Chem 126.
1 (Analytical Chemistry II Lab)
Midyear, Academic Year 2021-2022
Department of Chemistry, College of Arts and Sciences
University of the Philippines Visayas, Miag-ao, Iloilo
Assignment 1
Introduction to Instrumental Methods of Analysis
Assignment Report for Chem 126.1 (Analytical Chemistry II Lab)
submitted by
ADANIEL, Bryant, 2020-08801
BELDIA, Alexi Andrea, 2019-11637
Instructor:
Arnold GAJE, MSc
Assistant Professor
Department of Chemistry, College of Arts and Sciences
University of the Philippines Visayas, Miag-ao, Iloilo
August 2022
The Analytical Process
1. Briefly describe the purpose and importance of the following procedures in the
analytical process:
a. Sample preparation
After collection of a sample, preservation and preparation are the
succeeding steps in the sampling plan of analytical processes. Sample
preparation in particular is necessary to ensure that the sample is
representative of its source - that is, its conditions are as close as possible to
the source material since the information generated from the analysis is traced
back to the source. Such is done to minimize possible contamination
(especially during transport, when samples are taken outside of the laboratory)
which would consequently reduce errors, thereby providing more accurate and
precise measurements.
b. Replicate measurements
Typically for laboratory experiments, it is a standard procedure to have
replicate samples and the process shall be performed in the same manner, as in
the same analytical procedure, at the same time. Measurements are then
averaged by taking the mean and subjecting it to other statistical parameters.
By doing so increases the statistical confidence of the results as well as
provide a more precise and reliable data as opposed to only a single data point.
2. What is the general principle/idea behind the separation of chemical species? Answer
this question by discussing:
a. Why is it possible to separate chemical substances?
Substances have their own innate and unique chemical and physical
properties, which can be exploited through various methods that allow for
analytical separation. It isolates the substance of interest (analyte) which
enables the analyst to ensure that chemical analysis is done properly with the
target compound.
b. How does the other species in the sample affect the determination (qualitative
and quantitative) of the analyte?
The presence of other species in the samples could interfere – hence,
labelled as interference – with the analysis and may hinder the procedures, and
there is a higher possibility of the contribution of errors to the measured values
which means a significant decrease in the reliability and accuracy of the
results.
3. What are the important considerations in reporting analytical results?
For any analytical procedures, it is a must to write a report on the experimental
observations and measurements to provide conclusive results that are considered
valid. As such, any person involved with these processes must have integrity and
report observations and measurements as is and with honesty, without manipulating
the data to ensure that all written are true. Additionally, the report must also be
complete – calculations, tables, graphs, figures, and documentation, among others,
must be present and labelled accordingly. From my perspective, reports should also
aim to be easily understood, which means using simple language and only resorting to
jargon or technical terms when necessary to make sure the readers are able to
comprehend without much confusion. Finally, reports should also aim to be clear,
concise, and organized: it should be done in such a way that everything that needs to
be elaborated are present, explained properly with clarity without being redundant,
and presented systematically, following a proper scientific report.
Classification of Analytical Method: Classical vs Instrumental Methods
4. Briefly explain the main reason/s why instrumental methods have become the
preferred method of chemical analysis.
The classical method is an analytical method in which separation is
accomplished through precipitation, extraction, or distillation employing simple
materials and instruments. Furthermore, the analyte is determined in this method using
human senses, simple laboratory devices, titrimetric or gravimetric procedures. The
instrumental technique, on the other hand, involves tools and instruments to separate
and quantify individual components of a substance. It determines the analyte using
precise measurements of analytical responses as well as calibration and standardization
procedures. The latter has become the preferred method of chemical analysis because
instruments have become more accurate and precise upon quantifying information and
because it is a less expensive procedure.
Process of Instrumental Measurement
5. Concisely define and differentiate the following concepts
a. analytical information, analytical signal, and analytical results
Analytical information is a collection of specific physical or chemical
qualities that represent data to be studied in a chemical analysis.
All signals that are generated by analytical techniques and employed in
analytical chemistry in any way are referred to as analytical signals. Data banks,
test samples, and reference samples can all provide analytical signals, as well as
the interactions between the analyte species.
