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Analyzing, Preparation and Methods Sampling in Analytical Chemistry

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International Journal of Academic and Applied Research (IJAAR)
ISSN: 2643-9603
Vol. 6 Issue 11, November - 2022, Pages: 1-6

Analyzing, Preparation and Methods Sampling in Analytical

Chemistry
Irfan Ananda Ismail*1, Indang Dewata2, Desy Kurniawati2, Mawardi Mawardi2, Munadia Insani2, Vika Aumi2,
Agnes Febriyanti3,
1
Master Candidate in Chemistry Education, FMIPA Universitas Negeri Padang, West Sumatera, Indonesia
2
Chemistry Dept, FMIPA Universitas Negeri Padang, West Sumatera, Indonesia
3
Institut Kesehatan Mitra Bunda Batam, Bachelor of Pharmacy, Batam, Indonesia
[email protected]

Abstract: In any such procedure, the specific analytical method selected depends on how much sample is available and how much
analyte is present. This article used the Systematic Literature Review (SLR) method to review eleven articles published from 2000 to
2021 and focused on Analyzing, Preparation, Methods, Sampling then for next we call it Fundamental In Analytical Chemistry using
various source. The articles are systematically obtained from the online article database ERIC, Scopus, and SINTA. The purpose of
a review is to give information to readers about the definition of Analyzing, Preparation, Methods, Sampling, the important things
to know it in analytical chemistry, and how to implement it in research especially in analytica chemistry. The review results showed
that these topic is important to know for college student so they know what they gonna do in Analytical Chemistry. Also, it referred
to the use of various media We discuss here a general classification of the types of determinations based on these factors. after
selecting the particular method to be used, a representative sample must be acquired. In the sampling process, we make every effort
to select a small amount of material that accurately represents the bulk of the material being analyzed. We use statistical methods
to aid in the selection of a representative sample. Once the analytical sample has been acquired, it must be processed in a dependable
manner that maintains sample integrity without losing sample or introducing contaminants. Many laboratories use the automated
sample handling methods discussed here because they are reliable and cost effective. Because analytical methods are not absolute,
results must be compared with those obtained on standard materials of accurately known composition. Some methods require direct
comparison with standards while others involve an indirect calibration procedure. Mastery of these fundamental knowledge in
analytical chemistry will serve you well in chemistry courses and in related scientific fields. In addition, your efforts will be rewarded
with the consider- able satisfaction of having completed an analysis with high standards of good analytical practice and with levels
of accuracy and precision consistent with the limitations of the technique. Much of our discussion focuses on Analyzing, Preparation
and Methods Sampling in Analytical Chemistry. We conclude this chapter with a literature that reviewed from research that has
been conducted to summarize the fundamental aspects of sample preparation and anticipate future developments and research needs
Keywords— Analyzing, Preparation, Methods, Sampling, Fundamental Analytic
1. INTRODUCTION understanding of the basic principles that govern the transfer
of analytical parameters to multiple time systems. The purpose
Sample preparation and analysis methods often involve an
of this concept is to summarize the main aspects of sample
extraction process that results in the isolation and enrichment
preparation and to anticipate future developments and research
of components of interest from the sample matrix. Extraction
needs.
can vary in the degree of selection, speed and quality and
depends not only on the methods and conditions used, but also We calculate the results of the two-factor analysis by two
on the geometrical structure of the extraction time. The measurements. One is the size or volume of the analyzed
introduction of non-traditional extraction technologies has led sample. A secondary measurement is one in which some
to increased interest in sample preparation research (Zgorelec quantity corresponds to an analytical quantity in the sample,
et al. 2019). These technologies address the need to reduce such as mass, volume, heat, or electric charge. This second
solvents, automation and miniaturization and ultimately lead measurement completes the analysis, and we organize the
to site and in vivo implementation. These mining methods are analysis process according to the nature of this final
generally easy to use, but present the best challenges. More measurement. In the gravimetric method, we determine the
important knowledge is required by the surveyor not only of mass of the analyte or its chemical composition. In the
the measurement conditions, but, more importantly, of the volumetric method, we measure the volume of the solution
mass transfer process and the extraction system (Li et al. 2020). containing enough reagent to react with the assay (Acharya et
Optimizing this extraction process results in a more detailed al. 2013). In electronics, we measure electrical properties such
analysis. The proper design of the device and the extraction as power, current, resistance, and electric current. In
process makes its implementation effective on site, integration spectroscopic methods, we analyze the relationship between
and sampling and separation / quantity, automation, or both electromagnetic radiation and analyte atoms or molecules or
(Skoog, D. A., West, D. M., Holler, F. J., & Crouch 2004). Key the emission of radiation through analysis (Etikan and Bala
to rational selection, optimization and design is an 2017). Finally, in a different way, we measure quantities such

