Laboratory 1.1

The Language of Analytical Chemistry, Errors and
Statistical Data Treatment in Chemical Analysis

Sampling, Standardization and Calibration
Antonio G. Celajes Jr, RCh
WCC Prayer
Today’s Learning Objectives
• At the end of the lesson, the students will be able to appraise what
practices in analytical laboratory are safe and within standards.
Laboratory Orientation
a. Safety Rules and Procedures in the Laboratory
b. Laboratory Basic Equipment and Instrumentation
c. Preparation of Stock Solution
WCC VISION
We are one of Asia’s best multi-disciplinary colleges of choice and a
recognized leader in producing highly competent, industry-relevant,
and value-laden graduates who contribute to nation-building and
global progress.
WCC MISSION
WCC commits itself to the improvement of lives and advancement of
society by developing exemplary globally competitive professionals and
leaders through comprehensive outcomes-based quality education,
innovative learning design with an experiential approach, stakeholder
collaboration, and a culture upholding Christian values. These we do by
God’s grace to honor and glorify Him.
COLLEGE VISION
The World Citi College of Medical Technology is the premier school for
the development of highly competent and passionate Clinical
Laboratory Scientists committed to promote life for the benefit of
humankind.
COLLEGE MISSION
Being number one requires the College to follow a program of studies
that is relevant, competency and research based, a faculty committed
to teach with excellence and a culture that promotes the highest
professional ideals for the advancement of Laboratory medicine.
Safety Rules and Procedures in the Laboratory
1. Always wear complete personal protective equipment (PPE) while performing

laboratory experiment.
- Complete PPE’s – laboratory gown, gas / dust mask or respirator, safety goggles, gloves and hair net
2. Refrain from eating, drinking and smoking inside the laboratory. These acts are strictly
prohibited.
3. Keep your working area clean, free of any clutter and orderly.
4. Read and understand the procedures and discussions before performing the laboratory
experiment.
5. To prevent accidents in the laboratory, plan your work thoroughly in advance and do it
conscientiously. Report all cases of accidents to your instructor immediately.
6. Record all data and observations obtained in the experiment.
7. Perform only the experiments approved by the instructor.
8. Never take chemicals and equipment outside the laboratory.
9. Familiarize yourselves with the location of the safety and emergency devices
such as first aid equipment, fire exits and safety showers in the laboratory.
10. Be reminded that the laboratory instructor must be the last person to leave
the laboratory room in case of emergency.
11. Keep flammable liquids away from flames.

12. Wash off corrosive substances spilled on skin promptly with plenty of water. Clothes
spilled with chemicals must be removed immediately.
13. Perform under the fume hood experiments that use toxic and corrosive reagent as well
as those that produce undesirable gases.
14. Never flush liquid wastes down the sink. Instead, disposed them in designated waste
bottles.
15. Never return apparatus to the stockroom uncleaned.
16. Keep chemical / reagent bottles closed to avoid contamination and spillage.
17. Clean up working tables for the next users.

