WORKING WITH CHEMISTRY -- LAB SEPARATES
EXPERIMENT GROUP A Methods of Inquiry and Measurement
Experiment 1. Physical Properties: The Glass Bead Lab
Equipment
- Glass beads, assorted sizes, 36 mm diameter, larger if possible
- Rulers with varying degrees of precision; calipers
- Balances: centigram and milligram
- Graduated cylinders, available sizes, i.e., 10-mL, 100-mL
Experiment 2. Use of Volumetric Glassware: The Floating Egg Problem
Chemicals
- Sodium chloride, NaCl 500 g per group
- Eggs, varying degrees of freshness (if possible) 1 per group
Mark eggs of differing degrees of freshness with a waterproof marker, using a distinctive mark, square, circle, etc.)
Equipment
- 25-mL Mohr pipets 4 per group
- 25-mL Burets 24 per group
- 25-mL Volumetric pipets 4 per group
- 25-mL Volumetric flasks 4 per group
- 2-L plastic beakers 12 per group
- Pipet bulbs 4 per group
Experiment 3. Chemical Proportionality: Carbonate and Hydrochloric Acid
Chemicals
- Hydrochloric acid solutions: Labeled HCl A and HCl B (Acid A should be ~ 0.5 M HCl and Acid B can be any dilution of A, i.e., 2 parts A and 1 part H2O, etc.)
- Acetic acid solution: ~ 0.1 M
- Sodium carbonate Na2CO3
Equipment
- small beakers: 50 or 100-mL
- graduated cylinders: 10 and 100-mL
- spatulas
- use of centigram and milligram balances
EXPERIMENT GROUP B Elements in the Blood
Experiment 1. Spectrophotometry of Dyes
Chemicals
- Red food dye: Erythrosin B, almost saturated solution
- Blue food dye: Erioglaucine, almost saturated solution
- Yellow food dye: Tartrazine, almost saturated solution or commercial dyes bought at the grocery store
- Sodium Hydroxide6 M
- Hydrochloric Acid6 M
Equipment
- 10-mL Mohr pipets
- pipet helpers/rubber bulbs
- spectrophotometers
- plastic cuvets and caps
Experiment 2. Spectrophotometric Determination of Cu2+ Ion
Chemicals
- CuSO4 solution: 0.200 M
- Aqueous ammonia solution: 0.50 M
Equipment
- Spectrophotometer
- 5-mL and 1-mL pipets
- plastic cuvets, pipet helpers/rubber bulbs
- 10-mL, 25-mL and/or 50-mL volumetric flasks
Experiment 3. Total Serum Iron Assay
Chemicals
- Hydroxylamine hydrochloride 1.5% w/v in acetate buffer pH 4.7
Initial solution: Sodium acetate 0.1-M solution, adjust to pH 4.5 with 0.1 M acetic acid. Make up hydroxylamine solution using adjusted sodium acetate solution. Adjust final pH of hydroxylamine solution to pH 4.7 using 6 M NaOH.
- Ferrozine solution 100 mg/dL (1.0 g/L) = 1.0 g/L in H2O
- Deferoxamine solution 1 mg/dL (10 mg/L) = 10 mg deferoxamine mesylate to 1
- Ferrous ammonium sulfate 500 mg Fe/dL (5 mg Fe/L)
35.6 mg ferrous ammonium sulfate hexahydrate-acidify with 6 M H2SO4
- Ferric nitrate solution 500 mg Fe/dL (5 mg Fe/L)
36 mg iron (III) nitrate, dissolve in dilute nitric acid (5-mL 6 M HNO3/L)
EXPERIMENT GROUP C Analysis of Complex Solutions
Experiment 1. Stoichiometry of a Metal Ligand Complex
Chemicals
- Hydroxylamine Hydrochloride 1.5% w/v in acetate buffer pH 4.7
Initial: Sodium acetate 0.1 M solution, adjust to pH 4.5 with 0.1 M acetic acid. Make up Hydroxylamine solution using adjusted sodium acetate solution. Adjust final pH of Hydroxylamine solution to pH 4.7 using 6 M NaOH
- Ferrous ammonium sulfate (500 micrograms / dL) (50 mg / L)
356 mg / L Ferrous ammonium sulfate hexahydrate-acidify with 6 M H2SO4
FerroZine solution (1.0g/L)
