with peak maxima at ca . 196 °C and 205 °C, respectively. These polymorphs were successfully separated via sublimation and resulted in a metastable, lower melting polymorph in the sublimate and a thermodynamically stable, higher melting form in the sublimation residue. Clear evidence for the instability of the lower melting polymorph was found when the endotherms were examined under a range of heating rates. The proportion of the metastable form appeared to increase as the rate was increased, indicating that the metastable form underwent a solid–solid phase transition to the stable form at low heating rates. Recrystallization of fipronil from different solvents yielded five different forms. TGA curves revealed that all forms, except the acetone-derived one, were solvate pseudo-polymorphs that showed solvent loss between 60 and 100 °C. The acetone-derived sample was a hemihydrate that only started to show mass loss at 120 °C. SCXRD studies revealed that three of the five forms have similar structural characteristics, while the other two forms differ notably from each other and the rest of the structures. Despite these structural differences, all five forms exhibit near-identical intra- and intermolecular hydrogen bond networks.
最长约 10秒,即可获得该文献文件

科研通智能强力驱动
Strongly Powered by AbleSci AI
更新
PDF的下载单位、IP信息已删除 (2025-6-4)

科研通是完全免费的文献互助平台,具备全网最快的应助速度,最高的求助完成率。 对每一个文献求助,科研通都将尽心尽力,给求助人一个满意的交代。
实时播报
xue完成签到 ,获得积分10
2秒前
丘比特应助科研通管家采纳,获得10
3秒前
林利芳完成签到 ,获得积分0
43秒前
研友_8y2G0L完成签到,获得积分10
46秒前
47秒前
52秒前
1分钟前
小焦儿发布了新的文献求助10
1分钟前
1分钟前
吃的饭广泛应助小焦儿采纳,获得10
1分钟前
谭平完成签到 ,获得积分10
1分钟前
科研的豪哥完成签到 ,获得积分10
1分钟前
小焦儿完成签到,获得积分10
1分钟前
完美梨愁完成签到 ,获得积分10
1分钟前
wanci应助无限的以亦采纳,获得10
1分钟前
糟糕的翅膀完成签到,获得积分10
1分钟前
creep2020完成签到,获得积分10
1分钟前
谭凯文完成签到 ,获得积分10
2分钟前
lorentzh完成签到,获得积分10
2分钟前
2分钟前
YX完成签到 ,获得积分10
2分钟前
2分钟前
Sandy应助Am采纳,获得20
2分钟前
桐桐应助嘿嘿嘿侦探社采纳,获得10
2分钟前
ycool完成签到 ,获得积分10
2分钟前
小强完成签到 ,获得积分10
2分钟前
大树完成签到 ,获得积分10
3分钟前
3分钟前
3分钟前
3分钟前
3分钟前
3分钟前
naiyantang完成签到 ,获得积分10
4分钟前
科研通AI2S应助科研通管家采纳,获得10
4分钟前
周常通完成签到,获得积分10
4分钟前
4分钟前
xiaosui完成签到 ,获得积分10
4分钟前
lingling完成签到 ,获得积分10
4分钟前
浪麻麻完成签到 ,获得积分10
4分钟前
提提在干嘛完成签到,获得积分10
5分钟前
高分求助中
A new approach to the extrapolation of accelerated life test data 1000
Cognitive Neuroscience: The Biology of the Mind 1000
Technical Brochure TB 814: LPIT applications in HV gas insulated switchgear 1000
Immigrant Incorporation in East Asian Democracies 600
Nucleophilic substitution in azasydnone-modified dinitroanisoles 500
不知道标题是什么 500
A Preliminary Study on Correlation Between Independent Components of Facial Thermal Images and Subjective Assessment of Chronic Stress 500
热门求助领域 (近24小时)
化学 材料科学 医学 生物 工程类 有机化学 生物化学 物理 内科学 纳米技术 计算机科学 化学工程 复合材料 遗传学 基因 物理化学 催化作用 冶金 细胞生物学 免疫学
热门帖子
关注 科研通微信公众号,转发送积分 3968521
求助须知:如何正确求助?哪些是违规求助? 3513341
关于积分的说明 11167298
捐赠科研通 3248700
什么是DOI,文献DOI怎么找? 1794417
邀请新用户注册赠送积分活动 875030
科研通“疑难数据库(出版商)”最低求助积分说明 804664