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International Journal of Academic and Applied Research (IJAAR)
ISSN: 2643-9603
Vol. 6 Issue 11, November - 2022, Pages: 1-6

as mass-to-charge of ions by mass spectrometry, the rate of and used to diagnose and treat illnesses(Pawliszyn 2003).
radioactivity, the temperature of the reaction, the rate of the Quantities of hydrocarbons, nitrogen oxides, and carbon
reaction, the thermal conductivity of the sample, optical monoxide present in automobile exhaust gases are measured
function and refraction. index to deter- mine the effectiveness of emission-control devices.
Quantitative measurements of ionized calcium in blood serum
2. METHOD
help diagnose parathyroid disease in humans(Luis and
The method used in this article is systematic literature Moncayo n.d.). The quantitative determination of nitrogen in
review (SLR). Xiao & Watson (2019) explained that foods reflects their protein content and therefore their
Systematic Literature Review (SLR) is a literature review nutritional value. Analysis of steel during its production
process that follows standard rules to identify and develop allows to change the combination of elements such as carbon,
important research topics and determine what is known about nickel and chromium to obtain the required strength, hardness,
the subject being studied. The articles analyzed in this corrosion resistance and ductility.(Neolaka et al. 2018). The
literature review were obtained by searching the online mercaptan content of natural gas is continuously analyzed to
databases ERIC, Scopus and SINTA (Indonesian Research ensure that the gas has an unpleasant smell to warn of
database). Literature and analysis were collected from dangerous leaks (Fumes et al. 2015). Farmers adjust
September 24 to September 28, 2022. In this study, the fertilization and irrigation systems to meet the changing needs
keywords used are " Analyzing, Preparation and Methods of plants during the growing season, assessing these needs
Sampling in Analytical Chemistry After searching for a through plant and soil analysis.
keyword, the researcher reads the title of the article to select
3.3 Sampling
articles that meet the following inclusion criteria: (1) relate to
the defintion; (2) the year of publication articles; (3) articles A chemical analysis is most often performed on only a
from reputable journals that indexed internationally by Scopus small fraction of the material of interest, for example a few
or indexed nationally by SINTA. Based on the article search milliliters of water from a polluted lake. The composition of
results, there were 49 titles suitable with inclusion criteria. By this fraction must reflect as closely as possible the average
then, the abstracts of those 49 articles were analyzed. The composition of the bulk of the material if the results are to be
result of the abstract analysis was 25 articles following the meaningful. This process of obtaining representative samples
fundamental on analytic chemistry. Meanwhile, the other 24 is called sampling (Mitra and Brukh 2003). Often times,
articles were inappropriate because three articles were out of sampling is the most difficult step in the entire research process
topic and specific mention to object. Furthermore, all content and the most limiting step in the process. This statement is
especially true if the object to be analyzed is a large
of 25 articles was read. Finally, these 25 articles provided
inhomogeneous liquid, such as a pond, or an inhomogeneous
suitable information on what will be discussed. solid, such as metal, soil, or animal parts. the body. Sampling
3. RESULTS AND DISCUSSION for chemical analysis requires the use of statistics because
large-scale conclusions must be drawn from the analysis of
3.1 DEEP DIVE WITH FUNDAMENTAL small laboratory samples.(Horwitz 1990). This is the same
The purpose of a research study is to obtain information process that we dis- cussed in Chapters 6 and 7 for examining
about something or an object. Matter can be solid, liquid, gas a finite number of items drawn from a population. From the
observation of the sample, we use statistics, such as the mean
or organic matter. The information to be received may vary. It
and standard deviation, to draw conclusions about the
can be a chemical or physical composition, a structural or
population
surface structure, or a protein sequence in a gene (Horwitz
1990). Despite the large arsenal of research methods available, The first step is sampling, where the sample is obtained
it is not possible to find all the information, even with a small from the object to be analyzed. This is collected such that it
number of samples. For the most part, the current state of the represents the original object. Sampling is done with
equipment has not developed to the extent that we can bring variability within the object in mind. For example, while
the equipment and materials and get all the necessary collecting samples for determination of Ca2+ in a lake, it
information (Situmorang 2010). Although there is great should be kept in mind that its concentrations can vary
interest in these non-invasive devices, many tests are still depending on the location, the depth, and the time of
carried out by taking a portion (or part) of the object being year(Fumes et al. 2015). The next step is to save the sample.
This is an important step, since there is often a delay between
studied (called a sample). and verify it in the lab (or on the
sample collection and analysis. Sample preservation ensures
website). . Some common steps in this process are shown in that the sample retains its physical and chemical characteristics
Figure 1.1 (Mitra and Brukh 2003). so that the analysis represents the actual substance being
3.2 Sample Preparation studied..
Analytical chemistry is applied throughout industry,
medicine, and all the sciences. To illustrate, consider a few
examples. The concentrations of oxygen and of carbon
dioxide are determined in millions of blood samples every day

