I need someone to help me with my lab report Here is all the Data and I will send my documents through student support.
Experiment 4 Refractive Index Observations
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all solutions tested were clear and colorless
temperature at time of readings = 22 C (must do a temp. correction on all readings)
Refractive Index readings =
Fraction 1 1.4340
Fraction 2 1.4645
Fraction 3 1.4856
nD @ 22 C for Exp. 3A Impure cyclohexanol = 1.4693
nD @ 22 C for Exp. 3B Cyclohexane/Toluene 50:50 mixt. = 1.4611
Experiment 5 Separations Observations
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Part A Extraction of Org Acid and Org Base
Unknown Used = Unknown 350.5.A
Appearance = grayish yellow powder
Mass of Unknown used = 3.00 g
(assume it is a 1:1:1 mixture of organic acid: organic base: neutral)
dichloromethane (DCM) = clear and colorless liquid
DCM + Unknown = clear and yellow colored
Extraction of the Organic Acid
Unknown 350.5.A dissolved in DCM + 5% NaOH – two layers in sep funnel
(top layer is aqueous layer, bottom layer is organic layer)
both layers clear, bottom layer yellow colored
total volume of 5% NaOH used for extr’n= 2 x 20 mL
Washing the Aqueous 5% NaOH Layer with fresh dichloromethane (DCM)
dichloromethane (DCM) – clear and colorless liquid
DCM + 5% NaOH sol’n – two layers both clear and colorless liquids
Extraction of the Organic Base
Remaining Unknown dissolved in DCM (yellow) + 1.5M HCl – two layers in sep funnel
(top layer is aqueous layer, bottom layer is organic layer)
both layers clear, top layer initially colorless, bottom layer yellow colored
After extraction and separation yellow color moved to upper layer
total volume of 1.5 M HCl used for extr’n= 2 x 20 mL
Washing the Aqueous 1.5 M HCl Layer with fresh DCM
dichloromethane (DCM) – clear and colorless liquid
DCM + 1.5 M HCl sol’n – two layers both clear and colorless liquids
Part B Isolation of Org Acid
volume of combined 5% NaOH extract = ~40 mL
appearance of combined 5% NaOH – slightly cloudy, colorless solution
5% NaOH + conc HCl- solution goes cloudy white
volume of conc HCl added= ~5 mL
5% NaOH + conc HCl- solution goes cloudy white with a precipitate
appearance of crude organic acid = white powder
Org. Acid Recrystallization Observations
solvent used = distilled water
volume of solvent used = 30 mL
appearance of final purified organic acid = white shiny crystals
Part C Isolation of Org. Base
volume of combined 1.5 M HCl extract = ~30 mL
appearance of combined 1.5 M HCl – slightly cloudy, yellow colored solution
1.5 M HCl + 6M NaOH- solution goes cloudy yellow
volume of 6M NaOH added= ~12 mL
1.5 M HCl + 6M NaOH- solution goes cloudy yellow with a precipitate
appearance of crude organic base = yellow powder
Org. Base Recrystallization Observations
solvent used = hexanes
volume of solvent used = 10
appearance of final purified organic base = yellow needles
Part B Isolation of Organic Acid
appearance of combined 5% NaOH – v.slightly cloudy, yellow colored solution
total volume of 5% NaOH used for extr’n= 2 x 20 mL = 40 mL
Unknown dissolved in DCM + 5% NaOH – two layers in sep funnel
(top layer is aqueous layer, bottom layer is organic layer) both layers yellow colored
Washing the Aqueous 5% NaOH layer with fresh DCM
dichloromethane (DCM) – clear and yellow liquid
DCM + 5% NaOH sol’n – two layers both clear, colored yellow
5% NaOH + conc HCl (on ice)- solution goes cloudy white,with mixing the precipitate
redissolved
Kept adding conc.HCl until precipitate remained and checked pH. pH =1 (red) using universal
indicator paper
volume of conc (12M) HCl added= ~5 mL
5% NaOH + conc HCl- solution goes cloudy white with a precipitate
appearance of crude organic acid = white powder
