Analytical Instrumentation

Difference between normal and analytical

instruments
• Purpose:
• Normal Instruments: These instruments are generally designed for routine measurements and provide basic information. Examples include
thermometers, pressure gauges, voltmeters, and speedometers.
• Analytical Instruments: These instruments are specialized for precise and detailed analysis of the composition or properties of a sample.
They are used to obtain specific information about the quantity and nature of the components in a sample.
• Precision and Accuracy:
• Normal Instruments: They may have acceptable precision and accuracy for routine tasks but are not designed for high precision or accuracy
required in analytical work.
• Analytical Instruments: Precision and accuracy are critical in analytical work. These instruments are designed to provide highly accurate and
reproducible results for quantitative and qualitative analysis.
• Complexity:
• Normal Instruments: Typically, normal instruments are simpler in design and operation, with a focus on ease of use for routine
measurements.
• Analytical Instruments: These instruments tend to be more complex, often involving sophisticated technology and methodologies to
achieve high sensitivity and specificity in analytical measurements.
• Type of Information:
• Normal Instruments: Provide basic information such as temperature, pressure, voltage, speed, etc., without detailed analysis of the
components.
• Analytical Instruments: Provide detailed information about the composition, concentration, structure, and properties of the components
within a sample.
• Applications:
• Normal Instruments: Widely used in everyday activities and industrial processes for
monitoring and control purposes.
• Analytical Instruments: Commonly used in scientific research, quality control in industries
like pharmaceuticals and food, environmental monitoring, and forensic analysis.
• Sample Size:
• Normal Instruments: Often used for measurements on a macroscopic scale, where the
characteristics of the entire sample are measured.
• Analytical Instruments: Designed to analyze small quantities of samples, sometimes
down to the microscopic or molecular level.
• Cost:
• Normal Instruments: Generally more affordable due to their simpler design and
widespread use for routine measurements.
• Analytical Instruments: Tend to be more expensive, reflecting the advanced technology
and precision required for detailed analysis.
• Examples:
• Normal Instruments: Thermometers, barometers, ammeters, voltmeters, speedometers,
and basic meters used for everyday measurements.
• Analytical Instruments: Spectrophotometers, chromatographs (such as gas
chromatographs and liquid chromatographs), mass spectrometers, and various sensors
used for chemical and biochemical analysis.
Spectrometry
Spectrometry
Samples and Sampling
About sampling
• Sample: A small portion of material taken from the bulk material and
selected in such a way that it possesses the essential characteristics of
the bulk is called a sample.

• Sampling: Sampling is the process of obtaining a reasonable amount

of material that has all the essential properties of the bulk
material. Or sampling is the science of extracting from a larger
quantity of material, a small portion that is truly representative of the
bulk material.
Cont.
• Knowing how much sample to collect and how to further subdivide
the collected sample to obtain a laboratory sample is vital in the
analytical process.
• Statistical methods are used to aid in the selection of a representative
sample. The analytical sample must be processed in a dependable
manner that maintains sample integrity without losing sample or
introducing contaminants
• Types of Samples and Methods
• Quantitative methods are traditionally classified as
• gravimetric methods,
• volumetric methods,
• and instrumental methods.
• Other methods are based on the size of the sample and the level of
the constituents. Sample Size Techniques for handling very small
samples are quite different from those for treating macro samples.
• Constituent Types
• In some cases, analytical methods are used to determine major
constituents, which are those present in the range of 1 to 100% by
mass.
• Species present in the range of 0.01 to 1% are usually termed minor
constituents.
• Those present in amounts between 100 ppm and 1 ppb are called
trace constituents.
• Components present in amounts lower than 1 ppb are usually
considered to be ultratrace constituents.
Cont.
• Sampling for an analysis necessarily requires the use of statistics because
conclusions will be drawn about a much larger amount of material from
the analysis of a small laboratory sample

• Selection of sample
• The items chosen for analysis are often called sampling units or sampling
increments.
• The collection of sampling units or increments is called the gross sample.
• For laboratory analysis, the gross sample is usually reduced in size and
homogenized to create the laboratory sample.
• The composition of the gross sample and the laboratory sample must
closely resemble the average composition of the total mass of material to
be analyzed
Factors Involved in Sampling
• Nature of bulk material & its homogeneity :-
• If the bulk material is homogenous in nature then sampling is easy and
even a small amount of sample will give accuracy in observation &
readings. While sampling of heterogeneous bulk will involve a greater
number of steps to obtain a sample that will be a true representative of
bulk.
• The expected accuracy of result
• Depending upon the end-use of bulk, the accuracy of bulk sample result is
expected, and depending upon it the type or method of sampling is
selected.
• Cost and time of analysis:-
• The time required for sampling should not be very long and the cost of
sampling should not be more than the cost of the product.
Sampling Uncertainties
• Systematic errors can be eliminated by exercising care, by calibration,
and by the proper use of standards, blanks, and reference materials.
• For random and independent uncertainties, the overall standard
deviation so for an analytical measurement is related to the standard
deviation of the sampling process ss and to the standard deviation of
the method sm by the relationship
Gross Sample
• The gross sample is a miniature replica of the entire mass of material
to be analyzed. It is the collection of individual sampling units.
• Size of the Gross Sample is determined by
• (1) the uncertainty that can be tolerated between the composition of
the gross sample and that of the whole,
• (2) the degree of heterogeneity of the whole
• (3) the level of particle size at which heterogeneity begins.
 Example
• let us presume that a pharmaceutical mixture contains just two types
of particles: * type A particles containing the active ingredient and *
type B particles containing only an inactive filler material
• We wish to collect a gross sample that will allow us to determine the
percentage of particles containing the active ingredient in the bulk
material.
• Assume that the probability of randomly drawing an A type particle is
p and that of randomly drawing a B type particle is (1 - p).
• - If N particles of the mixture are taken, the most probable value for
the number of A type particles is pN, while the most probable
number of B type part is (1 – p)N.
• -- For such a binary population, the Bernoulli equation can be used to
calculate the standard deviation of the number of A particles drawn,
σA:
 • The relative standard deviation σr of drawing A type particles is,

• Thus, the number of particles needed is,

• To determine the number of particles and thus what mass we should

ensure that we have a sample with the overall average percent of active
ingredient P with a sampling relative standard deviation of σr

p-Probability, dA =density of A, d=average density, PA= percentage of sample,σr =relative standard deviation/ uncertainty
Sampling Particulate Solids
• It is often difficult to obtain a
random sample from a bulky
particulate material.
• Random sampling can best be
accomplished while the material
is being transferred.
• Mechanical devices have been
developed for handling many
types of particulate matter
Number of Laboratory Sample
• The number, of samples, depends on the required confidence interval
and the desired relative standard deviation of the method.

• If we solve above Equation for the number of samples N, we obtain

standard deviation of the sampling process ss, Mean value=x

 Automated sample handling
• Automated sample handling can lead to higher throughput (more analyses
per unit time), higher reliability, and lower costs than manual sample
handling.
• Discrete (Batch) Methods These often mimic the operations that would be
performed manually. Some discrete sample processors automate only the
measurement step of the procedure or a few chemical steps and the
measurement step.
• Continuous Flow Methods The sample is inserted into a flowing stream
where a number of operations can be performed prior to transporting it to
a flow-through detector. These methods can perform not only sample
processing operations but also the final measurement step.