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Laboratory 1
Instrument Accuracy and Error Propagation
Instrumentation and Measurements 1
Adam Rapke
260505848
Colin Rutherford
260528665
Jody Wong
260581325
Benjamin Burelle
260588111
Tamuno-Opubo Cookey-Gam
260529010
TABLE OF CONTENTS
-Title
- Abstract
-Table of Contents
- Introduction
- Experimental Methods
- Tabulated Results and Analysis
- Conclusions and Recommendations
- References.
INTRODUCTION
A common problem that arises in chemistry is to determine the identity of an unknown compound.
Throughout time, chemists have developed many methods to solve this issue. Chromatographic
methods, spectroscopic methods, X-ray crystallography and mass spectrometry are among some of
the modern methods that chemists employ. However, there exist simple methods that can also be
used to reach a similar answers such as using density tables and conductivity of known compounds.
As the name suggests, the density of a substance is the measure of how dense it is or, in other words,
its mass per unit volume. Density is defined by the following equation:
= m/V
Where is the density, m is the mass, and V is the volume. Its also worthwhile to mention that the SI
units for density are kg/m3. An important factor to note, as mentioned, about density is that it is not
independent to temperature. Volume of a substance increases as temperature increases due to
thermal expansion but the mass remains constant, therefore, at a higher temperature the density of a
substance is smaller. Due to this relationship, it is important to take note of the temperature of a
compound when measuring its density. Density is a physical property that is unique to every salt and
thus compounds can accurately be specified from their density measurements. All compounds have a
different solitary mass for a standard volume of 1ml. Any change in the chemical composition or
physical environment affects the density obtained. Hence, when a solution of the unknown salt is
used, we have to take into account the ratio of the volume of compound to distilled water that
comprises the solution. This is the concentration of the solution. Then a calibration curve has to be
applied since there would exist a range of values of density corresponding to the different
concentrations. The graph plotted would be that of density against concentration since
m (g) = amount in moles (mols) x m. mass (g/mol); and
Concentration (mol/L) = amount in moles (mols)/V (L)
Therefore,
(g/L) = m. mass (mols) x conc. (mol/L).
Where m is the mass, m.mass is the molar mass, conc. is its concentration, V its volume and its
density.
Therefore, a density-concentration graph would be able to give us a straight-line graph with the
gradient representing the molar mass of the compound. Here, the composition of the unknown
compound can be found by inserting the data obtained of the density and the concentration into the
different calibration curves and performing a comparison of its deviation from the straight line
graph.
A pycnometer is a device that is used to accurately measure the density of a solution. A pycnometer is
a small metal cylinder with a close-fitting metal stopper that has a capillary hole through it. It holds a
specific amount of liquid so any excess liquid is expelled through this hole. A pycnometer also has a
cylindrical component that binds the cap and the body of the pycnometer together. To measure the
density of a compound, the pycnometer is first filled with distilled water (because its density is
known) and its volume can be found with the following equation:
V = mH2O/ H2O
Where mH2O is the mass of water (obtained by subtracting the mass of the pycnometer filled with
water with the mass of the empty pycnometer) and H2O is the density of water. Since the volume of
the pycnometer is always constant, the following equation can be obtained:
mH2O/ H2O = mU/ U
U = (mU/ mH2O) H2O
Where mU is the mass of the unknown liquid (obtained by subtracting the mass of the pycnometer
filled with the liquid with the mass of the empty pycnometer) and U is the unknown density.
Once density is known, the density-concentration graph can be plotted and by performing linear
interpolation:
Y = mx + b
y= concentration (M)
m= constant, dependent on solution, independent of density molar mass)
x= density (g/ml)
b= concentration at 0.000 g/ml
The other factor involved in testing for the identity of a compound would be conductivity.
Conductivity is a measure of the number of free moving ions in a solution. The more concentrated a
solution is, the more conducting ions the solution will have and thus the solution will have a higher
conductivity. Therefore, conductivity should be in a direct linear relationship with concentration. The
following equation represents this relationship:
y = mx + b
y= conductivity (mS)
m= constant, dependent on solution, independent of concentration.
x= concentration (M)
b= conductivity at 0.000 M
Its worth noting that b should be 0 because 0.000 M means there are no conducting ions in
solution, which means there is no conductivity.