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International Journal of Academic and Applied Research (IJAAR)
ISSN: 2643-9603
Vol. 6 Issue 11, November - 2022, Pages: 1-6

exploratory research requires more intensive sample

preparation than primary resource research.

Figure 1.1. Steps in a measurement process

The sample preparation step in an analytical process
typically consists of an extraction procedure that results in the
isolation and enrichment of components of interest from a
sample matrix(Kratochvil, Wallace, and Taylor 1984).
Extraction can vary in degree of selectivity, speed, and
convenience and depends not only on the approach and Figure 1.2. Possible steps within sample preparation
conditions used but on the geometric configurations of the 3.4 Analysis method in analytical chemistry
extraction phase. The introduction of non-traditional extraction
techniques has led to increased interest in sample preparation Once the sample preparation is complete, the analysis is
research. These technologies address the need for solvent carried out by an instrument of choice. A variety of instruments
reduction, automation and miniaturization and ultimately lead are used for different types of analysis(Jungnickel and Forbes
to in vivo implementation at site and location(Pawliszyn n.d.), depending on the information to be acquired: for
1995). These mining methods are generally easy to use, but example, chromatography for organic analysis, atomic
present the best challenges. More important knowledge is spectroscopy for metal analysis, capillary electrophoresis for
required by the analytical chemist not only of equilibrium DNA sequencing, and electron microscopy for small
conditions but, more importantly, of mass transfer processes in structures(De La Guardia 1999). Common test tools and their
the extraction process. Optimizing this extraction process associated sample preparation are listed on Table 1.1(Mitra
results in a more detailed analysis. The proper design of the and Brukh 2003)
device and the extraction process makes its implementation
effective on site, integration and sampling and separation / Sample preparation depends on the analytical methods to
quantity, automation or both. Key to rational selection, be used and their strengths. For example, only a few microliters
optimization and design is an understanding of the can be injected into a gas chromatograph. Therefore, in the
fundamental principles that govern transfer analysis in example of the analysis of pesticides in fish liver, the final
multiphase systems.(Pavlović et al. 2007). product is a solution of a few microliters that can be injected
Once the sample is ready for analysis, sample preparation into a gas chromatograph.(Pavlović et al. 2007). Sampling,
is the next step. Most samples are not ready for direct sample preservation, and sample preparation are all aimed at
introduction into instruments. For example, in the analysis of producing those few microliters that represent what is in the
pesticides in fish liver, it is not possible to analyze the liver fish. It is obvious that an error in the first three steps cannot be
directly. The pesticides have to be extracted into a solution, rectified by even the most sophisticated analytical
which can be analyzed by an instrument. There might be instrument(Kratochvil et al. 1984). So, the importance of the
several processes within sample preparation itself. Some steps prior steps, in particular the sample preparation, cannot be
commonly encountered are shown in Figure 1.2(Mitra and under stressed
Brukh 2003). However, they depend on the sample, matrix and
concentration level that will be analyzed. For example,

