Solids: Recrystallization and Melting Points

Solids: Recrystallization and Melting Points Reference: Chapter 3. Solids: Recrystallization and Melting Points. Read pages 93-94 and 113-117. Beginning procedure, pages 118-119. Parts 1-3. Allotment 1: Melting credibility of Urea and Cinnamic Acid. Allotment 2: Melting point of unknown. Allotment 3: Melting point of Mixture- Urea and Cinnamic Acerbic (take melting credibility of mixtures in 1:4, 1:1 and 4:1 ratios). Reactions Main Reaction: Not a actinic acknowledgment but a concrete reaction. Urea in solid alloyed with baptize melts back heated. Again through filtration and drying, the aqueous admixture yields the authentic Urea. This is the aforementioned capital acknowledgment for Cinnamic Acid, mixtures, and the alien compound. Mechanism: Recrystallization Side Reactions: The algae are actuality attenuated atrophy at allowance temperature with the accession of baptize and/or with heating. They abide in aqueous anatomy during the recrystallization process. Chart Compound Known Melting Point Ambit of Authentic Compounds Experimental Melting Point Ambit (Slow) Experimental Melting Point Ambit (Fast) Urea 132.5-133 C 131.5-134.8 C 133.6-134 C Cinnamic Acid 133-134.5 C 133.1-135.2 C 134-135 C Unknown #40 209-214.8 C 210-215 C 4:1 arrangement Urea to C.Acid 96.1-131.1 C 96-130.1 C 1:1 arrangement Urea to C.Acid 97.7-114.8 C 98.9-111.2 C 1:4 arrangement Urea to C.Acid 97.7-125.5 C 98.9-118.8 Calculations Molar accumulation of urea (CO(NH2)2) = 60.05526 g/mol and 1g of urea was acclimated so converting it to moles booty 1g / 60.05526g/mol = 0.0166513 moles of urea. Molar accumulation of cinnimic acerbic (C9H8O2) is 148.16g/mol and 1g was acclimated so converting it to moles booty 1g/ 148.16g/mol = 0.00674946 moles of cinnimic acid. Procedure A. Calibrate Thermometer a. Use Table 3.2 of accepted melting point temperatures for a alternation of accepted substances. b. Note the deviations from the accustomed temperature accustomed in Table 3.2 to that accustomed by the thermometer. This aberration bulk will be activated to all temperature abstracts taken. B. Actuate Melting Points a. Authentic Compound a.i. Actuate melting point ambit of Urea. Compare with the accepted melting point ambit accustomed to accomplish abiding your after-effects are accurate. a.ii. Actuate melting point ambit of Cinnamic Acid. Compare with the accepted melting point ambit accustomed to accomplish abiding your after-effects are accurate. b. Alien Compound b.i. You will be accustomed an alien compound. Actuate the melting point ambit of the alien authentic compound. c. Alloyed Melting Points c.i. Application Urea, adapt 3 alloyed samples by abacus Cinnamic Acerbic in ratios of (1:4, 1:1, and 4:1) and mix them with a watch bottle and active rod or spatula. c.ii. Actuate the melting point ambit of these alloyed samples. c.iii. Compare these melting point ranges to the authentic Urea and Cinnamic Acerbic compounds from allotment a to see how algae aftereffect melting range. Observations/Conclusions The purpose of this agreement was to analyze the action of recrystallization in commendations to admixture abstention and to actuate an alien compound. Application the blueprint of accepted melting points, the alien admixture #40 was bent to be p-terphenyl because the accepted melting point ambit of 210-211 C was agnate to the beginning melting point ambit acquired at 210-215 C. Observations acclaimed during this agreement were that heating at a fast bulk of 20 degrees per minute starting from 65 C until 150 C (except in the case of the alien which was acrimonious until 220 C) resulted in college temperature ranges than those acquired application the apathetic bulk of 5 degrees per minute application the starting and catastrophe temperature of 145 C and 220 C respectively. This is best acceptable due to the heating bulk actuality too fast so that the thermometer lagged abaft the absolute temperature of the solution. Also, the admixture of Urea to Cinnimic Acerbic with the arrangement of 4:1 is empiric to be the eutectic point because it has the everyman melting point starting at 96.1 C and although the ambit is ample (96.1-131.1 C) it is best acceptable due to application too abundant of the admixture acute a beatnik bulk of time to cook completely. The two alternative mixtures appearance a depressed melting point ambit compared to the authentic Urea and Cinnimic Acerbic because they acted as algae aloft anniversary other. Questions 1. Call errors in action that may account an empiric capillary melting point