Once the composition of the compound is known, the conductivity of the unknown solution can be
compared to that of three other solutions of the same salt but of different concentrations. By linear
interpolation in a conductivity-concentration graph, the specific concentration of the unknown
solution can be found. Nevertheless, since all properties of the compound, including the identity of
the salt arent known, the unknowns concentration was compared to the concentrations of salt
solutions used in this lab. Solutions of different concentrations can be obtained through dilution of a
standard solution that was prepared. A set amount of mass of salt is first measured using an
electronic balance and used to create a 100mL solution in a volumetric flask. This would act as the
standard solution with the concentration calculated using the formula:
Conc. = m/V
Where conc. is the concentration of the solution, m is its mass and V its volume. A second solution of
the same composition but different concentration can then be obtained using dilution. A fixed
amount of the standard solution is extracted using a pipette; for higher accuracy and added to a new
and clean volumetric flask before filling up the flask with distilled water to form a new diluted
solution of volume 100mL. The theory used in dilution is that the number of moles in the extracted
volume of the standard solution is the same as new solution formed. Therefore, as a fixed amount of
volume is extracted from the standard solution, a fraction of the moles of the standard is being
transferred into the new solution. When the solution is made into a 100mL solution by adding
distilled water, the number of moles in the flask is retained but a decrease in concentration is
observed due to the increase in volume. Since,
n=MxV
Where n is the number of moles and M is the molarity/concentration. Hence, since the number of
moles remains the same in both solutions but the volume increases, concentration decreases. This
relationship can be shown by the following equation:
M1V1 = M2V2
According to this method, two new solutions with different concentrations were created for each salt
using a standard solution. The relationship between concentration and conductivity can then be
found by measuring the conductivity of these solutions. A conductivity meter is used for the accurate
measurement of conductivity. Approximately 5mL of the solution would be poured out into a smaller
cup and its conductivity is measured. Since the 5mL solution is taken to represent the conductivity of
the entire solution, extra care has to be taken to ensure that the solution was swirled thoroughly.
Also, the metal rods on the conductivity meter that takes the measurements have to be cleaned and
dried properly.
Contamination of the rod will lead to errors in the reading of conductivity while excess distilled
water left on the rods after drying may dilute the solution and would defeat the purpose of the
experiment. With the results obtained, a conductivity-concentration curve can be constructed and
linear interpolation can be carried out to find the conductivity of the unknown solution.
EXPERIMENT METHODS
I. Dilution of Solutions
4) Cap and mix, until the salt is dissolved into solution. This acts as the standard solution for the
salt.
5) Pour approximately 35mL of a standard salt solution into a small beaker or container.
6) Using a pipette, withdraw a 10mL aliquot from the beaker and place in a clean 100mL
volumetric flask. Repeat this two more times until there is 30mL of standard solution in the
flask.
7) Dilute the 30mL in volumetric flask to 100mL with RO water. This is the first dilution needed
of the standard salt solution.
8) Repeat steps 5 through 7, using the first dilution instead of the standard solution to get the
second dilution needed. Now there should be three salt solutions of different concentrations.
9) Repeat steps 1 through 8 using the other salts, getting three different concentrations of salt
solution for each of the three different salts, for a total of nine different solutions.
1) The metal rods on the conductivity meter were washed with distilled water
3) The conductivity meter was then calibrated using a solution of known conductivity.
5) Approximately 5mL of the standard solution of NaCl was poured out and its conductivity
measured. Assuming the conductivity of the extracted solution to be that of the standard
solution.
6) The metal rods were immersed into the solution and swirled.
7) The reading on the meter was taken and recorded once the value stabilized.
8) Steps 4 through 7 were repeated with the two other diluted solutions of NaCl.
9) Steps 4 through 8 were repeated with the standard and diluted solutions of the different
salts and also the unknown.
2) Fill pycnometer with water, dry (with a Kimwipe) the outside surface of pycnometer and
weigh it. Make sure to dry every spot where there may be any fluid (bottom, treads, etc.).
The presence of fluids anywhere other than inside the pycnometer will influence the weight
and produce error. Furthermore, it is key that the droplet at the tip of the pycnometer
remains somewhat constant throughout each measurement to ensure a constant volume.
Lastly, do not put the Kimwipe directly into the hole of the pycnometer because it will
absorb fluid found inside the pycnometer.
3) Fill pycnometer with standard solution of one of the three salt solutions, dry the outside of
pycnometer and weigh it.
4) Empty it, dry it and repeat the previous step for the two dilutes of that salt using the same
pycnometer.
5) Repeat steps the two previous steps for the two other salts using a different pycnometer for
every salt solution.