1,10-phenanthroline solution 1.0 g / L
terpyridine solution (dissolve in ethanol) 0.500 g / L
Equipment
- 24 well plates
- plastic pipets
- 5-mL mohr pipets
- 10-mL mohr pipets
- pipet bulbs
- cuvettes and caps
- 100-mL volumetric flask
- spectrophotometers
Experiment 2. Ka of an Indicator
Chemicals
- Buffer solution: ~100-mL per student
Combine the following:
0.005 M Citrate (Sodium Citrate 1.47 g / L)
0.005 M Phosphate (Use Phosphoric acid solid 0.50 g / L )
0.005 M Ammonium (Ammonium Chloride 0.27 g / L)
Combine all solids and dilute to 1 L with H2O
Adjust pH to 1.5 using concentrated HCl and pH meter
- M HCl (standardized)
- M NaOH (standardized)
- Sodium Hydroxide (3M) for adjusting pH of buffer solution
- Buffer pH 7.0 ( for standardizing pH meters)
Bromothymol Blue 0.1 g in 16-mL 0.01 N NaOH + 234-mL H2O
Thymolphthalein 0.1 g in 16-mL 0.01 N NaOH + 234-mL H2O
Bromocresol Purple 0.1 g in 16-mL 0.01 N NaOH + 234-mL H2O
Equipment
- 24 well plates
- plastic pipets
- 5-mL mohr pipets
- 10-mL mohr pipets
- pipet bulbs
- cuvettes and caps
- 100-mL volumetric flask
- spectrophotometers
Experiment 3. Determination of Serum Albumin
Chemicals
- Succinate buffer 0.1 mol/L pH 4.0
Dissolve 11.8 g succinic acid + 2.7 g Brij 35 in 800-mL of H2O. Warm slightly to dissolve Brij 35 if necessary. Adjust pH to 4.0 with NaOH (dropwise). Dilute to 1-L volume with H2O. Store in refrigerator.
- Bromocresol green 0.58 mmol/L
Dissolve 419 mg bromocresol green in 10 mL of 0.1 M NaOH. Dissolve completely and bring to 1-L volume with H2O.
- Working solution for students: BCG
1 volume of bromocresol green solution/3 volumes of succinate buffer. Adjust pH to 4.2 ± 0.05 pH units. Label: Bromocresol green working solution, pH 4.2; store in refrigerator.
- Sodium chloride solution 9g/L for protein solutions and dilutions.
Dissolve 9g of NaCl in 900 mL of H2O. Bring to 1-L volume with H2O.
Dissolve 2.50 g of Albumin in 800 mL NaCl 9g/L solution. Dissolve completely and bring to 1-L volume with NaCl 9g/L solution. Label: Albumin 0.250 g/dL in 9g/L NaCl solution ;store in refrigerator
Equipment
- 24 well plates
- plastic pipets
- 5-mL mohr pipets
- 10-mL mohr pipets
- pipet bulbs
- cuvettes and caps
- 100-mL volumetric flask
- spectrophotometers
EXPERIMENT GROUP D Acid-Base Titration and the Global Carbon Cycle
Experiment 1. AcidBase Titration
Chemicals
- KHP: potassium hydrogen phthalate, in small jars
- Sodium Hydroxide solution: ~0.13 M in carboys. Each student will use 500 mL of this solution (three 4-L bottles at each reagent station). Prepare 5.2 grams NaOH/L.
- Phenolphthalein indicator, in dropper bottles
- HCl and H2SO4 unknowns:
Each student will need approximately 125 mL of 1 HCl and 125 mL H2SO4. Unknown range from 0.0750.110 M. Label unknown bottles with letter codes and a label instructing students to take only 125 mL of the assigned unknown.
Equipment
- 125-mL and/or 250-mL Erlenmeyer flasks (extra in boxes):34 per student
- burets:1 per student
- 25-mL volumetric pipets:1 per student
- pipet helper or bulbs: 1 per student
- 600-mL beakers: 1 per studentfor holding NaOH solutionmove from side shelves to the center reagent area of each room
Experiment 2. Analysis of an Antacid (Plus Setup for Leaf Lab)
Chemicals
- Antacid tablets: Rolaids, Tums, etc.