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International Journal of Academic and Applied Research (IJAAR)
ISSN: 2643-9603
Vol. 6 Issue 11, November - 2022, Pages: 1-6

Table 1.1. Common Instrumental Methods and the Necessary Sample Preparation Steps Prior to Analysis

The objective of research can be qualitative or quantitative (Booksh and Kowalski 1994). For example, the presence of pesticides
in fish is a concern. The question may be: Are there pesticides in the fish? If yes, which ones? The study designed to answer these
questions is a qualitative study (Trullols, Ruisánchez, and Rius 2004), where the researcher looks for the presence of certain antibiotics.
The next obvious question is: how many pesticides are there? This type of research, quantitative research, not only looks at the presence
of the pesticide, but also at its concentration (Etikan and Bala 2017). Another important aspect is the medium analysis. The concern
here is not exactly how much they are, but whether it is above or below a certain point. An example is the prostate-specific antigen
(PSA) test for screening for prostate cancer. A PSA value of 4 ng/L (or more) indicates a high risk of prostate cancer. The goal here is
to determine whether the PSA is above or below 4 ng/L. Once the objectives of the research and the prospective studies are determined,
the methods of conducting the research will be evaluated taking into account accuracy, precision, cost and other important constraints
(Andersen and Hinthorne 1973). The number of tasks, the time required to perform the analysis and the degree of automation may also
be important (Currie 1968).
3.5 Qualitative and Quantitative Analysis
There is rarely one way to design a measurement system. Even well-defined research can be approached in different ways.
Different studies have different goals, different financial problems, staff with different skills and personal interests. The most
important step in designing a study is determining the objectives and at least some idea of the end results. It should generate data that
provides useful information to solve the problem at hand

Almost all measurement procedures, including sample preparation and analysis, require calibration against chemical
standards. The relationship between the detection signal and the number of tests is obtained by recording the response from the
known number (Augusto, Leite e Lopes, and Zini 2003). Similarly, if an extraction method is involved, it is necessary to add a known
amount of analysis to the matrix and measure its recovery. These methods require standards, which can be prepared in the laboratory
or obtained from commercial sources. An important consideration in choosing a pattern is the matrix. For some diagnostic tools,
such as X-ray fluorescence, the matrix is very important, but it may not be critical for others (Ellison and Fearn 2005). Sample
preparation is often matrix-based. It may be easy to remove polycyclic aromatic hydrocarbons from sand by critical extraction, but
not from aged soils with high organic content.

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International Journal of Academic and Applied Research (IJAAR)
ISSN: 2643-9603
Vol. 6 Issue 11, November - 2022, Pages: 1-6

