Table of Reagents Reagents Molecular Weight Density MP BP Lab
Transcription
Table of Reagents Reagents Molecular Weight Density MP BP Lab
Table of Reagents Reagents Molecular Density MP Weight BP Lab Hazard Health Hazard corrosive to skin combustible at high and eyes, 172.21 1.08g/c Sulfanilamide 165.5C Decomposes temp, never mix inhalation can g/mol m^3 with water, cause respiratory tract irritation. skin and eye irritant, 46.07g/mol carcinogenic, 190 proof ethyl (water 0.789g/ -114.1C 79.58C Flammable mutagenic, alcohol excluded, cm^3 teratogenic, 200proof) developmental toxicity 135.16 1.22 May combust at skin and eye Acetanilide 114.3C 304C g/mol g/cm^3 high temperatures irritant Produces carbon Eye and skin dioxide and 2-Nitrobenzoic 167.12 1.49 irritation, 149.5C 340.7C nitrogen oxides acid g/mol g/cm^3 respiratory under fire irritant conditions Produces carbon Causes serious 2dioxide and eye irritation, 137.14 1.412 Aminobenzoic 150.0C 200C nitrogen oxides skin irritation, g/mol g/cm^3 acid under fire harmful to conditions respiratory tract Experimental Procedure3B 1) 2) 3) 4) 5) 6) 7) 8) 9) Weight 0.10g impure sulfanilamide into craig tube Add 2-3mL 95% ethyl alcohol to small test tube w/ boiling stone Heat small test tube w/solvent on hotplate to light boil. Add just enough hot solvent from small test tube to craig tube to cover solid. Heat craig tube to boil, add drops hot solvent, and stir. After 15 seconds if solid isn't dissolved fully, add drops hot solvent, and stir. Repeat step 6 until solid fully dissolves. Remove craig tube from hotplate, insert inner plug, and place in 10mL Erlenmeyer flask. Wait until craig tube cools to room temp and crystallization is complete. (scratch glass if needed) 10) Ice-bath the craig tube. 11) Place craigtube w/safety wire in centrifuge tube in centrifuge, balance, run for five minutes. 12) Weigh watchglass. 13) Scrape crystals out onto watchglass 14) Air dry five to ten minutes, weigh watchglass + crystals 15) Calculate % recovery 16) Determine melting point of pure sulfanilamide and 2-Nitrobenzoic acid/2-Aminobenzoic acid mix. Results Impure Sulfanilamide 0.101g Watchglass 24.816g Crystals (Pure Sulfanilamide) + Watchglass 24.882g Crystal (Pure Sulfanilamide) 0.066g Impure Sulfanilamide 0.101g Percent Recovery (0.066g / 0.101g)x100% = 65.34% Pure Sulfanilamide HPLC Results STD Benzoic Acid Lit: 124.3C, Machine: 122.6 – 122.9C correction = +1.55C *Impure Sulfanilamide starting material 141.95 – 153.75C after correction STD Benzoic Acid Lit: 124.3C, Machine: 122.6 – 122.9C correction = +1.55C 2-Nitrobenzoic acid/2-Aminobenzoic 85/15 mix 119.0 – 128.0C after correction Pure Sulfanilamide 166.75 – 167.55C after correction