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Basic Terms/Concepts IN Analytical Chemistry

This document defines key terms used in analytical chemistry and outlines the typical steps involved in an analytical chemistry procedure. It defines terms like analyte, sample, matrix, concentration, contaminant, blank, and calibration. It then describes the general steps of an analysis as defining the problem, selecting an appropriate method, obtaining a representative sample, preparing the sample, performing any necessary separations, making measurements, and calculating and reporting results. Key factors to consider at each step are highlighted.

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Sheralyn Pelayo
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0% found this document useful (0 votes)
1K views53 pages

Basic Terms/Concepts IN Analytical Chemistry

This document defines key terms used in analytical chemistry and outlines the typical steps involved in an analytical chemistry procedure. It defines terms like analyte, sample, matrix, concentration, contaminant, blank, and calibration. It then describes the general steps of an analysis as defining the problem, selecting an appropriate method, obtaining a representative sample, preparing the sample, performing any necessary separations, making measurements, and calculating and reporting results. Key factors to consider at each step are highlighted.

Uploaded by

Sheralyn Pelayo
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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BASIC TERMS/CONCEPTS

IN
ANALYTICAL CHEMISTRY
DEFINITION OF BASIC TERMS IN
ANALYTICAL CHEMISTRY

ANALYTE – constituent of the sample to be studied by quantitative


measurements or identified qualitatively.
- or the chemical species to be identified or quantitated.
- can be a pure substance or one constituent in a
multi-component sample

SAMPLE – a portion of material selected from a larger quantity of material

MATRIX – the remainder of the sample of which the analyte forms a part.
- ( Sample = analyte + matrix)

CONCENTRATION – the amount of a substance present in a given mass of


volume of another substance.
- w/w, w/v, v/v
Contaminant – a substance, which can include the analyte itself, that is
introduced unintentionally into a sample or a test portion
during collection, processing, or measurement.

Blank – a measurement or observation in which the sample is replaced by


a simulated matrix, the conditions otherwise being identical to those
under which a sample would be analyzed

OR

A standard that contains no analyte, i.e. a concentration of 0.0. The composition,


solvent, analyte etc. should otherwise match the sample test portion. Variations
include method, equipment and instrument blanks for blanks that go through all or
only part of the sample of the sample processing procedures.
CALIBRATION – to measure the response of an instrument by first measuring
the response from a standard
-Series of Standard for Calibration Curve

- A process of measuring a known quantity to determine the relationship


between the measurement signal and the analyte amount or concentration.

CALIBRATION CURVE – a plot of signal vs analyte amount or concentration.


- used to calibrate a measurement over an extended
range.
- good practice is to measure five to ten standards that
are equally spaced through the measurement range.
Scientists typically make repeated
measurements of a quantity to ensure the
quality of their findings and to know both the
precision and the accuracy of their results.
What is Accuracy?

What is Precision?
Table 1: Four Measurements of the Dimensions of a Table
❑ Look at the data in Table 1:

❑ How do you determine the precision of the


series of data?

❑ What can you say about the precision of the


length and width of the table? Why do you say
so?
■ Precision – a measure of how close a
series of measurements are to one
another. A measure of how exact a
measurement is.
■ Measurements are said to be precise if
they yield very similar results when
repeated in the same manner. A
measurement is considered accurate if it
yields a result that is very close to the
true or accepted value. Precise values
agree with each other; accurate values
agree with a true value.
Example: Precision

Who is more precise when measuring the


same 17.0cm book?
Susan:
17.0cm, 16.0cm, 18.0cm, 15.0cm
Amy:
15.5cm, 15.0cm, 15.2cm, 15.3cm
■ The Precision of a set of measurements refers
to how close each measurement is to one
another.
■ The precision is good if the individual
measurements are close to the average.
■ The precision is poor if the measurements
have a wide deviation from the average value.
Accuracy
This refers to the closeness
of the average value to the
actual or true value or most
probable value.
❑ Accuracy - a measure of how close a
measurement is to the true value of the
quantity being measured.
Example: Evaluate whether the following are
precise, accurate or both.

Accurate Not Accurate Accurate


Not Precise Precise Precise
Activity…
• Look at the ruler below

• What would be the measurement in the correct


number of sig figs?
• _______________
❑ The bottom of the meniscus in this case
clearly lies between the 21 and 22 markings,
meaning the liquid volume is certainly greater
than 21 mL but less than 22 mL. The meniscus
appears to be a bit closer to the 22-mL mark
than to the 21-mL mark, and so a reasonable
estimate of the liquid’s volume would be 21.6
mL. In the number 21.6, then, the digits 2 and
1 are certain, but the 6 is an estimate.
QUALITATIVE ANALYSIS IS “WHAT”

QUANTITATIVE ANALYSIS IS “HOW


MUCH”
DEFINE THE PROBLEM
An analysis involves several steps
and operations which depend on:
- The particular problem
- Your expertise
SELECT THE METHOD
- The apparatus and equipment
available GROSS SAMPLE
OBTAIN A REPRESENTATIVE SAMPLE LAB SAMPLE (few gms)
The analyst should be involved ANALYSIS SAMPLE
in every step. (few gms)

PREPARE THE SAMPLE FOR ANALYSIS

PERFORM ANY NECESSARY


CHEMICAL SEPARATION

PERFORM THE MEASUREMENT

CALCULATE THE RESULTS AND REPORT


DEFINE THE PROBLEM
Factors:
• What is the problem ---- What needs to be found?
Quantitative or Qualitative?
• What will the information be used for? Who will use it?
• When will it be needed?
• How accurate and precise does it have to be?
• What is the budget?

The analyst (problem solver) should consult with the client to


plan a useful and efficient analysis including how to obtain a
useful sample.
SELECT A METHOD
FACTORS:
• Sample type
• Sample size
• Sample preparation method
• Concentration and range (sensitivity needed)
• Selectivity needed (interferences)
• Accuracy / precision needed
• Tools / instruments available
• Expertise / experience
• Cost
• Speed
• Does it need to be automated?
• Are methods available in the chemical literature?
• Are standard methods available?
OBTAIN A REPRESENTATIVE
SAMPLE

FACTORS:
• Sample type / homogeneity / size
• Sampling statistics /errors
PREPARE THE SAMPLE FOR ANALYSIS
FACTORS:
• Solid, liquid or gas?
• Dissolve?
• Ash or digest?
• Chemical separation or masking of interferences needed?
• Need to concentrate the analyte?
• Need to change the analyte for detection?
• Need to adjust the solution conditions (pH, reagents)?
PERFORM ANY NECESSARY CHEMICAL SEPARATION

• DISTILLATION
• PRECIPITATION
• SOLVENT EXTRACTION
• SOLID PHASE EXTRACTION
• CHROMATOGRAPHY (maybe done as part of the measurement step)
• ELECTROPHORESIS (maybe done as part of the measurement step)
PERFORM THE MEASUREMENT

FACTORS:
• CALIBRATION
• VALIDATION / CONTROLS / BLANKS
• REPLICATES
CALCULATE THE RESULTS AND REPORT

• STATISTICAL ANALYSIS

• REPORT RESULTS WITH LIMITATION / ACCURACY INTERPRETATION


End

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