Chapter 14: Experimental Chemistry
Quantitative chemical experiments involve numbers
the concentration of an acid in .345M
Qualitative chemical experiments do not involve numbers
Silver nitrate forms a white precipitate when added to a solution
Observations and details of an experiment should be recorded in a notebook.
contains complete experiment description, the equipment, chemicals used, and occasionally diagrams
Calculations can be done via dimensional analysis or memorized equations/laws
Accuracy is the closeness between the measured value and true value
Determinate errors can affect accuracy
poor technique or incorrectly calibrated tools
Precision is the closeness of repeated measurements to each other
Indeterminate errors are a measure of precision
errors in the last digit of measurement
random errors that cannot be eliminated
Significant figures (sig figs) is the precision of a measure number
Digits are significant if:
digit is not a zero
the zero is embedded
trailing zero is in a number that has a decimal point
digits are not significant if zeros are the left of all nonzero digits
Exact numbers involve no uncertainty
five plate at the dinner table
4.184 joules in each calorie
How to obtain and write correct answers:
number with the fewest sig figs in a multiplication or division problem determines the number of sig figs in the answer
number with the fewest decimal places in addition or subtraction problems determines the number of decimal places in the answers
Two types of uncertainty: absolute and relative
Absolute uncertainty is the uncertainty of the last digit of measurement.
for 45.47mL, the last digit is uncertain and the it could be ±.01mL
Relative uncertainty of a number is the absolute uncertaintly divided by the number itself
(.01mL) / (45.47mL) = 2x10^-4
Steps of rounding:
If the digit just after the kept digits is less than 5, the remaining digits are dropped
rounding 6.23499 to three sig figs yield 6.23 because 4 is less than 5
if the digit after the kept digit is 5 or more, the last kept digit is increased by one
34.25589 to three sig figs yields 34.3
8.445000 to three sig figs yields 8.45
Graphs illustrate the relationship between two variables
X-axis is typically independent variable
experimenter selects independent variable (IV)
concentrations of standard solutions that a chemist prepares
Y-axis is typically dependent variable
dependent variable (DV) is a measured property of the IV.
the amount of light that each standard solution absotbs
constructing graphs:
label x and y axis
number the axes
plot the data points and draw lines to connect dots
Parallax errors are caused by incorrect reading techniques
Meniscus of liquid is caused by the surface tension, which causes the curvature
Weight = (gravitational constant)(mass)
Samples collected on balances should be collected in appropriate containers, not directly on the balance.
Accurate liquid measurements can be made with pipets or burets
Glassware with “TD” or “to deliver” is pouring the the volume stated
graduated cylinders
Glassware with “TC” to “to contain” will not pour the full amount in the container because a film, or excess solution, will remain
volumetric flasks
Burets are controlled by a valve called the stockpot.
should be rinsed with the solution, not distilled water, before filling
Thermometers are used for temperature measurement
Mercury is used to measure temperature
Experiments determining boiling point must be done at 1 atmosphere of pressure for accuracy
Closed-end capillary tubes can be used for melting point determination
Density = Mass / Volume
density of liquid or solid = grams of material / cubic centimeters of material
density of gasses = grams of gas / liters of gas
pycnometers can be used to determine liquid density
a solid, typically metal, is heated to a certain temperature then submerged in water, where the temperature of the water is measured
q = (mass)(specific heat)(ΔT)
Bumping is a violent burst of boiling that could splatter hot liquid
typically occurs in test tubes
occurs because burner flame superheats one portion of liquid
hot water baths, steam baths, sand bath, and electrical heating can minimize bumping
powders added to very hot liquids can cause bumping
Crushed ice bath and water is most effective to cool
Ice is particularly efficient
Heat-resistant lab glassware should be used because glass will shatter at rapid temperature change
Volumetric flasks should be used to prepare molar concentrations of specific volumes
acid should be added to water
if water is added to sulfuric acid, it will not mix because of the density, causing high heat and splattering/boiling
(Cinitial)(Vinitial) = (Cfinal)(Vfinal)
where c is concentration
v is volume
Pneumatic troughs can collect gas produced in a reaction
For Ba 2+ (aq) + SO4 2- (aq) → BaSO4 (s)
Barium solution should be added slowly with rapid stirring to precipitate sulfate ions as barium sulfate
once precipitation is complete, the mixture should be heated to form the smaller crystals to larger ones for easy filtration
Filtration is used to separate solid particles from a liquid
Folded, cone-shaped filter paper on a flask lets liquid pass through while solid is left behind
Small amounts of precipitate can be collected through centrifugation
spins at high speeds to compact solid at the bottom