Laboratory Glasswares and Basic Apparatus
Measuring Apparatus
1. Graduated Cylinder – used to measure volume of liquid
2. Pipette / pipet – used to measure small volume of liquid
3. Buret – used to measure and deliver volumes of acid and
bases during titration
a. acid buret
b. base buret
4. Balance – used to measure exact weight of solid reagents
a. Analytical Balance
b. Top Loading Balance
c. Triple Beam Balance
Measuring Apparatus
5. Thermometer – used to measure temperature
6. Pycnometer – used to measure relative density of liquids
7. Hydrometer – used to measure density of liquids at room
temperature
a. Light hydrometer – used to measure density of light
liquid materials such as solvents
b. Heavy hydrometer – used to measure density of
heavy liquid materials such as solutions
Heating Apparatus
8. Alcohol Lamp / Bunsen Burner – used to heat reaction using
open flame in the laboratory
9. Tripod – used to assist apparatus during heating
10. Wire Gauze – used to prevent direct contact of heat and
apparatus
11. Crucible and cover – used to heat dry substance at high
temperature
12. Clay triangle – used to hold the crucible and cover in place
during high temperature ignition
13. Evaporating dish – used to removed liquid materials from a
solution by heating
14. Wing top / Fish Tail – used to spread out flames of a Bunsen
burner
Apparatus used as containers / vessels
15. Beaker – used as container in prepare, heating and mixing solutions
16. Erlenmeyer flask – used as container to observe chemical reactions;
swirled constantly during chemical reaction
17. Volumetric Flask – used to prepare exact volume of solutions
18. Test tube – used to observe chemical reactions in small volume; used to
hold small volumes of substances
19. Ignition tube – used in heating small amount of substance
20. Mortar and Pestle – used to grind solids
21. Spot Plate – used to observe chemical reactions involving small amounts
22. Watch Glass – used as container in weighing solid substances; used to dry
solutions without heating
Used in separation
23. Separatory funnel – used in separating immiscible liquids
24. Filter Paper – used to separate solids from liquids
25. Glass Funnel – used to assist filter paper during separation of
solids and liquids; facilitates transfer of liquid from wide to small
mouthed containers
26. Distilling Flask – used to separate miscible liquids through
heating
27. Condenser – assist distilling flask during separation of liquids
Clamping and Holding Apparatus / Equipment
28. Iron Stand – where the holding apparatus is mounted
29. Buret Clamp – used to hold buret in place
30. Iron Clamp – used to hold glasswares in place
31. Test tube holder – used to hold test tube during heating
32. Iron ring – used to hold round bottom flasks in place
33. Test tube rack – used to hold test tubes in place
Transferring / Mixing Apparatus
34. Spatula – used to transfer solid material from one container to another
a. Porcelain Spatula
b. Metal Spatula
35. Aspirator – used to assist pipet in drawing out liquid from a container
36. Medicine dropper – used to transfer liquids drop by drop; can also be
used as measuring device but only for approximation
37. Nichrome wire – used to observe reaction of small amount of materials in
flame / flame reaction
38. Stirring rod – used to stir prepared solutions
39. Crucible Tong – used to hold crucible and cover before and after heating
40. Deflagrating spoon - long-handled spoon with a cover, lowered into a glass
vessel filled with a gas to demonstrate heating a substance until it burns away
rapidly
Basic Laboratory Techniques and Operation
Use of Bunsen Burner / Hot Plate
Porcelain /
Stainless Steel
Plate
Barrel
Temperature
Display
Gas Inlet
Air Hole
Temperature
Gas Adjustment
Adjustment Knob
Knob
Use of Weighing Balance
A. Triple Beam Balance

1.Determine if the balance is properly calibrated and zeroed;
2.Use a weighing paper or preferably, a watch glass, in weighing solids;
3.Move the riders such that the pointer points at 0 on the scale; and
4.Sum up the masses shown on the beams when the pointer is zeroed.
Remember to subtract the weight of the container.
Use of Weighing Balance
B. Top Loading / Analytical Balance