An analytical result is the outcome of a chemical analysis through
sampling, field sample preparation, laboratory processing, laboratory testing,
computations, and results presentation.
b. transducer, sensor, and detector
Transducers, sensors, and detectors are electrical, opto-electrical, or
electronic devices that are made of specialized electronics or otherwise sensitive
materials that detect the presence of a specific entity or function. Transducers
are referred to as energy converters. It is a device that converts one type of
energy into another, such as converting a non-electrical signal into an electrical
signal or electricity into electromagnetic waves. Specifically, it is a device that
converts non-electrical domain information into electrical domain signals.
While a sensor is a device that detects and converts physical changes in the
environment, such as temperature and light, into a readable signal. Furthermore,
capable of monitoring a specific chemical species continuously and reversibly.
On the other hand, detectors are mechanical, electrical, or chemical devices that
identifies, records, or indicates a single variable change, it converts incident
photons into quantifiable signals. All detectors can be assessed based on their
fundamental features, which include spectrum response, linearity, quantum
efficiency, dynamic range, response time, and noise susceptibility. Based on
how well they perform in certain areas, certain detectors are better suited to
specific applications.
c. nonelectrical and electrical data domains
Electrical and non-electrical data domains are the two broad categories
of data domains. Non-electrical domains are where the measurement process
begins and concludes. These data domains contain the physical and chemical
information relevant to a specific experiment. These properties include length,
density, chemical composition, and light intensity. While electrical domains are
ways of encoding information as electrical values, they are further classified
into analog domains, temporal domains, and digital domains.
d. analog domain, time domain, and digital domain
Analog domains are information encoded as the magnitude of current,
voltage, and charge. It is a continuous variable.
Digital domain is a discrete variable where data is encoded in a two-
level scheme, such as on/off and hi/Lo.
Time domain, which is a continuous variable, are information stored as
the time relationship of signal, such as frequency, pulse width, and phase.
e. readout devices and computers
Readout devices are a transducer that converts an electrical signal into
an information that is easily recognizable and readable for humans. Some
examples include dials, digital readouts, oscilloscopes, and strip chart recorders.
While computers are instruments that incorporate one or more simple to
complex electrical devices.
f. transducer transfer function
An expression of the relationship between the input and output of a
sensor or transducer. This could take a variety of different forms, including an
equation, a graph representing the response or a validated calibration curve.
6. List four input transducers and very briefly describe how they are used.
Input transducers include solar cells, piezoelectric devices, and thermocouples,
and pyrometer.
a. Solar cells - through the photovoltaic effect, solar cells and other
photovoltaic devices transform light energy or absorbed photons directly
into electrical energy.
b. Piezoelectric devices - electrical charge is directly converted from
physical strain using piezoelectric sensors
c. Thermocouple - it is a device that measures temperature, which converts
heat differentials into voltage differentials
d. Pyrometer - it is a device that uses the thermal radiation generated by a
heated item to measure temperatures
7. In modern instruments, an analog signal is usually converted to a digital signal.
Briefly, cite important reasons why it is more advantageous to encode measurement
information in digital-domain?
Digitalizing information is the standard practice in analytical chemistry (and other
branches of chemistry as well) because it takes advantage of modern technology to
make the process easier for the chemist. Additionally, as opposed to analog signals
whose outputs are obtained manually, signals in the digital domain are encoded
directly to a software which is subsequently forwarded to a digital display, which
makes it more reliable and efficient in terms of transmission and since there is less
room for error as it is displayed concisely for the chemist to record and interpret.
8. Give a concise definition of a computer and based on this definition infer why
computers have become an integral part of modern analytical instruments.
A computer is an instrument that provides such vast flexibility and
sophistication in the execution and control of experiments. Computers are being used
more and more in analytical work as it allows for the qualification and classification of
background information, utilizing a variety of chemometric techniques including the
use of analytical intelligence through the recognition of patterns or expert control of
chemical analysis systems, which are frequently used by instruments made for routine
analysis. In a nutshell, computers have become an integral part of modern analytical
instruments because of the dependability, accessibility, and proficiency it provides
upon doing an experiment.
