Qualitative and Quantitative Chemical Analysis

Analytical Chemistry Laboratory Term 3, AY2022–2023

Laboratory Activity 1
Measurements and the Statistical Evaluation of Data (DRY LAB)

Analytical chemistry has been an indispensable tool in many fields of study, encompassing the
natural sciences, allied health sciences, engineering, and even space and astronomical sciences.
The qualitative determination of compounds in a wide array of samples has become instrumental
in the overall physical and chemical characterization of matter. Consequently, the quantitative
determination of specific components from different samples, the analytes, has paved the way for
understanding concentration effects, formulating regulatory guidelines for chemicals, and
diagnosing critical parameters in the medical field. Thus, the results of a given analytical
measurement are expected to have a high confidence level and an unwavering degree of
precision.

Errors in Chemical Analysis

Error is the difference between an experimental value, a measured response of an analyte, and
the true value, or the known or accepted value. There are many causes of errors, systematic
(determinate) or random (indeterminate), and all measurements are subject to uncertainties.
Errors can be caused by faulty calibration of an instrument, experimental errors in standardization,
random variations, and even human or experimenter errors and biases. These cause
measurements to be influenced by uncertainties giving results that are scattered.

Accuracy is the closeness of a measurement to the true or “accepted value”. The measurement
of accuracy can be done by using the following metrics:
Absolute error or Error, E = xi - µ where µ is the true value and xi is the experimentally
measured quantity.
(x i - µ )
Relative error (%), ER = ´ 100
µ
Precision is the closeness of results among one another obtained in exactly the same way. It
measures the reproducibility of measurements. The measurement of precision can be done by
using the following metrics:

Deviation d = ½xi - x½ where 𝑋" is the mean or average of measurements.

Relative deviation, =
(x i - x ) x100
x
Qualitative and Quantitative Chemical Analysis
Analytical Chemistry Laboratory Term 3, AY2022–2023

å (x i - x )
2
Standard deviation, s =
(n - 1)
s
Coefficient of Variation, CV = ´ 100 (Note: The CV is also referred to as %RSD)
x

s
Relative Standard Deviation, RSD = ´ 1000
x
This laboratory exercise will explore measurements and the statistical treatment of data. The
activity involved the measurement of mass and volume. This experiment will be done as a DRY
LAB activity. You must read the experimental procedures to understand the context of the
measurement. The data is already provided in the worksheet. Your goal is to perform the statistical
treatment of the data.

Materials and Glassware:

10-mL Volumetric Pipet Three 5--peso coins 3- 50-mL beakers
25 mL Volumetric Flask 250-mL beaker Funnel
Watch Glass Base Burette

Experimental Procedure
A. Measurement of Mass

1. Weighing by Addition (Note: Use an analytical balance)

Fill a clean 250-mL beaker with about 200 mL of distilled H2O.
Label each of the 3 clean and dry 50-mL beakers. Weigh the first beaker and
record each value correctly. Fill a clean volumetric pipet (10 mL capacity) with
distilled H2O and drain it into the first beaker. Measure the total mass of the beaker
and distilled H2O and record the value under Trial 1.
Repeat the same procedure described above and record the values under Trial 2
and Trial 3.
Always be certain that the volume of the distilled H2O is constant for all 3 trials.

2. Weighing by Difference (Note: Use an analytical balance)

Reset the analytical balance to zero. Put all three 5-peso coins into the dry watch
glass and record their value. Remove one coin and record the total mass of the
watch glass and the other two coins.
Qualitative and Quantitative Chemical Analysis
Analytical Chemistry Laboratory Term 3, AY2022–2023
Remove the second coin and record the total mass of the watch glass and the
remaining coin.
Remove the last coin and record the mass of the watch glass.

B. Measurement of Volume Capacity of Volumetric Flask

Weigh a dry 25-mL volumetric flask with a stopper and record its value. Add
enough distilled H2O until the flask is filled to the mark. Wipe the flask and cover
it with the stopper. Weigh the flask filled with distilled H2O.