1.Determine if the balance is properly calibrated and zeroed (bubble at the side
should be at the center prior to weighing);
2.Use a weighing paper or preferably, a watch glass, in weighing solids; and
3.Record the reading up to the maximum decimal capacity of the balance (for
analytical balance, close the cover first before reading)
Close cover first
prior to reading
Handling Solid Reagents
1. Take only the amount of solid needed. Do not return unused solids to the
reagent bottle because they may cause contamination.
2. When taking solid samples, use a spatula that is specific for that reagent.
3. When transferring solids to a test tube, used a piece of creased paper to
prevent spillage.
4. When transferring solids from a bottle to a wide-mouthed container like a
beaker, gently rotate the reagent bottle until the solids slowly drop into
the beaker.
Handling Liquid Reagents
1. Never set the stopper of the liquid container directly on the bench.
2. Do not return unused liquid reagents into the reagent bottle.
3. When taking liquids, do not put a pipette inside the reagent bottle.
Instead, put the approximate amount needed in a beaker and then
measure the amount needed.
4. When pouring liquid into a large-mouth container, use a glass
stirring rod to avoid splattering.
Basic Laboratory
Techniques and
Operation
Measuring Liquids
1. Refer to the meniscus (the
curved surface of liquid inside a measuring
device) in determining volume of liquids.
2. Use the upper meniscus for
dark colored liquid and the lower meniscus
X
for clear liquid.
3. Read the volume at eye level.
O
X
Filtration
1. Fold the filter paper twice equally then fit it in a glass funnel.
2. Moisten the edge of the filter paper for it to adhere to the
funnel.
3. Slowly pour down the sample in a stirring rod into a folded
filter paper inside a glass funnel making sure that none of the
mixture rise above the edge of the filter paper.
• At the end of the lesson, the students will be able:

- to generate appreciation of the different analytical techniques;
- produce standard solutions with very minimal margin of error.
The Language of Analytical Chemistry
a. Analysis, Determination, Measurement and Significant Figures
b. Techniques, Methods, Procedures and Protocols
c. Classifying Analytical Techniques
d. Selecting Analytical Methods
e. Developing Procedures and Protocols
f. The Importance of Analytical Methodology
Errors and Statistical Data Treatment in Chemical Analysis, Sampling,

Standardization and Calibration
a. Characterizing Measurements, Results and Experimental
Errors
b. Statistical Analysis of Data
c. Calibration, Standardization and Blank Corrections
d. Obtaining and Preparing Samples for Analysis
Analysis, Determination, and Measurement

- An analysis provides chemical or physical information about a sample;
- The components of interest in the sample are called analytes, and the
remainder of the sample is the matrix;
- In an analysis we determine the identity, concentration, or properties of

the analytes;
- To make this determination we measure one or more of the analyte’s

chemical or physical properties.
Techniques, Methods, Procedures, and Protocols

- A technique is any chemical or physical principle that can be used to study an analyte;
- A method is the application of a technique for the determination of a specific analyte in a

specific matrix;
- A procedure is a set of written directions detailing how to apply a method to a particular

sample, including information on proper sampling, handling of interferents, and validating
results;
- A protocol is a set of stringent written guidelines detailing the procedure that must be
followed if the agency specifying the protocol is to accept the results of the analysis. Protocols
are commonly encountered when analytical chemistry is used to support or define public
policy.
Classifying Analytical Techniques

- Analyzing a sample generates a chemical or physical signal whose magnitude
is proportional to the amount of analyte in the sample;
- The signal may be anything we can measure - common examples are mass,
volume, and absorbance
Analytical Techniques are classified as

Classical / Total Analysis Technique - techniques responding to the absolute
amount of analyte; mass, volume, and charge are the most common signals for
total analysis techniques, and the corresponding techniques are gravimetry,
titrimetry and coulometry.
Analytical Techniques are classified as
- Instrumental / Concentration Analysis Technique - most

concentration techniques rely on measuring an optical or electrical
signal; the signal is proportional to the relative amount of analyte in
a sample; spectroscopy, potentiometry and voltammetry belongs
to this analytical technique
Selecting an Analytical Method

- In choosing a method, consideration is given to some or all the following design criteria: accuracy,
precision, sensitivity, selectivity, robustness, ruggedness, scale of operation, analysis time, availability of
equipment, and cost
Accuracy is a measure of how closely the result of an experiment agrees with the expected result. The
difference between the obtained result and the expected result is usually divided by the expected result
and reported as a percent relative error