Supernatant is the clear liquid remaining after centrifugation
Distillation separates two liquids with two different boiling points, one low and one high
The stationary phase of chromatography has different attractive forces for different parts of the mobile phase
Different attractive forces cause the mobile phase to move at different speeds
Rf = (distance of color spot)/ (distance of water)
pH meter or pH paper can determine pH
Litmus paper simply determines if the solution is acidic or basic
Spectrophotometer measures the amount of light that a colored solution absorbs
Absorbance of a sample is the quantity determined by the spectrophotometer
Reagent blank zeroes out the spectrophotometer to get an accurate reading
Beer’s Law: Absorbance (A) = abc
a is absorptivity
b is optical path
c is concentration
By decomposing certain compounds, gasses can be collected
KClO3 forms O2 when a catalyst is present
Gasses that do not react with water can be collected via pneumatic trough
Precipitated in double-replacement reactions or reactions of gasses with soluble substance
Ag (aq) + Cl (aq) → AgCl (s)
Ba (aq) + SO4 (aq) → BaSO4 (s)
Ni (aq) + SO2 (g) + H2O (l) → NiSO3 (s) + 2H (aq)
Can be separated by evaporation, with or without heat
Pure salt sample can only be obtained if the solution only contains the ions of that salt
Filtration can be used to separate unneeded ions
Qualitative analysis techniques determine if a sample contains a certain ion
Sequence of reactions used to analyze a sample is called qualitative analysis scheme, or qual-scheme
When a separation is by filtration, the liquid is called the filtrate.
When separation is by centrifugation, the liquid is called the supernatant
Organic compounds, typically with low molar masses
methane, butane, etc.
Ethers react to produce explosive peroxides over time
Dry picric acid is explosive
nitrogen triiodide and nitroglycerin are shock sensitive
Perchloric acid, sulfuric acid, nitric acid, and hydrogen peroxide can cause immediate skin injury
Perchloric acid with organic material causes spontaneous combustion
White phosphorus burn spontaneously in air with hazardous fumes
Active metals may react explosively with water
Li, Na, K, Rb, Cs, Ca, Ba, Sr
Substances can emit large amounts of heat in water
active metals, their solible oxides and hydroxides, and concentrated sulfuric and nitric acids
calcium oxide and phosphorus pentoxide
mixing concentrated bases with concentrated acids
Benzene, chloroform, carbon tetrachloride
Chlorinated organic compounds
Quantitative chemical experiments involve numbers
the concentration of an acid in .345M
Qualitative chemical experiments do not involve numbers
Silver nitrate forms a white precipitate when added to a solution
Observations and details of an experiment should be recorded in a notebook.
contains complete experiment description, the equipment, chemicals used, and occasionally diagrams
Calculations can be done via dimensional analysis or memorized equations/laws
Accuracy is the closeness between the measured value and true value
Determinate errors can affect accuracy
poor technique or incorrectly calibrated tools
Precision is the closeness of repeated measurements to each other
Indeterminate errors are a measure of precision
errors in the last digit of measurement
random errors that cannot be eliminated
Significant figures (sig figs) is the precision of a measure number
Digits are significant if:
digit is not a zero
the zero is embedded
trailing zero is in a number that has a decimal point
digits are not significant if zeros are the left of all nonzero digits
Exact numbers involve no uncertainty
five plate at the dinner table
4.184 joules in each calorie
How to obtain and write correct answers:
number with the fewest sig figs in a multiplication or division problem determines the number of sig figs in the answer
number with the fewest decimal places in addition or subtraction problems determines the number of decimal places in the answers
Two types of uncertainty: absolute and relative
Absolute uncertainty is the uncertainty of the last digit of measurement.
for 45.47mL, the last digit is uncertain and the it could be ±.01mL
Relative uncertainty of a number is the absolute uncertaintly divided by the number itself
(.01mL) / (45.47mL) = 2x10^-4
Steps of rounding:
If the digit just after the kept digits is less than 5, the remaining digits are dropped
rounding 6.23499 to three sig figs yield 6.23 because 4 is less than 5
if the digit after the kept digit is 5 or more, the last kept digit is increased by one
34.25589 to three sig figs yields 34.3
8.445000 to three sig figs yields 8.45
Graphs illustrate the relationship between two variables
X-axis is typically independent variable
experimenter selects independent variable (IV)
concentrations of standard solutions that a chemist prepares
Y-axis is typically dependent variable
dependent variable (DV) is a measured property of the IV.
the amount of light that each standard solution absotbs
constructing graphs:
label x and y axis
number the axes
plot the data points and draw lines to connect dots
Parallax errors are caused by incorrect reading techniques
Meniscus of liquid is caused by the surface tension, which causes the curvature
Weight = (gravitational constant)(mass)
Samples collected on balances should be collected in appropriate containers, not directly on the balance.