Carefully empty the flask. Refill the flask with distilled water to the mark and
remove the excess water. Weigh the assembly and record the total mass under
Trial 2. Repeat this procedure and record the measurement under Trial 3.
Qualitative and Quantitative Chemical Analysis
Analytical Chemistry Laboratory Term 3, AY2022–2023

Group No. Student Number Date

Name

Exercise 1
Measurements and the Statistical Evaluation of Data
Data & Calculation Sheet

A. Measurement of Mass
1. Weighing by Addition
Details Trial 1 Trial 2 Trial 3
Volume (mL) of Distilled H2O in Each Beaker 25.00 25.00 25.00
Temperature of the Distilled H2O (°C) 23.0
Mass (g) of beaker plus Distilled H2O 53.7141 53.7102 53.7070
Mass (g) of empty beaker 29.0361 29.0358 29.0373
Mass (g) of Distilled H2O
Density of Distilled Water
Theoretical Value of the Density of Distilled H2O 0.997542
Average Density of Distilled Water
Absolute Error
Relative Error (%)

Show sample calculation:

Qualitative and Quantitative Chemical Analysis
Analytical Chemistry Laboratory Term 3, AY2022–2023
2. Weighing by Difference
Details Trial 1 Details Trial 2 Details Trial 3
Mass (g) of Watch Mass (g) of Mass (g) of
Glass plus 3 Coins 45.5567 Watch Glass 37.7254 Watch Glass 29.9695
with 2 Coins with 1 Coin
Mass (g) of Watch Mass (g) of Mass (g) of
Glass plus 2 Coins 37.7254 Watch Glass 29.9695 Watch Glass 22.2340
plus 1 Coin
Mass (g) of Coin Mass (g) of Mass (g) of Coin
Removed Coin Removed Removed
Average Mass of
Coin
Deviation Deviation Deviation
Standard Deviation
Coefficient of Variation
(%RSD)

Show sample calculation:

Qualitative and Quantitative Chemical Analysis
Analytical Chemistry Laboratory Term 3, AY2022–2023
B. Measurement of Volume Capacity of Volumetric Flask

Temperature of the Distilled H2O (°C) 23.0

Theoretical Value of the Density of distilled H2O 0.997542
Trial 1 Trial 2 Trial 3
Mass (g) of Volumetric Flask + Distilled H2O 43.8833 43.8836 43.8831
Mass (g) of dry Volumetric Flask 19.21670 19.2670 19.2666
Mass (g) of Distilled H2O
Volume (mL) of Distilled H2O in Volumetric Flask
Average Volume (mL) of Distilled H2O
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

Show sample calculation:

Qualitative and Quantitative Chemical Analysis
Analytical Chemistry Laboratory Term 3, AY2022–2023
PROBLEMS AND QUESTIONS
1. Explain the difference between systematic and random error.

2. State whether the following errors are random or systematic:

a) A 25-mL transfer pipet consistently delivers 25.031 ± 0.009mL.

b) When taking your mass measurements using a (weighing) scale, different readings
were obtained when you slightly changed your position on the scale each time.
c) A 10-mL burette consistently delivers 1.98 ± 0.01 mL when drained from exactly 0
to exactly 2 mL and consistently delivers 2.03 mL ± 0.02 mL when drained from 2 to
4 mL.
d) A 10-mL burette delivered 1.983 9 g of water when drained from exactly 0.00 to 2.00
mL. The next time I delivered water from the 0.00 to the 2.00 mL mark, the delivered
mass was 1.990 0 g.
e) Measuring your height is affected by minor posture changes.

3. What does the standard deviation of a set of data measure? What is its significance?

4. Spreadsheets are useful for computing a data set's mean and standard deviation. The
spreadsheet here is a template for the following exercise/question (see next page).

Part 1:

a) Reproduce the template on your spreadsheet. Cells B4 to B8 contain the data (x

values) whose mean and standard deviation you must compute.
b) Write a formula in cell B9 to compute the sum of numbers in B4 to B8.
c) Write a formula in cell B10 to compute the mean value.
d) Write a formula in cell C4 to compute (x – mean), where x is in cell B4 and the mean
is in cell B10. Use Fill Down to compute values in cells C5 to C8.
e) Write a formula in cell D4 to compute the square of the value in cell C4. Use Fill
Down to compute values in cells D5 to D8.
f) Write a formula in cell D9 to compute the sum of the numbers in cells D4 to D8.
g) Write a formula in cell B11 to compute the standard deviation.
h) Use cells B13 to B18 to document your formulas.
Qualitative and Quantitative Chemical Analysis
Analytical Chemistry Laboratory Term 3, AY2022–2023
Part 2:

i) Simplify life by using formulas built into the spreadsheet. In cell B21 type
“=SUM(B4:B8)”, which means find the sum of numbers in cells B4 to B8. Cell B21
should display the same number as cell B9. You will not generally know what
functions are available and how to write them.
j) Select cell B22. When you type “=AVERAGE(B4:B8)” in cell B22, its value should
be the same as B10.
k) For cell B23, find the standard deviation function (“=STDEV(B4:B8)”) and check
that the value agrees with cell B11.
l) Take a screenshot of your resulting spreadsheet and attached it in your report.

5. State the importance of basic statistical data treatment in your future career or chosen
field of study.