A method could be highly accurate (with 1% error); moderately accurate (1% to 5% error) and low
accuracy (greater than 5% error)
Precision is a measure of this variability.
Sensitivity is a measure of its ability to establish that such differences are significant. Sensitivity is often
confused with a method’s detection limit. The detection limit is the smallest amount of analyte that can
be determined with confidence.
Selectivity is measure of a method’s freedom from interferences as defined by the method’s selectivity
coefficient.
A selectivity coefficient greater than +1 or less than –1 indicates that the method is more
selective for the interferent than for the analyte.
where kI is the sensitivity of interferent; kA – analyte When a method is relatively free from
chemical interferences, it can be applied to the determination of analytes in a wide variety of sample
matrices. Such methods are considered robust. A rugged method is relatively insensitive to changes in
experimental conditions.
Scale of operation, equipment, time and cost – other important considerations in selecting analytical
methods
Developing the Procedure

Compensating for Interferences
Calibration and Standardization
Calibration ensures that the equipment or instrument used to measure the signal is
operating correctly by using a standard known to produce an exact signal;
Standardization is the process of experimentally determining the relationship
between the signal and the amount of analyte.
For a total analysis method, standardization is usually defined by the stoichiometry of the
chemical reactions responsible for the signal. For a concentration method, however, the
relationship between the signal and the analyte’s concentration is a theoretical function that
cannot be calculated without experimental measurements
Developing the Procedure

Sampling
A proper sampling strategy ensures that samples are representative of the material from which
they are taken
Validation
Validation is an evaluation of whether the precision and accuracy obtained by following the
procedure are appropriate for the problem. In addition, validation ensures that the written
procedure has sufficient detail so that different analysts or laboratories following the same
procedure obtain comparable results
Developing the Protocol
Besides all the considerations taken into account when designing the procedure, a protocol also contains
very explicit instructions regarding internal and external quality assurance and quality control (QA/QC)
procedures
The Importance of Analytical Methodology
The importance of analytical methodology is evident when examining the results of environmental
monitoring programs. The purpose of a monitoring program is to determine the present status of an
environmental system and to assess long term trends in the quality of the system
Errors and Statistical Data Treatment in
Chemical Analysis, Sampling, Standardization
and Calibration
Characterizing Measurements and Results
Measures of Central Tendency
Two common ways to report this estimate of central tendency are the mean and the median.
The mean, X, is the numerical average obtained by dividing the sum of the individual
measurements by the number of measurements
where X1 is the individual component; n is the number of