- M HCl
- M NaOH
- Bromothymol blue indicator, in dropper bottles
- Phenolphthalein, in dropper bottles
Equipment
- burets: 2 per team
- buret clamps: 1 per team
- hot plates
Setup for Leaf Lab
: Done by each student
Chemicals
- Leaf litter: ~ 4 leaves per student
- Sodium hydroxide 1.0 M: 40 mL per student
- M NaNO3 solution: 5 mL per student
Equipment
- plastic containers: 3 per student
- 20-mL volumetric pipets
- 50-mL plastic beakers: 3 per student
- pipet helper
Experiment 3. Tree Leaves and the Global Carbon Cycle
Chemicals
- M solutions: SrCl2, Mg(NO3)2, KNO3, Na2CO3, AgNO3, NaOH (in 250-mL dropper bottles)
- Strontium Chloride 1.0 M (label as 1.0 M, possibly use 0.5 M as substitute)
- Hydrochloric acid 1.00 M (standardized): in 4-L bottles
- Phenolphthalein: in dropper bottles
Equipment
- 24 well culture plates or spot plates
- burets: 1 per student
- 20-mL pipets
- pipet helpers
EXPERIMENT GROUP E Buffers and Life
Chemicals
- Sodium Hydroxide 0.050 M Standardized
- Hydrochloric acid 0.050 M Standardized
Equipment
- pH meters
- standardized pH solutions
Experiment 1. Stabilization of pH with Buffers
Chemicals
Dissolve 74.1 g CH3CH2CO2H (propionic acid) (75-mL) in 250-mL of H2O, add 13.2 g NaOH. Dilute to 1 L with H2O.
- Buffers: 0.020 M dilute 20.0-mL to 1.0 L
0.030 M dilute 30.0-mL to 1.0 L
0.040 M dilute 40.0-mL to 1.0 L
Experiment 2. Design of a Buffer
Chemicals
- 0.050 M NH4Cl = 2.67 g / L
- 0.050 M NH3 = 3.3-mL / L
- 0.050 M CH3COOH = 2.85-mL / L
- 0.050 M CH3COONa = 6.80 g / L
- 0.050 M Lactic acid = 5.30 g 85% solution / L
- 0.050 M Sodium lactate = 5.30 g 85% lactic acid solution
adjust pH = 7.00 with 6 M NaOH
EXPERIMENT GROUP F Measurements of Chemical Reaction Rates
Experiment 1. Hydrolysis of an Ester
Chemicals
- Standardizing Solution for pH meters, pH 7
- Potassium Hydroxide 2M = 112.22 g KOH per liter
- 0.20 M phosphate buffer, pH = 6.50
Dissolve 108.80 g potassium dihydrogen phosphate in 2 L of deionized H2O. After dissolving, insert pH probe and adjust pH to 6.50 with 2 M KOH. After adjustment, bring solution to 4-L mark with H2O.
- 0.40 M phosphate buffer, pH = 6.50
Dissolve 217.60 g potassium dihydrogen phosphate in 2 L of deionized H2O. After dissolving, insert pH probe and adjust pH to 6.50 with 2 M KOH. After adjustment, bring solution to 4-L mark with H2O.
- 4-nitrophenyl acetate (PNA) 5.0 x 104 M (aq)
Dissolve 0.362 g 4-nitrophenyl acetate in 3.5 L H2O. Bring to 4 L.
Imidazole, 25-mM concentration
Dissolve 6.80 g Imidazole in 3.5 L H2O. Bring to 4 L
2-Methylimidazole, 25-mM concentration
4-Methylimidazole, 25-mM concentration
Equipment
- spectrophotometers
- pH meters w/probes
- 100-mL volumetric flasks
- 25-mL volumetric flasks
- 5-mL mohr pipets
- pipet bulbs
- plastic cuvets
Experiment 2. Decomposition of 2-Chloro-2 methylpropane
Chemicals
- 2 % 2-chloro-2 methylpropane in isopropyl alcohol (1015 mL / group)
NaOH: ~0.040 M, adjust to pH 11.1011.30
NaOH: ~0.040 M, adjust to pH 11.7012.0
- pH standard: pH 10.0, use preparation envelopes
Equipment
- pH meters
- stir bar (from stockroom)
- stir plate
- 2- and 5-mL mohr pipets (must be dry)
- pipet helpers
- 25-mL burets
Experiment 3. Decomposition of Hydrogen Peroxide
Chemicals
- MnO2 (manganese IV dioxide), in small plastic bottles
- Hydrogen peroxide 3% (0.9 M): 4-L bottles ´
2
- Potassium iodide 1.0 M solution: 4-L bottles ´
2
Equipment
- eudiometer tubes 100mL capacity
- 125-mL side arm flasks: 1 per team
- rubber tubing: 2-3 ft. section, 1 per team
- pinch clamps: 1 per team
- stoppers for 125-mL side arm flasks - 1 per team
- 2-L beakers: 1 per team
- graduated disposable pipet tips, with tips cut off
- disposal carboy for all waste, labeled for this lab
EXPERIMENT GROUP G Electrochemical Glucose Monitoring: Construct Your Own Electrode
Experiment 1. Electrochemical Measurement
