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Qualitative Analysis and Quantitative Analysis

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104 views

Qualitative Analysis and Quantitative Analysis

Uploaded by

Umair Umair
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Qualitative and Quantitative Analysis

What Does Each Tell Us?


The discipline of analytical chemistry consists of qualitative analysis and
quantitative. Qualitative analysis tells us what chemicals are present. Quantitative
analysis tells us how much. The former deals with the identification of elements,
ions, or compounds present in a sample (we may be interested in whether only a
given substance is present), while the latter deals with the determination of how
much of one or more constituents is present. The sample may be solid, liquid, gas,
or a mixture. The presence of gunpowder residue on a hand generally requires only
qualitative knowledge, not of how much is there, but the price of coal will be
determined by the percent of undesired sulfur impurity present .

Qualitative tests:
May be performed by selective chemical reactions or with the use of
instrumentation. The formation of a white precipitate when adding a solution of
silver nitrate in dilute nitric acid to a dissolved sample indicates the presence of a
halide. Certain chemical reactions will produce colors to indicate the presence of
classes of organic compounds, for example, ketones. Infrared spectra will give
“fingerprints” of organic compounds or their functional groups. A clear distinction
should be made between the terms selective and specific:
● A selective reaction or test is one that can occur with other substances but exhibits
a degree of preference for the substance of interest.
● A specific reaction or test is one that occurs only with the substance of interest.
Unfortunately, very few reactions are truly specific but many exhibit selectivity.
Selectivity may be also achieved by a number of strategies. Some examples are
 Sample preparation (e.g., extractions, precipitation)
 Instrumentation (selective detectors)
 Target analyte derivatization (e.g., derivatize specific functional groups)
 Chromatography, which separates the sample constituents
Quantitative analysis:
For quantitative analysis, the typical sample composition will often be known
(we know that blood contains glucose), or else the analyst will need to perform
a qualitative test prior to performing the more difficult quantitative analysis.
Modern chemical measurement systems often exhibit sufficient selectivity that a
quantitative measurement can also serve as a qualitative measurement. However,
simple qualitative tests are usually more rapid and less expensive than quantitative
procedures. Qualitative analysis has historically been composed of two fields:
inorganic and organic. The former is usually covered in introductory chemistry
courses, whereas the latter is best left until after the student has had a course in
organic chemistry.

Analytical Methods
 Classical methods
 Instrumental methods
ACQUIRING THE SAMPLE
 A material is Heterogeneous if its constituent parts can be distinguished
visually or with the aid of a microscope. Coal, animal tissue, and soil are
heterogeneous. When the bulk is large and heterogeneous, great effort is
required to get a representative sample.
 Sampling is the process of collecting a small mass of a material whose
composition accurately represents the bulk of the material being sampled.
 The material to be sampled may be solid, liquid, or gas. It may be
homogeneous or heterogeneous in composition. In analyzing for the average
protein content of a shipment of grain, a small sample may be taken from
each bag, or tenth bag for a large shipment, and combined to obtain a gross
sample. Sampling is best done when the material is being moved, if it is
large, in order to gain access. The larger the particle size, the larger should
be the gross sample. The gross sample must be reduced in size to obtain a
laboratory sample of several grams, from which a few grams to milligrams
will be taken to be analyzed (analysis sample).
 The gross sample consists of several portions of the material to be tested.
The laboratory sample is a small portion of this, taken after homogenization.
The analysis sample is that actually analyzed.
 Certain precautions should be taken in handling and storing samples to
prevent or minimize contamination, loss, decomposition, or matrix change.
In general, one must prevent contamination or alteration of the sample by (1)
the container, (2) the atmosphere, (3) heat/temperature, or (4) light.

PROCESSING THE SAMPLE


 The first step in processing the sample is often the preparation of a
laboratory sample. A solid laboratory sample is ground to decrease
particle size, mixed to ensure homogeneity, and stored for various
lengths of time before analysis begins.
 Most chemical analyses are performed on replicate samples whose
masses or volumes have been determined by careful measurements
with an analytical balance or with a precise volumetric device.
Replication improves the quality of the results and provides a measure
of their reliability. Replicate samples, or replicates, are portions of a
material of approximately the same size that are carried through an
analytical procedure at the same time and in the same way.
 Most analyses are performed on solutions of the sample made with a
suitable solvent. Ideally, the solvent should dissolve the entire sample,
including the analyte, rapidly and completely. The conditions of
dissolution should be sufficiently mild that loss of the analyte cannot
occur.
 Converting the analyte in such materials into a soluble form is often
the most difficult and time-consuming task in the analytical process.
The sample may require heating with aqueous solutions of strong
acids, strong bases, oxidizing agents, reducing agents, or some
combination of such reagents. Once the analyte is made soluble, we
then ask whether the sample has a property that is proportional to
analyte concentration and that we can measure. If it does not, other
chemical steps may be necessary, as shown in Figure 1-2, to convert
the analyte to a form that is suitable for the measurement step.
 Organic materials that are to be analyzed for inorganic constituents, for
example, trace metals, may be destroyed by dry ashing. The sample is
slowly combusted in a furnace at 400 to 700◦ C, leaving behind an
inorganic residue that is soluble in dilute acid. Alternately, the organic
matter may be destroyed by wet digestion by heating with oxidizing
acids. A mixture of nitric and sulfuric acids is common. Ashing is the
burning of organic matter. Digestion is the wet oxidation of organic
matter.

ELIMINATING INTERFERENCES
 Once we have the sample in solution and converted the analyte to an
appropriate form for measurement, the next step is to eliminate
substances from the sample that may interfere with measurement.
Species other than the analyte that affect the final measurement are
called interferences, or interferent. An interference or interferent is a
species that causes an error in an analysis by enhancing or attenuating
(making smaller) the quantity being measured.
CALIBRATING AND MEASURING CONCENTRTION
All analytical results depend on a final measurement X of a physical or chemical
property of the analyte, as shown in Figure 1-2. This property must vary in a
known and reproducible way with the concentration Ca of the analyte. Ideally, the
measurement of the property is directly proportional to the concentration, that is,
Ca=kX
where k is a proportionality constant. With a few exceptions, analytical methods
require the empirical determination of k with chemical standards for which Ca is
known. The process of determining k is thus an important step in most analyses;
this step is called a calibration. Calibration is the process of determining the
proportionality between analyte concentration and a measured quantity.

CALCULATING RESULTS
EVALUATING RESULTS BY ESTIMATING RELIABILITY

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