independent measurement
and Calibration
The median, Xmed, is the middle value when data are ordered from the smallest to the largest
value.
When the data include an odd number of measurements, the median is the middle value. For
an even number of measurements, the median is the average of the n/2 and the (n/2) + 1
measurements, where n is the number of measurements.
and Calibration
1. The weight of sediments found in the urine of a BS Medical Laboratory Science students were determined 7
times and the following results were obtained: 63.4mg, 49.7mg, 56.5mg, 60.8mg, 59.0mg, 61.5mg and
53.2mg. The actual amount of sediments was found to be 52.8mg. Determine the mean and the median.
2. The creatinine concentration of a blood samples was measured and recorded 8 times. The following results
were obtained: Sample Results, µmol/L Sample Results, µmol/L
1 68.3 5 67.5
2 87.6 6 80.8
3 73.7 7 77.4
4 90.2 8 81.9
Determine the mean and the median from these measurements. The actual creatinine concentration was found
to be 85.3µmol/L.
and Calibration
Measures of Spread
the spread of the individual measurements must provide an estimate of the variability
in the masses of individual samples;
Three common measures of spread are range, standard deviation, and variance. The range, w, is the
difference between the largest and smallest values in the data set.
Range = w = Xlargest – Xsmallest
The absolute standard deviation, s, describes the spread of individual measurements about the mean
and is given as
where Xi is one of n individual measurements
and Calibration
Measures of Spread
Frequently, the relative standard deviation, Sr, is reported.
The percent relative standard deviation is obtained by multiplying Sr by 100%.
Variance - the square of the standard deviation
Determine the range, the absolute standard deviation, the relative standard deviation
and the percent relative standard deviation and the variance of the 2 examples in slide 20.
and Calibration
Characterizing Experimental Errors
Errors associated with central tendency reflect the accuracy of the analysis, but the precision of the analysis is
determined by those errors associated with the spread.
Accuracy is a measure of how close a measure of central tendency is to the true, or expected
value, . Accuracy is usually expressed as either an absolute error
or a percent relative error,
Errors affecting the accuracy of an analysis are called determinate and are characterized by a
systematic deviation from the true value, may be divided into four categories: sampling errors,
method errors, measurement errors, and personal errors.
and Calibration
1. The analysis of fasting blood glucose concentration (FBS) from the blood sample of a BSMLS 1 – MTB
student was repeated 8 times and the following results were observed. The actual FBS reading as found
to be 91.2mg/dL. Determine the mean, median, range, standard deviation, relative standard deviation,
variance, error and percent error.
Student Results, mg/dL Student Results, mg/dL
A 85.7 E 88.2
B 100.8 F 103.5
C 78.9 G 90.8
D 92.7 H 97.6
and Calibration
We introduce determinate sampling errors when our sampling strategy fails to provide a representative sample;
Determinate method errors are introduced when assumptions about the relationship between the signal and the
analyte are invalid;
Analytical instruments and equipment, such as glassware and balances, are usually supplied by the manufacturer
with a statement of the item’s maximum measurement error, or tolerance;
Analytical work is always subject to a variety of personal errors, which can include the ability to see a change
in the color of an indicator used to signal the end point of a titration; biases, such as consistently overestimating
or underestimating the value on an instrument’s readout scale; failing to calibrate glassware and
instrumentation; and misinterpreting procedural directions. Personal errors can be minimized with proper care
and Calibration
Precision is a measure of the spread of data about a central value and may be expressed as the range, the
standard deviation, or the variance. Precision is commonly divided into two categories: repeatability and
reproducibility
Repeatability is the precision obtained when all measurements are made by the same analyst during a single
period of laboratory work, using the same solutions and equipment.
Reproducibility, on the other hand, is the precision obtained under any other set of conditions, including that
between analysts, or between laboratory sessions for a single analyst.
Errors affecting the distribution of measurements around a central value are called indeterminate and are
characterized by a random variation in both magnitude and direction. Indeterminate errors can be traced to
several sources, including the collection of samples, the manipulation of samples during the analysis, and the
making of measurements.
and Calibration
Error and Uncertainty
Error is the difference between a single measurement or result and its true value. Uncertainty
expresses the range of possible values that a measurement or result might reasonably be
expected to have.
and Calibration
Statistical Analysis of Data
The process by which we determine the probability that there is a significant difference between two
samples is called significance testing or hypothesis testing. Before turning to a discussion of specific examples,
however, we will first establish a general approach to conducting and interpreting significance tests.
A significance test is designed to determine whether the difference between two or more values
is too large to be explained by indeterminate error.
The null hypothesis, H0, is that indeterminate error is sufficient to explain any difference in the values being
compared.
The alternative hypothesis, HA, is that the difference between the values is too great to be explained by
random error and, therefore, must be real
and Calibration
Outliers - data points that are not consistent with the remaining data points;
The most commonly used significance test for identifying outliers is Dixon’s Q-test;
The null hypothesis is that the apparent outlier is taken from the same population as the
remaining data;
The alternative hypothesis is that the outlier comes from a different population, and, therefore,
should be excluded from consideration.
and Calibration
Detection limit is the smallest amount or concentration of analyte that can be detected with statistical
confidence;
The International Union of Pure and Applied Chemistry (IUPAC) defines the detection limit as the smallest
concentration or absolute amount of analyte that has a signal significantly larger than the signal arising from
a reagent blank.
and Calibration
Sampling
A chemical analysis uses only a small fraction of the available sample, the process of sampling is a very important
operation.
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.
Many laboratories use the automated sample handling methods

