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

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