Accurate liquid measurements can be made with pipets or burets
Glassware with “TD” or “to deliver” is pouring the the volume stated
graduated cylinders
Glassware with “TC” to “to contain” will not pour the full amount in the container because a film, or excess solution, will remain
volumetric flasks
Burets are controlled by a valve called the stockpot.
should be rinsed with the solution, not distilled water, before filling
Thermometers are used for temperature measurement
Mercury is used to measure temperature
Experiments determining boiling point must be done at 1 atmosphere of pressure for accuracy
Closed-end capillary tubes can be used for melting point determination
Density = Mass / Volume
density of liquid or solid = grams of material / cubic centimeters of material
density of gasses = grams of gas / liters of gas
pycnometers can be used to determine liquid density
a solid, typically metal, is heated to a certain temperature then submerged in water, where the temperature of the water is measured
q = (mass)(specific heat)(ΔT)
Bumping is a violent burst of boiling that could splatter hot liquid
typically occurs in test tubes
occurs because burner flame superheats one portion of liquid
hot water baths, steam baths, sand bath, and electrical heating can minimize bumping
powders added to very hot liquids can cause bumping
Crushed ice bath and water is most effective to cool
Ice is particularly efficient
Heat-resistant lab glassware should be used because glass will shatter at rapid temperature change
Volumetric flasks should be used to prepare molar concentrations of specific volumes
acid should be added to water
if water is added to sulfuric acid, it will not mix because of the density, causing high heat and splattering/boiling
(Cinitial)(Vinitial) = (Cfinal)(Vfinal)
where c is concentration
v is volume
Pneumatic troughs can collect gas produced in a reaction
For Ba 2+ (aq) + SO4 2- (aq) → BaSO4 (s)
Barium solution should be added slowly with rapid stirring to precipitate sulfate ions as barium sulfate
once precipitation is complete, the mixture should be heated to form the smaller crystals to larger ones for easy filtration
Filtration is used to separate solid particles from a liquid
Folded, cone-shaped filter paper on a flask lets liquid pass through while solid is left behind
Small amounts of precipitate can be collected through centrifugation
spins at high speeds to compact solid at the bottom
Supernatant is the clear liquid remaining after centrifugation
Distillation separates two liquids with two different boiling points, one low and one high
The stationary phase of chromatography has different attractive forces for different parts of the mobile phase
Different attractive forces cause the mobile phase to move at different speeds
Rf = (distance of color spot)/ (distance of water)
pH meter or pH paper can determine pH
Litmus paper simply determines if the solution is acidic or basic
Spectrophotometer measures the amount of light that a colored solution absorbs
Absorbance of a sample is the quantity determined by the spectrophotometer
Reagent blank zeroes out the spectrophotometer to get an accurate reading
Beer’s Law: Absorbance (A) = abc
a is absorptivity
b is optical path
c is concentration
By decomposing certain compounds, gasses can be collected
KClO3 forms O2 when a catalyst is present
Gasses that do not react with water can be collected via pneumatic trough
Precipitated in double-replacement reactions or reactions of gasses with soluble substance
Ag (aq) + Cl (aq) → AgCl (s)
Ba (aq) + SO4 (aq) → BaSO4 (s)
Ni (aq) + SO2 (g) + H2O (l) → NiSO3 (s) + 2H (aq)
Can be separated by evaporation, with or without heat
Pure salt sample can only be obtained if the solution only contains the ions of that salt
Filtration can be used to separate unneeded ions
Qualitative analysis techniques determine if a sample contains a certain ion
Sequence of reactions used to analyze a sample is called qualitative analysis scheme, or qual-scheme
When a separation is by filtration, the liquid is called the filtrate.
When separation is by centrifugation, the liquid is called the supernatant
Organic compounds, typically with low molar masses
methane, butane, etc.
Ethers react to produce explosive peroxides over time
Dry picric acid is explosive
nitrogen triiodide and nitroglycerin are shock sensitive
Perchloric acid, sulfuric acid, nitric acid, and hydrogen peroxide can cause immediate skin injury
Perchloric acid with organic material causes spontaneous combustion
White phosphorus burn spontaneously in air with hazardous fumes
Active metals may react explosively with water
Li, Na, K, Rb, Cs, Ca, Ba, Sr
Substances can emit large amounts of heat in water
active metals, their solible oxides and hydroxides, and concentrated sulfuric and nitric acids
calcium oxide and phosphorus pentoxide
mixing concentrated bases with concentrated acids
Benzene, chloroform, carbon tetrachloride
Chlorinated organic compounds