The Effect of Dissolved Gases as Impurities on Crystallization

Huang, Jinpei; Yin, Qiuxiang; Ulrich, Joachim

doi:10.1002/ceat.201500674

Cited by 13 publications

(5 citation statements)

References 40 publications

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“…The present study highlights that bubbles in fluid inclusions can have different compositions (gaseous solvent or a predominant gas dissolved in the mother liquor such as O 2 , CO 2 or N 2 ). Moreover, it was evidenced in other studies that dissolved gases in mother liquors play a significant role in the crystal growth rate 25 and in the formation of inclusions. 20 In order to compare the influence of the three main gases of the atmosphere on the formation of inclusions and their consequence on the behaviour of bubbles, crystallisations under N 2 , O 2 and CO 2 were performed under stagnant conditions (Fig.…”

Section: Influence Of Dissolved Gases In the Mother Liquor On The For...mentioning

confidence: 94%

Evidence of two types of fluid inclusions in single crystals

Bobo

Lefez²,

Caumon

et al. 2016

CrystEngComm

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Supplementary InfoInternational audiencea Investigations about the physico-chemical behaviour of fluid inclusions by means of thermal treatments and slow crystal dissolution lead to the evidence of two different kinds of gas bubbles. The results are reproducible for several organic and inorganic crystals obtained in aqueous solutions or organic solvents. Experiments under various pressures highlighted that the solubility of dissolved gases can play a significant role in the number of formed vacuoles. In addition, the nature of the dissolved gas in the mother liquor had an influence on the type of trapped bubbles. Raman spectroscopy confirmed that gaseous bubbles in fluid inclusions were rich in the gas that was dissolved in the mother liquor. Moreover, the pressure inside frozen aqueous fluid inclusions was estimated by measuring the temperature of the non-congruent fusion of the CO 2 clathrate that formed inside the vacuoles at −60 °C. Interferometry experiments were performed in order to visualise the consequences of the presence of vacuoles at the surface of the crystals. This study about fluid inclusion behaviours sheds new light on the formation of 3D defects in single crystals , whose mechanismĲs) of formation is (are) still difficult to understand

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Section: Influence Of Dissolved Gases In the Mother Liquor On The For...mentioning

confidence: 94%

Evidence of two types of fluid inclusions in single crystals

Bobo

Lefez²,

Caumon

et al. 2016

CrystEngComm

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“…One advantage compared to other nucleation methods like sonication , or wet milling is the simple application without extensive additional equipment and less energy input to the system, by introducing the inert gas already present in the system into the solution. Here it should be noted that the choice of inert gas may affect the crystallization process, as studies by Ceyhan et al and Huang et al suggest, explained by the combined effects of dissolved gas on solubility and crystallization kinetics and changing properties of the gas–liquid interface. In this study, argon is chosen for inert gassing.…”

Section: Introductionmentioning

confidence: 90%

Inert Gassing Crystallization for Improved Product Separation of Oleo-Chemicals toward an Efficient Circular Economy

Seifert

Simons

Gutsch

et al. 2022

Org. Process Res. Dev.

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Selective product crystallization for separation and recycling of homogeneous catalysts represents one novel promising method to develop sustainable chemical processes. This specific application holds two main challenges: (1) In the crystallization and subsequent filtration and washing process, isolation of a pure crystalline product is required to obtain the maximum quantity of catalyst in the filtrate for recycling, and (2) the entire process must be operated in an inert atmosphere to maintain the catalytic activity of oxygen-sensitive species. Key to the isolation of a pure product is precise control of the crystallization process, which is realized in this work by gassing-induced nucleation using inert argon. Assuming that the nucleation step is crucial for the control of particle properties of the crystalline product and the related efficiency of downstream separation by filtration and washing, we systematically investigated the effect of controlled nucleation by gassing on these quantities using the oleo-chemical model system, 1,12-dimethyl dodecanedioate/methanol. The experimental results verify that by gassing with argon, the nucleation step can be initiated at lower supersaturation compared to uncontrolled cooling crystallization with spontaneous nucleation despite the comparably small metastable zone width of the investigated model system in the range of 1–3 K. It is further demonstrated that consequently less nuclei are formed that grow to larger product crystals, which can be more efficiently separated from the mother liquor in the filtration and washing step, reducing the mother liquor leaching to the isolated product to nearly 100 ppm. Finally, it is verified that gassing crystallization with argon offers a considerable benefit for the isolation of a pure crystalline product while maintaining inert operating conditions required for recycling of oxygen-sensitive catalysts.

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“…Despite no change of pH in bulk solution, but local pH changes near the CO 2 gas-liquid interfaces may influence the nucleation on the air bubble surfaces. 40,41 The mean lysozyme crystal sizes at 56 h were 268.3 μm, 207.5 μm, 349.6 μm and 325.2 μm in the solution with bubbles of He, N 2 , O 2 and CO 2 , respectively. The mean size of crystals obtained in the solution with He and N 2 bubbles was smaller than the crystals obtained in the solution with bubbles of oxygen and carbon dioxide.…”

Section: Resultsmentioning

confidence: 99%

“…Despite no change of pH in bulk solution, but local pH changes near the CO 2 gas–liquid interfaces may influence the nucleation on the air bubble surfaces. 40,41…”

Section: Resultsmentioning

confidence: 99%