Case Study 1: Recently, our research group in the Department have developed a simple,
quick and portable analytical method for the detection of Pb 2+ (a toxic heavy metal) in
aqueous solutions. It is based on the fluorescent properties of the nanomaterials known as
carbon quantum dots (CQD). These nanomaterials are highly soluble in water and in aqueous
solutions, they emit blue-green light when irradiated with an ultraviolet light (from a UV
lamp or laser diode). In the presence of Pb2+, the intensity of the light emitted by CQD
decreases, and the decrease of intensity of fluorescence is related to the concentration of Pb2+.
In this method, the intensity of emitted light is measured by taking a photograph of the
fluorescent test sample using a smartphone camera (Iphone 8) and then determining using an
image analysis software the value of image pixel variables that are related to the intensity of
the blue-green light emitted by the sample.
(For more info about this research and innovation project see:
https://www.upv.edu.ph/index.php/news/upv-s-innovation-project-is-a-finalist-in-the-bpi-
dost-innovation-awards-
2022?fbclid=IwAR2ZlJHDFkv5Vdt2NXTlUXVNaLGgPXeU2vdA9_N7Tn8ybS3Iw0IJ_uU
bZMo,
9. In the Case Study 1 above, identify the
a. Analyte and the desired information
In this case study, the analyte is Lead (Pb2+) and its presence in
aqueous solution is determined through a decrease intensity of the blue-
green light emitted by the CQD. This information is crucial since Pb2+ is a
toxic heavy metal which poses risks to human health.
b. Stimulus
The stimulus in this case study, which can be redefined as the energy
source capable of evoking a response for the onset of the chemical
reaction, is the UV light from a UV lamp or a laser diode.
c. Analytical signal
As previously mentioned, carbon quantum dots (CQD) emit blue-green
light when irradiated with UV light. The intensity of the light CQDs emit
serve as the analytical signal in the case study.
d. The transducer
A smartphone camera contains a photodiode which translates as the
transducer in the case study. A photodiode can convert the emitted blue-
green light into an electric signal; the image pixels that are subjected for
analysis in determining the intensity are outputs of the photodiode.
10. Perform an internet or library research on how a digital camera (such as in
smartphone) works, particularly, how it can record an image in a pixel. Using the
concepts and principles that you’ve learned, concisely discuss how the smartphone
camera is used in the instrumental method described in Case Study 1. Specifically,
describe how it can be used to obtain the desired chemical information about the
analyte.
A single picture is composed of millions of pixels, and these are basically dots
that contain data. Digital cameras are able to capture images because they possess
lenses, which focuses light passing through it onto a sensor: either a charge coupled
device (CCD) or a complementary metal oxide semiconductor (CMOS). Both of these
sensors have photodiodes that can convert the light (photon) that bounces off the
subject to an electrical signal (electron) which is then encoded into binary, enabling it
to generate an image in a digital format. As aforementioned, digital camera (from an
iPhone 8) is utilized in the study to take an image of the sample as it emits a blue-
green light. The image’s pixels are subjected to analysis via a software, and since the
light intensity of CQDs is affected by the concentration of lead in the sample, it is
indicative of the presence of lead and therefore a viable method of detection.
11. Draw block diagrams similar with those in Figure 3.5 for the instrumental method
presented in Case Study 1.
a. Present schematic representation of the experimental set up used in the
method.
b. Using given information in Case Study 1, your knowledge of instrumental
measurement and the results in Item 10, draw a diagram showing the flow of
information during the measurement process, and the rules defining the data-
domain transformations.
c. Using the results in 11a and 11b, concisely but accurately describe step by step
how the analytical signal was obtained and processed to determine the desired
chemical information.
Obtaining the analytical signal in this case study, which was previously
defined as the intensity of light the CQDs emitted once the sample is
illuminated with UV light, was done through capturing a picture using a
digital (smartphone) camera. At this juncture, the sample is fluorescent and
emits a blue-green light. Following this, the processing phase is done by
subjecting the picture to an imaging software that is able to generate the
needed information through the value of pixel variables, which is related to the
measurement of the intensity of the light, allowing the analyst to detect and
confirm the presence of Pb2+.
Credits/Contribution of Authors: The items were divided as such: AAB worked on
items 1, 2, 3, 7, 9, 10, and 11 while BA worked on items 4, 5, 6, and 8 and 9. AAB
finalized and submitted the report.