Pycnometers: - A (Na2SO4)
- C (NaCl)
- D (KCl)
Mass Balance: Fisher Scientific AB204 Mettle Toledo
Conductivity Meter: Ecotester EC High
Pipette: - Autoclavable and UV Resistant Fisherbrand EX
- Autoclavable Nichipet EX Nichiryo
Volumetric Flask: Pyrex 100mL
Unknown Solution: B
Temperature of Air: 22*C (assumed)
Density of Water: 0.9977735 g/mL (for 22*C)
Errors of Equipment
Data Manipulation
= ( ) ( )
( )
=
=
30
= ( )
100
= 0.00005 ( )
= 3 0.0052
= (% )2 + 02 - No Error on Molar Mass
= (% )2 + (% .. )2
= . (% )2 + (% )2
Table 2 Solution Density Data
Mass
V Error
(solution+ Error M Sol'n Density
NaCl Error (g) (Pycnometer) Error (g) (g/mL)
Pycnometer) (mL) (g) (g/mL)
(mL)
(g)
7.07107E- 7.07107E- 8.64E-06
Standard 62.282 0.00005 11.60474 11.6787 1.006373
05 05
7.07107E- 8.62E-06
Dilution 1 62.2198 0.00005 11.6165 1.001014
05
7.07107E- 8.62E-06
Dilution 2 62.2046 0.00005 11.6013 0.999704
05
Mass V
(solution+ Error M Sol'n Density Error
KCl Error (g) (Pycnometer) Error (g)
Pycnometer) (mL) (g) (g/mL) (g/mL)
(g) (mL)
7.07107E- 7.07107E-
Standard 62.3812 0.00005 11.59512 11.6394 1.003819 8.64E-06
05 05
7.07107E-
Dilution 1 62.3344 0.00005 11.5926 0.999783 8.62E-06
05
7.07107E-
Dilution 2 62.3304 0.00005 11.5886 0.999438 8.62E-06
05
Na2SO4
Mass V
(solution+ Error M Sol'n Density Error
Na2SO4 Error (g) (Pycnometer) Error (g)
Pycnometer) (mL) (g/mL) (g/mL)
(g)
(g) (mL)
7.07107E- 7.07107E-
Standard 62.5715 0.00005 11.62258 11.7112 1.007625 8.64E-06
05 05
7.07107E-
Dilution 1 62.5188 0.00005 11.6585 1.003091 8.62E-06
05
7.07107E-
Dilution 2 62.4793 0.00005 11.619 0.999692 8.6E-06
05
Sample Error:
= 0.00005 ( )
= 2 2
= 2 + 2
Note: Density Error on Water=0 and Mass Solution Error = Mass Water Error
= (% )2 + (% )2
Table 3 Solution Conductivity Data
= 0.05 ( )
The table
Graph 2: Conductivity Vs. Salt NaCL: y = 73.443x + 0.6644; R =
0.9879 above
Concentration KCL: y = 86.733x + 0.7198; R = 0.9815 clearly
Na2SO4: y = 130.6x + 0.5339; R =
16 illustrates
0.9871
14
Conductivity (mS)
the
12
10 KCl Concentration Vs.
Conductivity
8
6 Na2SO4 Concentration Vs.
4 Conductivity
2 NaCl Concentration Vs.
0 Conductivity
0 0.05 0.1 0.15 0.2
Concentration (mol/L)
relationship between conductivity and concentration of the salts that were tested. Apart from minor
deviations from the regressions, the relationships are all linear, which can be compared to true values,
which (on small scales), give a linear relationship as well. This observation is explained by analyzing
each of the salts used. Na2SO4 has three separate ions in solution, whereas both NaCl and KCl have only
two ions. Our tests indicate that Na2SO4 also has the highest conductivity in solution, and therefore one
can conclude that conductivity is proportional to the number of ions that dissociate in solution from
one mole of salt. But this does not describe the difference between the conductivities of the NaCl and
KCl solutions. Na+ is a smaller and more electronegative ion than K+, and as a result the electrons in
Na+ are held together more tightly, restricting their freedom to flow. This can also be explained through
experimental research on various solutions, which gives rise to the conclusion that K + ions are more
conductive than Na+ ions; i.e. they have a higher conductance (Chem Ed.).
Unknown Solution: During the experiment, an unknown salt solution was given, with the purpose of
finding out its approximate concentration and type of salt, from the three salts used (Na2SO4, KCl,
NaCl). Using the same testing techniques used throughout this lab the conductivity and density were
determined.
= 7.4 = 1.00568 /
Using linear interpolation it is possible to determine the concentration of the unknown solution from
the experimental conductivity.
Graph 3: Solution Density Vs. Salt
1.01 Concentration
1.008
Density (g/mL)
1.006
1.004
KCl Concentration Vs.
1.002 Solution Density
1 Na2SO4 Concentration Vs.
0.998 Solution Density
0.996 NaCl Concentration Vs.
0 0.05 0.1 0.15 0.2 Density
Concentration (mol/L)
Given the experimental density of 1.00568 g/mL, it is possible to determine the necessary
concentrations of each salt to achieve such a density in solution. The necessary concentrations would
be:
[2 4 ] = 0.055 /
[] = 0.17 /
[] > 0.19 /
These are the three options for the concentration of the unknown solution, dependent on the type of
salt. To determine which type of salt is present in the unknown solution, use linear interpolation of the
different concentrations against the known conductivity (7.4 mS) as follows:
Graph 4
REFERENCES
Chem Ed., U. o. W. "Ions in Solution." from
http://chemed.chem.wisc.edu/chempaths/GenChem-Textbook/Ions-in-Solution-
Electrolytes-598.html.
Sigma-Aldrich. "Material Safety Data Sheets." Retrieved October 29th, 2013, from
http://www.sigmaaldrich.com/catalog/AdvancedSearchPage.do.
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