Chemicals
- Lead nitrate, 1.0 M: Pb(NO3)2 331.2 g /L
- Zinc nitrate, 1.0 M: Zn(NO3)2 297.0 g /L
- Copper nitrate, 1.0 M: Cu(NO3)26H2O 295.0 g /L
- Ferrous ammonium sulfate (saturated):
Fe(NH4)2(SO4)26H2O: approx. 300 g/L, then add 3 M sulfuric acid until acidic
- Potassium nitrate 1.0 M: KNO3 101 g/L
- Silver nitrate 0.01 M: AgNO3 1.37g/L
- Hydrochloric acid 6 Mfor cleaning from stock
Equipment
1 digital multimeter w/ alligator clips
1 chem cell plastic
1 small piece of silver wire
- electrodes: lead, copper, zinc, iron (nails)
- steel wool, for cleaning
- filter paper strips
- 600-mL beakers, to support chemical cells, if needed
Experiment 2. Construct and Use Your Own Electrode
Chemicals
- Copper sulfate electrode solution: 0.10 M
- Silver nitrate titrant solution: 0.0040 M AgNO3
- Chloride standard solution: 0.00100 M Sodium chloride NaCl
Equipment
- glass tubes, 79 mm outer diameter, 1315 cm long, polished both ends
- red rubber septum stoppers, to fit tubing end
- parafilm, small strips, to form gasket on tubing ends if needed
- thread, cotton
- silver wire, ca. 24 gauge, 34 cm length, soldered to 15 cm length of same-gauge copper wire
- copper wire, 15 cm length (Or use 15 cm length of insulated 2-strand 24 gauge bell wire, ends stripped of insulation)
- small corks, to fit end of tubing
- voltmeters
- stir plates
- spin bars
- voltmeter with kit: silver wire-copper wire combo, voltmeter, stir bar
- 25-mL burets
- buret clamps
Experiment 3. The Glucose Biosensor
Chemicals
- Hydrochloric acid 6M in 2.5 L bottles for cleanings
- Copper(II) sulfate solution, acidified 1.0 M
250 g/L Cu(SO4)25H2O, add sulfuric acid to acidify solution.
Equipment
- copper electrodes
- steel wool, for cleaning
- digital multimeters
- plugs for DC power sources in lab or battery packs (1.5 V)
EXPERIMENT GROUP H Heat Capacity: Design a Fireproof Safe
Experiment 1. The Heat Capacity of Some Solid Elements
Chemicals
- Copper shot, lead shot, zinc shot
Equipment
- cardboard squares, for calorimeters
- rubber bands (if needed, to secure the top of the thermometer through a piece of cardboard)
- hot plates
- calorimeters
- collection trays for wet metal samples
- thermometer: 10 to 110oC
Experiment 2. Thermochemistry of Reactions in Solutions
Chemicals
- Hydrogen peroxide solutions: 1%, 3% and 5% by mass H2O2
- 150-mL of solution per student, one solution per student
- 1% solution: 33.3-mL 30% H2O2 diluted to 1 L with distilled water
- 3% solution: 99.9-mL 30% H2O2 diluted to 1 L with distilled water
- 5% solution: 165-mL 30% H2O2 diluted to 1 L with distilled water
- Catalase solution, dispensed from dropper bottles
Catalase source: Sigma Chemicals, product No. C-9322
Catalase from bovine liver, 3260 units/mg solid
Concentration of catalase solution is determined by experimentation. The age of the catalase solid or solution determines how concentrated the solution must be. Start with a 0.5 g catalase / 100-mL solution concentration and test the reaction using 4 drops of catalase in 75 mL of 5% H2O2. The reaction should proceed rapidly with swirling, but with a minimum amount of foaming. Adjust the concentration up if the reaction does not come to completion in 24 minutes.
Equipment
- cardboard squares, for calorimeters
- rubber bands
- hot plates
- cotton
- top loader balances
- calorimeters
- collection trays for wet metal samples
- thermometer: 10 to 110oC
Experiment 3. The Fireproof Safe
Chemicals
- copper shot or sheet
- concrete (chunks) to fit easily in a calorimeter
These can be made as "concrete ice cubes," using concrete mix from a hardware store. Mix this in a bowl and fill an ice cube tray with the wet mixture. Spray the ice cube tray with a silicone spray before filling the tray with the concrete mix. The pieces of concrete come out easily, just like ice from a tray.