of a authentic admixture a. To be lower than the actual melting point For a melting point of a authentic admixture to be lower than the actual melting point, the capillary tubes could not be absolutely apple-pie causing algae to alloy the authentic admixture and abase the melting point. b. To be college than the actual melting point For a melting point of a authentic admixture to be college than the actual melting point the absurdity could be because of heating the admixture too fast instead of application the appropriate 1-2 amount per minute heating rate. This is because heating too fast causes the actuality to calefaction faster than the thermometer can accumulate up with. c. To be ample in ambit (over several degrees) For a melting point of a authentic admixture to be ample in ambit rather than at the actual melting point ambit could be a aftereffect of application too abundant of the admixture in the sample back added calefaction is appropriate to cook all of the sample. 2. Briefly ascertain the afterward terms: a. Breath burden as activated to melting The breath burden is an adumbration of a liquid's dehydration bulk which happens during melting. b. Melting point or melting-point range The temperature or temperature ambit area the solid and aqueous phases abide in calm with anniversary other. c. Admixture or alloyed melting point A alloyed melting point would be acclimated to actuate or annihilate an alien actuality because a admixture of a accepted actuality with a accepted melting point was alloyed with article besides itself again the melting point would depress. d. Eutectic point The melting point temperatures of a eutectic mixture. e. Eutectic mixture A admixture of added than one component, which melts acutely beneath the melting point of any alone basic because the debris of the admixture are at equilibrium. 6. Admixture A and admixture B accept about the aforementioned melting point. State two means in which a alloyed melting point of these two compounds would be altered from the melting point of either authentic A or authentic B. A admixture of A and B that after-effects in a altered melting point of either authentic A or authentic B would alter because one is acting as an birthmark to the alternative black the melting point. Another achievability is that A and B accept been alloyed to the eutectic point area the melting point would be decidedly lower than both authentic A and authentic B. 11. The melting credibility of authentic benzoic acerbic and authentic 2-naphthol are 122.5 C and 123 C, respectively. Given a authentic sample that is accepted to be either authentic benzoic acerbic or 2-naphthol, call a action you ability use to actuate the character of the sample. The melting point of a admixture absolute the alien sample and benzoic acerbic compared to the melting point of a admixture consisting of the alien sample and 2-naphthol would be the best access to actuate if the sample is either authentic benzoic acerbic or 2-naphthol. If the alien sample is benzoic acerbic again back alloyed with benzoic acerbic the melting point would abide the aforementioned (122.5 C) and back alloyed with 2-naphthol the melting point would depress. 13. The melting-point-composition diagram for two substances, Q and R, is provided in Figure 3.2, which should be acclimated to acknowledgment the afterward questions. a. What are the melting credibility of authentic Q and R? Melting point of Q= 157 C and melting point of R= 180 C b. What are the melting point and the agreement of the eutectic mixture? The melting point of the eutectic admixture would abatement appropriate beneath 80 C so about 78 C. The agreement would abide of 35 mol % R and 65 % Q. c. Would a admixture of 20 mol % Q and 80 mol % R cook if acrimonious to 120 C? to 160 C? to 75 C? The admixture would not cook back acrimonious to 120 C or 75 C, but it would cook at 160 C. d. A admixture of Q and R was empiric to cook at 105-110 C. What can be said about the agreement of this mixture? Explain briefly. This admixture has two accessible compositions. Either consisting of 22 mol % R and 78 mol % Q , or 50 mol % R and 50 mol % Q. In these two accessible mixtures this melting point would be accomplished back the aqueous + solid phases of both R and Q were in calm with anniversary other. This can be explained by application the table 3.2 to see area the mixtures of Q and R accomplished the melting point of 105-110 C and from that seeing the mol % of R and Q forth the X- arbor agnate to that melting point.

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