3.6 Methods of Quantitation and Aruna Nigam. 2013. “Sampling: Why and How
The best planning method is to prepare a standard of of It?” Indian Journal of Medical Specialities 4(2).
known concentrations, covering the expected concentration in doi: 10.7713/ijms.2013.0032.
the sample. The standard matrix should be as close to the [2.] Andersen, C. A., and J. R. Hinthorne. 1973.
sample as possible. For example, if the sample is to be “Thermodynamic Approach to the Quantitative
extracted in some organic solvent, the standard must be fixed Interpretation of Sputtered Ion Mass Spectra.”
in the same solvent (Currie 1968). The classification system Analytical Chemistry 45(8):1421–38. doi:
is a detection response scheme as a function of concentration. 10.1021/ac60330a034.
The calibration process is shown in Figure 1.3. It is used to [3.] Augusto, Fabio, Alexandre Leite e Lopes, and
determine the number of tests in an unknown sample. Cláudia Alcaraz Zini. 2003. “Sampling and Sample
Classification can be done in two ways, the best of which is Preparation for Analysis of Aromas and Fragrances.”
using examples (Situmorang 2010). Let's say that the amount TrAC - Trends in Analytical Chemistry 22(3):160–
of lead in the soil is measured. The analytical procedure 69. doi: 10.1016/S0165-9936(03)00304-2.
involves sample preparation by acid extraction followed by [4.] Booksh, Karl S., and Bruce R. Kowalski. 1994.
absorption analysis (AA) (Currie 1968). Patterns can be made “Theory of Analytical Chemistry.” Analytical
by doping pure soil with known conductivity. Then, the values Chemistry 66(15):782A-791A. doi:
are taken from all the steps of extraction and analysis. Finally, 10.1021/ac00087a718.
the response of the instrument is estimated as a function of [5.] Currie, Lloyd A. 1968. “Limits for Qualitative
concentration (Andersen and Hinthorne 1973). Another Detection and Quantitative Determination:
option is to take numerical extraction and these values are Application to Radiochemistry.” Analytical
used to make AA only. The first way is better; the latter is Chemistry 40(3):586–93. doi:
simple (Hatfield et al. 1987)
10.1021/ac60259a007.
4. CONCLUSION [6.] Ellison, S. L. R., and T. Fearn. 2005. “Characterising
the Performance of Qualitative Analytical Methods:
Based on studies from the articles obtained systematically,
Statistics and Terminology.” TrAC - Trends in
the definition of Analyzing, Preparation and Methods
Sampling in Analytical Chemistry refers to the fundamental Analytical Chemistry 24(6):468–76. doi:
aspects of sample preparation and anticipate future 10.1016/j.trac.2005.03.007.
developments and research needs.It can also refer to various [7.] Etikan, Ilker, and Kabiru Bala. 2017. “Biometrics
instrument and their role, but these instrument are used to and Biostratistics.” International Journal Sampling
measure and gettin data from reasearch that was conducted. and Sampling Methods 5(6):215–17.
The three keys of fundamental in chemical analytic has a [8.] Fumes, Bruno Henrique, Meire Ribeiro Silva, Felipe
positive influence for student, including improving Nascimento Andrade, Carlos Eduardo Domingues
understanding of concepts for the theory, improving Nazario, and Fernando Mauro Lanças. 2015.
performance on the laboratory during research, reducing error, “Recent Advances and Future Trends in New
improving self- efficacy, making cognitive structures develop Materials for Sample Preparation.” TrAC - Trends in
for the better, and improving skill and ability, and can reduce Analytical Chemistry 71:9–25. doi:
misconceptions. The results showed that three keys of 10.1016/j.trac.2015.04.011.
fundamental in chemical analytic is Analyzing, Preparation [9.] Hatfield, Galen R., Gary E. Maciel, Oktay Erbatur,
and Methods Sampling in Analytical Chemistry effectively and Gaye Erbatur. 1987. “Qualitative and
improved learners' mastery or understanding of concepts. Quantitative Analysis of Solid Lignin Samples by
Based on the results of the article review that has been done, it Carbon-13 Nuclear Magnetic Resonance
is essential to to learn and understand this thing so student can Spectrometry.” Analytical Chemistry 59(1):172–79.
follow the analytical chemistry course properly. Teachers doi: 10.1021/ac00128a036.
should teach this topic at first in chemistry learning because, [10.] Horwitz, William. 1990. “Nomenclature for
through these three fundamental keys, the abstractness of Sampling in Analytical Chemistry
chemistry skill will become more real and easier to understand
(Recommendations 1990).” Pure and Applied
for learners. As a result, their understanding of chemistry
Chemistry 62(6):1193–1208. doi:
concepts can increase, and the impact of their learning
10.1351/pac199062061193.
outcomes can also increase. In addition, involving Analyzing,
Preparation and Methods Sampling in Analytical Chemistry in [11.] Jungnickel, J. L., and J. W. Forbes. n.d.
learning can reduce learners' assumptions about chemistry “RMNQ1963 JUNGNICKEL.Pdf.” 938–42.
analytic as hard subject to understand.. [12.] Kratochvil, Byron, Dean Wallace, and John K.
Taylor. 1984. “Sampling for Chemical Analysis.”
5. REFERENCES Fundamental Reviews 56(5). doi:
[1.] Acharya, Anita S., Anupam Prakash, Pikee Saxena, 10.1021/ac00231a714.

