US EPA

6928780 

Journal Article 

Qualitative methods of identification of acetylsalicylic acid by differential scanning calorimetry and melting point method 

Pehlic, E; Srabovic, M; Sapcanin, A; Nuhanovic, M; Banjanin, B; Nanic, H; Redzic, S; Muric, A; Salimovic, C; Poljakovic, M; , 

2011 

Yes 

HealthMED
ISSN: 1840-2291 

DRUNPP-SARAJEVO 

SARAJEVO 

5 

6 

1782-1787 

English 

WOS:000298663500058 

https://www.scopus.com/inward/record.uri?eid=2-s2.0-84855394393&partnerID=40&md5=c0ddcb6a85e76734e56307f840f977ab
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Aim: purity determination of synthesized acetylsalicylic acid by differential scanning calorimetry and melting point method, changing parameters of synthesis.Material and methods: For laboratory synthesis and acetylsalicylic acid precrystallisation are used: salicylic acid, acetic acid anhydride, benzene, petroleum ether, ethanol 96%. Identification of synthesized aspirin is performed by instrumental methods: determination of melting point by capillary method and differential scanning calorimetry (DSC).Results: Melting point of standard acetylsalicylic acid analysed on Buchi melting point apparatus is 133.9 degrees C, and melting point of acetylsalicylic acid precrystallised in ethanol is in range of 0.5-1 degrees C, what leads to conclusion that acetylsalicylic acid precrystallised in ethanol is pure compound and ethanol is suitable solvent for purification of raw aspirin. Melting point by DSC method is 138.40 degrees C and melting point of acetylsalicylic acid precrystallised in ethanol is 139.01 degrees C. Melting point is in range of 0.5-1 degrees C what leads to conclusion that acetylsalicylic acid precrystallised in ethanol is pure compound and that ethanol is suitable solvent for precrystallisation of acetylsalicylic acid. Accuracy of performed analysis is 99.77%.Discussion: Acetylsalicylic acid or aspirin is compound which could be synthesized in less referent laboratories. Considering huge importance of aspirin in medicine and beyond, this synthesis is made for finding out differences in purity of synthesized aspirin in laboratory in relation to synthesis in pharmaceutical industry. Also, in this work there are comparison of raw aspirin properties and aspirin precrystallised in one and later in another solvent. After that, studied are conditions of crystallisation and precrystallisation, and choice is made for best suitable solvent. Synthesized acetylsalicylic acid is identified by determining of melting point by capillary method and identification of synthesized acetylsalicylic acid by differential scanning calorimetry (DSC).Conclusion: Obtained melting point of standard acetylsalicylic acid on Buchi melting point apparatus is 133.9 degrees C, and melting point of acetylsalicylic acid precrystallised in ethanol is 134.4 degrees C. Melting point by DSC method is 138.40 degrees C, and melting point of acetylsalicylic acid precrystallised in ethanol is 139.01 degrees C. Melting point is in range of 0.5-1 degrees C what leads to conclusion that acetylsalicylic acid precrystallised in ethanol is pure compound and that ethanol is suitable solvent for precrystallisation of acetylsalicylic acid.