Recrystallized Unknown Organic Acid Yield = 0.98 g
Appearance of Unknown Acid = white needles and flakes
mp of Unknown Acid = 120-121 C
mixed mp of Unknown Acid + 2-methylbenzoic acid = 108-114 C
mixed mp of Unknown Acid + benzoic acid = 119-121C
ID of Unknown Organic Acid = benzoic acid
Part C Isolation of Organic Base
Extraction of the Organic Base
Unknown dissolved in DCM + 1.5M HCl – two layers in separatory funnel
(top layer is aqueous layer, bottom layer is organic layer)
both layers clear, bottom layer slightly colored yellow
total volume of 1.5 M HCl used for extraction= 2 x 20 mL
Washing the Aqueous 1.5 M HCl Layer with fresh DCM
dichloromethane (DCM) – clear and colorless liquid
DCM + 1.5 M HCl sol’n – two layers both clear and colored yellow
volume of combined 1.5 M HCl extract = ~30 mL
appearance of combined 1.5 M HCl – slightly cloudy, colored solution
1.5 M HCl + 6M NaOH- solution goes cloudy yellow
volume of 6M NaOH added= ~12 mL
1.5 M HCl + 6M NaOH- solution goes cloudy white with a precipitate
appearance of crude organic base = yellow powder
Recrystallized Unknown Organic Base Yield = 0.82 g
Appearance of Unknown Base = yellow needles
mp of Unknown Base = 110-112 C
mixed mp of Unknown Base + 3-nitroaniline = 110-112 C
mixed mp of Unknown Base + 4-chloroaniline = 78-85 C
ID of Unknown Organic Base = 3-nitroaniline
Part D Isolation of Neutral Compound (TA DEMO)
DCM solution + neutral hydrocarbon (naphthalene) = cloudy solution
Wash DCM layer with two 20-mL aliquots of distilled water.
Dry the DCM in a 125-mL Erlenmeyer flask by adding anhydrous magnesium sulfate
used 3 scoops of drying agent. clear colorless solution above fine precipitate on bottom of flask
Filter off the drying agent (gravity filtration) -white powder on filter paper, filtrate is clear and
colorless
Evaporate off the dichloromethane using the rotary evaporator
(solvent removed is clear and colorless) Crude off white colored naphthalene remaining in round
bottom flask
Sublimation process yields shiny translucent white flasks of naphthalene.
melting point of pure naphthalene = not determined (demo)
yield of naphthalene = not determined (demo)
Experiment 6 Functional Group Test Observations
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Appearance of pentane -clear and colorless liquid
Appearance of cyclohexene -clear and colorless liquid, strong odor
Appearance of phenyl acetylene -clear and colorless liquid
Appearance of biphenyl -clear and colorless liquid
Appearance of toluene -clear and colorless liquid
Test Observations:
Pentane
Bromine-no immediate reaction (rxn) . aft.1h-acidic gas+++
Baeyer -no rxn. purple colour stayed
Ammoniacal Silver Nitrate -no rxn.
Sulfuric Acid-no rxn.
Cyclohexene
Bromine-orange color fades, goes pale yellow immediately
Baeyer -purple colour fades gradually
Ammoniacal Silver Nitrate -no rxn.
Sulfuric Acid- goes yellow immediately
Phenylacetylene
Bromine-orange color fades, goes pale yellow immediately
Baeyer -purple colour fades gradually
Ammoniacal Silver Nitrate -whitish brown precipitate forms immediately.
Sulfuric Acid- goes dark brown immediately, gas + heat produced
Biphenyl
Bromine-stays orange, no rxn
Baeyer -stays purple, no rxn
Ammoniacal Silver Nitrate -stays clear, no reaction
Sulfuric Acid- stays clear, no rxn
Toluene
Bromine-no immed. rxn. 2 layers color lost from top layer aft 1 hour in light
Baeyer-2 layers, no rxn
Ammoniacal Silver Nitrate-2 layers, no rxn
Sulfuric Acid – clear two layers, no rxn
Part B for Experiment 6 there are the 20+ unknown Infrared Spectra. Choose any 4 to submit
for marking.
http://science.athabascau.ca/Labs/resources/350Unkns/index.php
username = auchem350 password = reaction