5
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ISSN: 2643-9603
Vol. 6 Issue 11, November - 2022, Pages: 1-6

[13.] De La Guardia, Miguel. 1999. “An Integrated

Approach of Analytical Chemistry.” Journal of the
Brazilian Chemical Society 10(6):429–37.
[14.] Luis, Francisco, and Gil Moncayo. n.d.
“Development of a Method for Cadmium
Determination in Lipstick. Considerations about the
Digestion Process Assisted by Microwaves and the
Matrix Interferences in the Atomic Absorption
Technique.” 1–39.
[15.] Mitra, Somenath, and Roman Brukh. 2003. Sample
Preparation: An Analytical Perspective.
[16.] Neolaka, Yantus A. B., Eka B. S. Kalla, Gusti A.
Malelak, Nia K. Rukman, Ganden Supriyanto, and
Ni Nyoman Tri Puspaningsih. 2018. “Adsorption of
Methylene Blue Using Acid Activated Green Color
Natural Zeolite from Ende-Flores, Indonesia.”
Rasayan Journal of Chemistry 11(2):494–504. doi:
10.7324/RJC.2018.1121994.
[17.] Pavlović, Dragana Mutavdžić, Sandra Babić, Alka J.
M. Horvat, and Marija Kaštelan-Macan. 2007.
“Sample Preparation in Analysis of
Pharmaceuticals.” TrAC - Trends in Analytical
Chemistry 26(11):1062–75. doi:
10.1016/j.trac.2007.09.010.
[18.] Pawliszyn, Janusz. 1995. “New Directions in Sample
Preparation for Analysis of Organic Compounds.”
Trends in Analytical Chemistry 14(3):113–22. doi:
10.1016/0165-9936(95)94044-F.
[19.] Pawliszyn, Janusz. 2003. “Sample Preparation: Quo
Vadis?” Analytical Chemistry 75(11):2543–58. doi:
10.1021/ac034094h.
[20.] Situmorang, Manihar. 2010. “Kimia Analitik Lanjut
Dan Instrumentasi.” 228.
[21.] Skoog, D. A., West, D. M., Holler, F. J., & Crouch,
S. R. 2004. Fundamentals of Analytical Chemistry
Ed. Eight. Canada: Thomson LearningTM.
[22.] Trullols, Esther, Itziar Ruisánchez, and F. Xavier
Rius. 2004. “Validation of Qualitative Analytical
Methods.” TrAC - Trends in Analytical Chemistry
23(2):137–45. doi: 10.1016/S0165-9936(04)00201-
8.
[23.] Zgorelec, Zeljka, Branka Grahovac, Aleksandra
Percin, Vlatka Jurkovic, Lola Gandjaeva, and Nada
Maurović. 2019. “Comparison of Two Different
CEC Determination Methods Regarding the Soil
Properties.” Agriculturae Conspectus Scientificus
84(2):151–58.

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