and Calibration
Sampling
Sample Size
Techniques for handling very small samples are quite different from those for
treating macro samples.
and Calibration
Sampling
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 (0.01%) and 1 ppb are called trace constituents.
Components present in amounts lower than 1 ppb are usually considered to be ultratrace
constituents.
and Calibration
Sampling
Constituent Types
and Calibration
Sampling
Real Samples
The analysis of real samples is complicated by the presence of the sample matrix.
The matrix can contain species with chemical properties similar to the analyte.
If the interferences are caused by extraneous species in the matrix, they are often called matrix effects.
Such effects can be induced not only by the sample itself but also by the reagents and solvents used to
prepare the samples for the determination.
Samples are analyzed, but constituents or concentrations are determined

and Calibration
Sampling
The process by which a representative fraction is acquired from a material of interest is termed sampling. (
e.g. a few milliliters of water from a polluted lake)
It is often the most difficult aspect of an analysis.
Sampling for a chemical 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
and Calibration
Sampling
Obtaining a Representative 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
and Calibration
Sampling
Statistically, the goals of the sampling process are:
1. To obtain a mean analyte concentration that is an unbiased estimate of the population mean.
This goal can be realized only if all members of the population have an equal probability of being
included in the sample.
2. To obtain a variance in the measured analyte concentration that is an unbiased estimate of the
population variance so that valid confidence limits can be found for the mean, and various hypothesis
tests can be applied. This goal can be reached only if every possible sample is equally likely to be drawn.
Both goals require obtaining a random sample.
A randomization procedure may be used wherein the samples are assigned a number and then a sample
to be tested is selected from a table of random numbers
and Calibration
Calibrations, Standardizations, and Blank Corrections
Calibration determines the relationship between the analytical response and the analyte concentration, which is
usually determined by the use of chemical standards prepared from
purified reagents.
To reduce interferences from other constituents in the sample matrix, called concomitants,
standards are added to the analyte solution (internal standard methods or standard addition
methods) or matrix matching or modification is done.
Almost all analytical methods require calibration with chemical standards.
Gravimetric methods and some coulometric methods are absolute methods that do not rely on calibration with
chemical standards.
and Calibration
TYPES OF STANDARDS
Primary Standards: must have a known stoichiometry, a known purity, must be
stable for long term storage.
Secondary Standards: have their concentrations determined relative to a primary

standard.
It is crucial to know the amount of all other solution components when preparing standards (e.g.
solvents, acids...)
and Calibration
STANDARD SOLUTIONS
A single standard solution is typically insufficient for accurate calibration of the signal (Stotal)
particularly if the relationship between signal and analyte is not linear.
Two methods exist for creating a range of standards with different concentrations:
Individual preparation: weight standard for each solution to be prepared.
Serial dilution: A high concentration standard solution is prepared and a portion is taken
to make a lower concentration standard. This process is repeated for each successive solution
creating a range of solutions from one weighing of standard.
and Calibration
DETERMINING SENSITIVITY
Determining the relationship between the signal (S) and the amount (nA or CA) of
anlayte in the sample.
Stotal = kAnA + Sreag or Stotal = kACA + Sreag
Stotal: is the measured signal (voltage, mass, volume...)

nA(or CA): is the number of moles, or concentration, of analyte
Sreag: is the signal from components other than the analyte
kA: is the sensitivity of the method to the analyte
and Calibration
SIGNAL CALIBRATION
Equipment used for analysis can yield a range of different signal types, depending
on the tool: glassware, balances, pH meter, spectrophotometer...
Calibration of the signal is necessary to ensure that there are no determinant (systematic) errors
in the measurements to determine kA or Sreag.
This is similar to the calibration of your pipettes and buret.
Calibration ensures that Stotal = Sstd without calibration each measurement will have a
systematic error (X): Stotal = Sstd ± X
and Calibration
STANDARDIZATION
Single-point standardization: Sstd = kAnstd
Using a known standard we can determine the sensitivity (kA) of the technique.
Poor choice for two reasons:

Errors in kA will carry over to all other measurements.
We cannot accurately predict how the system will respond to other concentrations. May assume a
linear relationship, but that may not be true
and Calibration
STANDARDIZATION
Multiple-point standardization
Involves multiple standard solutions, which ideally bracket the expected analyte ranges.
This also minimizes the error of that may afflict a single-point calibration.
Allows us to know the actual relationship between the signal and analyte concentration
and Calibration
BLANK CORRECTIONS
There is more than one type of blank that can be involved in chemical measurements.
The “calibration blank” is a blank used to ensure that the measurement device gives a
zero signal when there is no sample present. This can be an electronic adjustment of
the signal intensity in the absence of sample.
The “reagent blank” is a solution that contains all the same components (matrix) as the
sample solution, but no known analyte materials. The reagent blank identifies the amount of
the signal that is due to the reagents used in the preparation of the samples.
Both blanks can, and should, be subtracted from the measured signal of a sample in order to
determine the signal due to the analyte alone.
and Calibration
Standardization of Sodium Hydroxide and Hydrochloric Acid Solutions
USES Potassium hydrogen phthalate (KHP, MW = 204g/mole) as primary standard
Sodium hydroxide solution is standardized against KHP
Hydrochloric acid solution is standardized using the standard sodium hydroxide solution

Laboratory 1.1

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Laboratory 1.1

Uploaded by

Copyright:

Available Formats

The Language of Analytical Chemistry, Errors and

Statistical Data Treatment in Chemical Analysis

1. Always wear complete personal protective equipment (PPE) while performing

6. Record all data and observations obtained in the experiment.

7. Perform only the experiments approved by the instructor.

8. Never take chemicals and equipment outside the laboratory.

11. Keep flammable liquids away from flames.

15. Never return apparatus to the stockroom uncleaned.

17. Clean up working tables for the next users.

A. Triple Beam Balance

B. Top Loading / Analytical Balance

• At the end of the lesson, the students will be able:

Errors and Statistical Data Treatment in Chemical Analysis, Sampling,

Analysis, Determination, and Measurement

- In an analysis we determine the identity, concentration, or properties of

- To make this determination we measure one or more of the analyte’s

Techniques, Methods, Procedures, and Protocols

- A method is the application of a technique for the determination of a specific analyte in a

- A procedure is a set of written directions detailing how to apply a method to a particular

Classifying Analytical Techniques

Analytical Techniques are classified as

Analytical Techniques are classified as

- Instrumental / Concentration Analysis Technique - most

Selecting an Analytical Method

Selecting an Analytical Method

Precision is a measure of this variability.

Selecting an Analytical Method

Selecting an Analytical Method

Developing the Procedure

Developing the Procedure

Developing the Protocol

The Importance of Analytical Methodology

where X1 is the individual component; n is the number of

Range = w = Xlargest – Xsmallest

The percent relative standard deviation is obtained by multiplying Sr by 100%.

Variance - the square of the standard deviation

or a percent relative error,

Statistical methods are used to aid in the selection of a representative sample.

Many laboratories use the automated sample handling methods

Samples are analyzed, but constituents or concentrations are determined

It is often the most difficult aspect of an analysis.

The collection of sampling units or increments is called the gross sample.

Both goals require obtaining a random sample.

Almost all analytical methods require calibration with chemical standards.

Secondary Standards: have their concentrations determined relative to a primary

Stotal = kAnA + Sreag or Stotal = kACA + Sreag

Stotal: is the measured signal (voltage, mass, volume...)

This is similar to the calibration of your pipettes and buret.

Poor choice for two reasons:

USES Potassium hydrogen phthalate (KHP, MW = 204g/mole) as primary standard

Sodium hydroxide solution is standardized against KHP

You might also like