Equipment
- hot plates
- 600-mL beakers
- calorimeters with cardboard lids
- rubber bands
- corks, must fit easily in a calorimeter
- small plastic zip-loc bags, to hold concrete and cork for testing
- thermometer: 10 to 110oC
EXPERIMENT GROUP I Engineering of a Reaction
Experiment 1. Synthesis of Metal Complexes
Chemicals
- Zinc chloride: 2 g/team
- Copper(II) sulfate: 2 g/team
- Iron(II) chloride: 2 g/team
- Sodium saccharinate: 6 g/team
- Mixture of salicylic acid/sodium chloride: 10 g/team
Equipment
- 250-mL filter flask
- Büchner funnels
- pressure tubing
- 5.5 cm filter paper, Whatman No. 1
- hot plates
- ice
Experiment 2. Control of Reaction Products
Chemicals
- Cobalt(II) chloride hexahydrate: 2 g/team
- Ethylenediamine solution 2 M in water: 120.2 g/L
- Hydrogen peroxide 1-M solution: 113-mL /L
- Ethanol 95% solution
- Hydrochloric acid, concentrated
Equipment
- 250-mL filter flask
- Büchner funnels
- pressure tubing
- 5.5 cm filter paper Whatman No. 1
- hot plates
Experiment 3. Engineering a Reaction
Chemicals
- 95% ethanol
- M HCl
- Dowex resin, HCR-W2; 16-40 mesh
- M NaOH in dropper bottles
- Reaction solution: 10. g L1 methyl salicylate in 95% ethanol
Equipment
- column reactors: use Kontes Flex-Column equipment, 1 cm o.d., 30 cm length. Connections made using 3-way stopcocks and rubber tubing
- syringe barrel (100-mL), or 1-L carboy to hold reactor feed
- hot plates
EXPERIMENT GROUP J Ecological Elemental Cycles
Experiment 1. Gravimetric Analysis of Phosphorus
Chemicals
- Dropper bottles of solutions:
Silver nitrate, 0.1 M
Sodium chloride, 0.1 M
Sodium phosphate, 0.1 M
Sodium nitrate, 0.1 M
Sodium carbonate, 0.1 M
Sodium sulfate, 0.1 M
Zinc sulfate, 0.1 M
- Zinc sulfate, 0.1 M in 1-L bottles
- Sodium phosphate sand mix: various mix ratios
Use white coral sand and powdered sodium phosphate. Various mixtures of anhydrous sodium phosphate and sand containing 1575% sodium phosphate by mass. The key to the unknowns should report the phosphorus present as P2O5, because that is how students are to report their results and it should include the percent sand by mass. Students will obtain this information from the lab instructor after they complete the experiment.
Equipment
- 24 well microplates
- filter paper
- Erlenmeyer flasks
- hot plates
Experiment 2. NO2 Analysis
Chemicals
TEA (triethanolamine) analytical grade, Brij-35
(solution TEA: 20% v/v aqueous solution, containing 80 microliters of 10% Brij-35 solution)
Tubes are loaded with 40 microliters of mesh solution each
2% w/v aqueous solution of sulfanilamide in 6% v/v phosphoric acid.
Prepare 250-mL of aqueous solution containing 5 g of sulfanilamide and 15-mL of concentrated phosphoric acid)
0.14% w/w aqueous solution of NEDA
Prepare 250-mL of aqueous solution containing 0.35 g NEDA
(N-1-naphthylethylene-diamine dihydrochloride)
- Sodium nitrite solution: use freshest highest grade affordable to you
- Make dilutions from standard solution: 10 micromoles/L
Equipment
- spectrophotometers
- 13 ´
100 mm Test Tubes or cuvets for spectrophotometers
- 12 ´
75 mm I.D. plastic tubes with caps(analysis tubes)
- stainless steel screen or mesh (smaller than 16 ´
16 mesh size)
Cut to small squares and pushed to the bottom of analysis tubes with a dowel.
Experiment 3. Nitrogen and Mud
Chemicals
- Boric acid absorbant: 200 g boric acid dissolved (using heat) in 4 L of water.
Dilute to 18 L with water in a 20-L carboy. Add 0.099 g of bromocresol green sodium salt and 0.066 g of methy red sodium salt; dissolve. Bring to 20- L volume with water. Adjust pH to 4.85.0 using sodium hydroxide pellets.
- Potassium chloride solution: 2 M
- Devardas alloy: small amounts
- Magnesium oxide, MgO
- Ammonia-N standard: dissolve 0.236 g of high grade (NH4)2SO4 in water; dilute the solution to 1 L in a volumetric flask. This gives 50 mg/mL of ammonia-N. Store in refrigerator, if possible.
- Sulfuric acid: 0.00125 M, to analyze samples
Equipment
- plastic containers: 2 per student
- 50-mL plastic beakers: 2 per student
- 20-mL volumetric pipets
- burets: 1 per student